CN106032486B

CN106032486B - Lubricant composition and preparation method thereof

Info

Publication number: CN106032486B
Application number: CN201510106370.8A
Authority: CN
Inventors: 何懿峰; 孙洪伟; 段庆华; 张建荣; 郑会; 刘中其; 姜靓; 陈政
Original assignee: Sinopec Research Institute of Petroleum Processing; China Petroleum and Chemical Corp
Current assignee: Sinopec Research Institute of Petroleum Processing; China Petroleum and Chemical Corp
Priority date: 2015-03-11
Filing date: 2015-03-11
Publication date: 2019-01-08
Anticipated expiration: 2035-03-11
Also published as: CN106032486A

Abstract

The present invention relates to lubricating grease fields, disclose a kind of lubricant composition, the lubricant composition contains base oil and thickening agent, thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium, thickening agent also optionally contains non-newtonian fluid sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, one of non-newtonian fluid calcium oleate is a variety of, on the basis of the weight of the lubricant composition, the content of base oil is 10-80 weight %, the content of non-newtonian fluid sulfurized alkylphenol calcium is 10-70 weight %, the content of non-newtonian fluid sulfoacid calcium is 0-70 weight %, the content of non-newtonian fluid calcium naphthenate is 0-70 weight %, the content of non-newtonian fluid calcium salicylate is 0-70 weight %, the content of non-newtonian fluid calcium oleate is 0-70 weight %.Also disclose the preparation method of lubricant composition.Lubricant composition of the invention has excellent performance.

Description

Lubricant composition and preparation method thereof

Technical field

The present invention relates to a kind of lubricant compositions and preparation method thereof.

Background technique

SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER has preferable detergent-dispersant performance, good acid neutralization capacity and excellent diffusion Property, it is used as the detersive of lubricating oil, is widely used in modulation medium and high classes I. C. engine oil, is particularly suitable for supercharged diesel engine For oil to reduce the carbon deposit of top land and the additive of marine cylinder oil, technology development mainly makes its height alkalization, be exactly Calcium carbonate, which is distributed in flux oil with the sulfurized alkylphenol calcium with surface-active, becomes a kind of colloidal dispersion system.High base number Sulfurized alkylphenol calcium is that alkyl phenol is reacted with CaO, vulcanized, carbonated contour alkalization technology and obtain, and the correlation in relation to preparation is specially Benefit has CN101423483 etc..

It is that raw material produces lubricating grease using calcium sulfonate with high base number, because it is with excellent antirust and anticorrosive property, from investment Since market, the extensive concern of domestic and international lubricating grease industry is caused, however, although high base number composite calcium sulfonate base grease has Very excellent antirust and anticorrosive property, but hardening is easy in storage process, and its raw materials for production calcium sulfonate with high base number is high Price and complicated preparation process itself cause it not promoted rapidly, meanwhile, the requirement with people to environmental protection is got over Come higher, necessary sulfonation process is also increasingly subject to the concern of people to the pollution of environment in calcium sulfonate with high base number production process. It finds a kind of antirust and anticorrosive property is similar with high base number composite calcium sulfonate base grease but can reduce the lubrication of the above problem Rouge becomes the big problem that people face at present.

Summary of the invention

The object of the present invention is to provide one kind to have good antirust and anticorrosive property, storage good security and its raw material system Standby simple process, lubricating grease of environmental protection and preparation method thereof.

The present inventor has found that sulfurized alkylphenol calcium may hold at high temperature due to containing active sulfur under study for action Elemental sulfur easily is precipitated and generates corrosion, therefore, when as detersive, the antirust and anticorrosive property of sulfurized alkylphenol calcium are far below Sulfoacid calcium, but when sulfurized alkylphenol calcium is prepared lubricating grease as thickening agent, but it can get and high base number composite calcium sulfonate Ji Run Consistent lubricant quite even preferably antirust and anticorrosive property, and storage good security.

Therefore, to achieve the goals above, on the one hand, the present invention provides a kind of lubricant composition, the lubricating grease Composition contains base oil and thickening agent, and the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium, and the thickening agent is also optional Contain one of non-newtonian fluid sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate in ground Or it is a variety of, on the basis of the weight of the lubricant composition, the content of base oil is 10-80 weight %, non-newtonian fluid vulcanization The content of alkyl phenol calcium is 10-70 weight %, and the content of non-newtonian fluid sulfoacid calcium is 0-70 weight %, non-newtonian fluid aphthenic acids The content of calcium is 0-70 weight %, and the content of non-newtonian fluid calcium salicylate is 0-70 weight %, the content of non-newtonian fluid calcium oleate For 0-70 weight %.

Preferably, on the basis of the weight of the lubricant composition, the content of base oil is 20-70 weight %, non-ox The content of body sulfurized alkylphenol calcium is 20-65 weight %, and the content of non-newtonian fluid sulfoacid calcium is 0-50 weight %, non-newtonian fluid The content of calcium naphthenate is 0-50 weight %, and the content of non-newtonian fluid calcium salicylate is 0-50 weight %, non-newtonian fluid calcium oleate Content be 0-50 weight %.

Second aspect, the present invention provides the preparation methods of lubricant composition as described above, this method comprises: by thick Agent and part basis oil are uniformly mixed, and refine in 180-230 DEG C of constant temperature, surplus base oil is added, necessary additive is added, Finished product is obtained, the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium, and the thickening agent also optionally contains non-newtonian fluid sulphur One of sour calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate are a variety of.

The third aspect, the present invention provides a kind of preparation methods of lubricant composition, this method comprises:

(1) newton body sulfurized alkylphenol calcium, optional newton body and/or non-newtonian fluid sulfoacid calcium, optional ox will be contained Body and/or non-newtonian fluid calcium naphthenate, optional newton body and/or non-newtonian fluid calcium salicylate and optional newton body and/ Or high base number material and part basis the oil mixing of non-newtonian fluid calcium oleate, obtain mixture；

(2) transforming agent is added, heats up to material retrogradation；

(3) heating dehydration；

(4) it is warming up to 180-230 DEG C of constant temperature refining, surplus base oil is added, necessary additive is added, obtains finished product.

Lithium base or complex lithium, sodium base or compound sodium, potassium base or compound are optionally carried out before or after step (2) Potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or compound zirconium, aluminium base or clad aluminum, polyureas chemical combination One of object or a variety of reactions, and/or it is optionally added into bentonite and/or silica gel.Preferably, it is carried out before step (2) Lithium base or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound Barium, zirconium base or one of compound zirconium, aluminium base or clad aluminum, polyurea compound or a variety of reactions, and/or be added bentonite and/ Or silica gel；Or, carrying out lithium base or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base before and after step (2) Or one in composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or compound zirconium, aluminium base or clad aluminum, polyurea compound Kind or a variety of reactions, and/or bentonite and/or silica gel is added.

Fourth aspect, the present invention provides the lubricant compositions as made from method as described above.

Lubricant composition of the invention with the antirust quite even more excellent with complex calcium sulfonate grease and is prevented Corrosivity, and there is excellent storage stability, also have the viscous resistance better than complex calcium sulfonate grease, machinery stable Property, water-resistance, colloid stability, abrasion resistance and extreme pressure anti-wear, and also there are the performances such as excellent heat-resisting quantity.The present invention Lubricating grease feed preparation process it is simple and environmentally-friendly, stable product quality.

Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.

Specific embodiment

Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.

The present invention provides a kind of lubricant composition, this lubricant composition uses synthesis sulfurized alkylphenol calcium, And optional calcium mahogany sulfonate and/or calcium alkylbenzenesulfonate, optional petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, optionally Salicylate calcium, optional natural calcium oleate and/or synthesis calcium oleate be raw material.

The present invention also provides the preparation methods of foregoing grease composition.

On the one hand, the present invention provides a kind of lubricant composition, lubricant composition contains base oil and thickening agent, thick Agent contains non-newtonian fluid sulfurized alkylphenol calcium, and thickening agent also optionally contains non-newtonian fluid sulfoacid calcium, non-newtonian fluid aphthenic acids One of calcium, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate are a variety of, on the basis of the weight of lubricant composition, The content of base oil is 10-80 weight %, and the content of non-newtonian fluid sulfurized alkylphenol calcium is 10-70 weight %, non-newtonian fluid sulphur The content of sour calcium is 0-70 weight %, and the content of non-newtonian fluid calcium naphthenate is 0-70 weight %, non-newtonian fluid calcium salicylate Content is 0-70 weight %, and the content of non-newtonian fluid calcium oleate is 0-70 weight %.

Preferably, on the basis of the weight of lubricant composition, the content of base oil is 20-70 weight %, non-newtonian fluid The content of sulfurized alkylphenol calcium is 20-65 weight %, and the content of non-newtonian fluid sulfoacid calcium is 0-50 weight %, non-newtonian fluid ring The content of alkanoic acid calcium is 0-50 weight %, and the content of non-newtonian fluid calcium salicylate is 0-50 weight %, non-newtonian fluid calcium oleate Content is 0-50 weight %.

In the present invention, " optionally containing " refers to can be containing the component or without containing the component, that is, non-newtonian fluid One of sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate or it is a variety of be optional group Point, it may include the component in lubricant composition of the invention, can not also include the component.

In the present invention, thickening agent can also containing higher fatty acids, aromatic acid, small molecule inorganic acid, lower fatty acid lithium One of salt, sodium salt, sylvite, calcium salt, strontium salt, barium salt, zirconates, aluminium salt and polyurea compound, bentonite and silica gel are more Kind, that is, thickening agent is also optionally containing higher fatty acids, aromatic acid, small molecule inorganic acid, the lithium salts of lower fatty acid, sodium salt, potassium One of salt, calcium salt, strontium salt, barium salt, zirconates, aluminium salt and polyurea compound, bentonite and silica gel are a variety of.

For higher fatty acids, aromatic acid, small molecule inorganic acid, the lithium salts of lower fatty acid, sodium salt, sylvite, calcium salt, strontium Salt, barium salt, zirconates, aluminium salt and bentonite and silica gel can be higher fatty acids commonly used in the art, virtue without particular/special requirement Acid, small molecule inorganic acid, the lithium salts of lower fatty acid, sodium salt, sylvite, calcium salt, strontium salt, barium salt, zirconates, aluminium salt and bentonite And silica gel, this is known to those skilled in the art, and details are not described herein.

In the present invention, polyurea compound can be polyurea compound commonly used in the art, for example, polyureas without particular/special requirement The structural formula of compound can be

Wherein, n is preferably 0-3 integer.

Wherein, R¹、R⁴It can be the same or different, can be alkyl, naphthenic base or aryl, the carbon of alkyl or cycloalkyl Number can be 8-24, preferably 10-18, and aryl can be phenyl or substituted phenyl, preferably the alkyl of phenyl or C1-C3 or The phenyl that halogen replaces.

Wherein, R²It can be alkylidene or arlydene, the carbon number of alkylidene can be 2-12, preferably 2-8, arlydene It can be phenylene or biphenylene.

Wherein, R³It can be arlydene, alkylidene or cycloalkylidene, the carbon number of arlydene, alkylidene or cycloalkylidene can Think 6-30, preferably 6-20, R³More preferably With-(CH₂)₆In at least It is a kind of.

In the present invention, single polyureas can be used, mixing polyureas also can be used, for example, polyurea compound can be two At least one of polyurea compound, four polyurea compounds, six polyurea compounds and eight polyurea compounds.

Above-mentioned polyurea compound can be obtained using the thinkable various methods of those skilled in the art institute, such as can be by The method system recorded according to CN103060069A, CN103060070A, CN103060068A, CN103060067A, US3243372 It is standby to obtain.

For higher fatty acids, aromatic acid, small molecule inorganic acid, the lithium salts of lower fatty acid, sodium salt, sylvite, calcium salt, strontium The content of salt, barium salt, zirconates, aluminium salt and polyurea compound, bentonite and silica gel in lubricant composition without particular/special requirement, Can be customary amount, for example, on the basis of the weight of lubricant composition, higher fatty acids, aromatic acid, small molecule inorganic acid, The content of the lithium salts of lower fatty acid can be 0-30 weight %, preferably 0-20 weight %；Higher fatty acids, aromatic acid, small point Sub- inorganic acid, lower fatty acid the content of sodium salt can be 0-30 weight %, preferably 0-20 weight %；Higher fatty acids, Aromatic acid, small molecule inorganic acid, lower fatty acid the content of sylvite can be 0-30 weight %, preferably 0-20 weight %；It is high Grade fatty acid, aromatic acid, small molecule inorganic acid, lower fatty acid the content of calcium salt can be 0-30 weight %, preferably 0-20 Weight %；The content of the strontium salt of higher fatty acids, aromatic acid, small molecule inorganic acid, lower fatty acid can be 0-30 weight %, excellent It is selected as 0-20 weight %；Higher fatty acids, aromatic acid, small molecule inorganic acid, lower fatty acid the content of barium salt can be 0-30 Weight %, preferably 0-20 weight %；Higher fatty acids, aromatic acid, small molecule inorganic acid, lower fatty acid the content of zirconates can Think 0-30 weight %, preferably 0-20 weight %；The aluminium salt of higher fatty acids, aromatic acid, small molecule inorganic acid, lower fatty acid Content can be 0-30 weight %, preferably 0-20 weight %；The content of polyurea compound can be 0-30 weight %, preferably For 0-20 weight %；Bentonitic content can be 0-30 weight %, preferably 0-20 weight %；The content of silica gel can be 0-30 weight %, preferably 0-20 weight %.

In the present invention, higher fatty acids can be that carbon number is 8-20, preferably the fatty acid of 10-18 or hydroxy fatty acid, Such as can be at least one of lauric acid, palmitinic acid, stearic acid, 12- hydroxy stearic acid, eicosyl carboxylic acid, preferably 12- hydroxy stearic acid.

In the present invention, aromatic acid is the carboxylic acid that at least 1 carboxyl and aromatic ring are connected directly, and aromatic acid can be substituted or not Substituted aromatic acid, substituent group can be in alkyl, alkenyl, alkynyl, aryl, halogenated or perhalogeno alkyl or aryl etc. extremely The molecular weight of few one kind, aromatic acid is preferably smaller than equal to 550.Aromatic acid is preferably binary aromatic acid, for example, can selected from unsubstituted or The alkyl-substituted phthalic acid of C1-C5, M-phthalic acid, terephthalic acid (TPA), biphenyl dicarboxylic acid, in multi-joint phthalic acid extremely Few one kind.Preferably phthalic acid, M-phthalic acid, terephthalic acid (TPA), biphenyl dicarboxylic acid and methyl substituted biphenyl two At least one of formic acid, multi-joint phthalic acid etc..

In the present invention, the molecular weight of small molecule inorganic acid and lower fatty acid is less than or equal to 250.Wherein, small molecule is inorganic Acid can be selected from least one of boric acid, phosphoric acid, sulfuric acid etc., preferably boric acid and/or phosphoric acid；Lower fatty acid can select From at least one of acetic acid, ethanedioic acid, propionic acid, malonic acid, butyric acid, succinic acid, adipic acid, azelaic acid, decanedioic acid etc., preferably For decanedioic acid.

Non-newtonian fluid sulfurized alkylphenol calcium, non-newtonian fluid sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid salicylic acid Calcium, non-newtonian fluid calcium oleate or combinations thereof object are in infrared spectrum 873cm^-1-886cm^-1There is crystal form calcium carbonate characteristic absorption in place Peak.Non-newtonian fluid sulfurized alkylphenol calcium is converted by newton body sulfurized alkylphenol calcium, non-newtonian fluid sulfurized alkylphenol calcium Total base number be 250-450mgKOH/g, preferably 300-400mgKOH/g；Non-newtonian fluid sulfoacid calcium is by newton body sulfoacid calcium What conversion obtained, the total base number of non-newtonian fluid sulfoacid calcium is 250-450mgKOH/g, preferably 300-400mgKOH/g；Non newtonian Body calcium naphthenate is converted by newton body calcium naphthenate, and the total base number of non-newtonian fluid calcium naphthenate is 250- 450mgKOH/g, preferably 300-400mgKOH/g；Non-newtonian fluid calcium salicylate is converted by newton body calcium salicylate, The total base number of non-newtonian fluid calcium salicylate is 250-450mgKOH/g, preferably 300-400mgKOH/g；Non-newtonian fluid calcium oleate It is to be converted by newton body calcium oleate, the total base number of non-newtonian fluid calcium oleate is 250-450mgKOH/g, preferably 300- 400mgKOH/g.And newton body sulfurized alkylphenol calcium, newton body sulfoacid calcium, newton body calcium naphthenate, newton body calcium salicylate, ox Contain unformed calcium carbonate in body calcium oleate, in infrared spectrum 860cm^-1-865cm^-1There is unformed calcium carbonate feature and inhales in place Receive peak.Newton body sulfurized alkylphenol calcium is synthesis sulfurized alkylphenol calcium, total base number 250-450mgKOH/g, preferably 300- 400mgKOH/g；Newton body sulfoacid calcium is calcium mahogany sulfonate and/or calcium alkylbenzenesulfonate, total base number 250-450mgKOH/g, Preferably 300-400mgKOH/g；Newton body calcium naphthenate is petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, total base number For 250-450mgKOH/g, preferably 300-400mgKOH/g；Newton body calcium salicylate is salicylate calcium, and total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g；Newton body calcium oleate be natural calcium oleate and/or synthesis calcium oleate, Its total base number is 250-450mgKOH/g, preferably 300-400mgKOH/g.Non-newtonian fluid sulfurized alkylphenol calcium, non-newtonian fluid The alkali for the high base number material that sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate mix Value is the weight average value of the base number of each component.

In the present invention, base oil can be mineral oil, synthetic oil, vegetable oil or their mixture, 100 DEG C of dynamic viscosities For 4-150mm²/ s, preferably 10-60mm²/s.Synthetic oil can be poly-a-olefin oil (PAO), Esters oil, alkyl-silicone oil, Fischer-Tropsch Synthetic oil etc..

Various additives, such as antioxidant, extreme pressure anti-wear additives, antirust agent can also be contained in lubricating grease of the invention. Wherein, the preferred arylamine kind antioxidant of antioxidant, accounts for the 0.01-5% of lubricating grease total weight, preferably 0.1-2.5%, can be hexichol At least one of amine, phenyl-α-naphthylamine and di-iso-octyldiphenylamine, preferably di-iso-octyldiphenylamine；Extreme pressure anti-wear additives account for profit The 0.5-12% of consistent lubricant total weight, preferably 0.8-8% can be two thio Acidic phosphates zinc, two thio dialkyl amido first Sour molybdenum, two thio dialkyl amido lead formates, triphenylphosphorothionate, organic molybdenum complex compound, olefine sulfide, molybdenum disulfide, Polytetrafluoroethylene (PTFE), thiophosphoric acid molybdenum, chlorinated paraffin, dibutyl dithiocaarbamate antimony, tungsten disulfide, selenium disulfide, fluorination At least one of graphite, calcium carbonate and zinc oxide；Antirust agent accounts for the 0.01-4.5% of lubricating grease total weight, preferably 0.1-2%, It can be in barium mahogany sulfonate, petroleum sodium sulfonate, benzothiazole, benzotriazole, zinc naphthenate and alkenyl succinic acid at least It is a kind of.

Second aspect, the present invention provides the preparation methods of lubricant composition as described above, this method comprises: by thick Agent and part basis oil are uniformly mixed, and refine in 180-230 DEG C of constant temperature, surplus base oil is added, necessary additive is added, Finished product is obtained, thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium, and thickening agent also optionally contains non-newtonian fluid sulfoacid calcium, non-ox Pause one of body calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate or a variety of.

In the present invention, " optionally containing " is as previously mentioned, details are not described herein.

In the present invention, non-newtonian fluid sulfurized alkylphenol calcium, non-newtonian fluid sulfoacid calcium, non-newtonian fluid calcium naphthenate, non newtonian Body calcium salicylate, non-newtonian fluid calcium oleate, base oil and additive are as previously mentioned, details are not described herein.

It will be understood by those skilled in the art that the sum of the amount of part basis oil and the amount of surplus base oil are used Base oil total amount, in the present invention, the weight ratio of part basis oil and surplus base oil is preferably 1:0.1-5.

For non-newtonian fluid sulfurized alkylphenol calcium, non-newtonian fluid sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid bigcatkin willow Sour calcium, non-newtonian fluid calcium oleate or combinations thereof object, can be by newton body sulfurized alkylphenol calcium, newton body sulfoacid calcium, newton body ring Alkanoic acid calcium, newton body calcium salicylate, newton body calcium oleate or combinations thereof object pass through transforming agent respectively and convert to obtain, for example, by ox Pause body sulfurized alkylphenol calcium, optional newton body sulfoacid calcium, optional newton body calcium naphthenate, optional newton body salicylic acid Calcium, optional newton body calcium oleate and base oil Hybrid Heating are added required transforming agent and are reacted to 50-80 DEG C, own After transforming agent adds, 80-100 DEG C constant temperature 60-90 minutes, then heat to 100-130 DEG C of dehydration.

In the present invention, " optional " refer to can there is the raw material or no raw material, for example, " optional newton body Sulfoacid calcium ", which refers to, can this raw material of newton body sulfoacid calcium, can also not have this raw material of newton body sulfoacid calcium.

(2) transforming agent is added, heats up to material retrogradation；

(3) heating dehydration；

" optional " as previously mentioned, details are not described herein.

In the present invention, newton body sulfurized alkylphenol calcium, newton body sulfoacid calcium, non-newtonian fluid sulfoacid calcium, newton body aphthenic acids Calcium, non-newtonian fluid calcium naphthenate, newton body calcium salicylate, non-newtonian fluid calcium salicylate, newton body calcium oleate, non-newtonian fluid oleic acid Calcium is as previously mentioned, details are not described herein.

In step (1) of the present invention, " optional newton body and/or non-newtonian fluid sulfoacid calcium " refers to that sulfoacid calcium is optional Component, sulfoacid calcium can be newton body sulfoacid calcium, or non-newtonian fluid sulfoacid calcium.Remaining is same.

In step (1) of the present invention, the weight ratio of high base number material total weight and part basis oil is preferably 1:0.1-3.

The present invention can be carried out before or after step (2) lithium base or complex lithium, sodium base or compound sodium, potassium base or Compound potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or compound zirconium, aluminium base or clad aluminum, polyureas One of compound or a variety of reactions, and/or bentonite and/or silica gel is added.That is, appointing before or after step (2) Selection of land carries out lithium base or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound strontium, barium base Or compound barium, zirconium base or one of compound zirconium, aluminium base or clad aluminum, polyurea compound or a variety of reactions, and/or optionally plus Enter bentonite and/or silica gel.This includes four kinds of situations: (i) is without lithium base or complex lithium, sodium base or compound sodium, potassium base or answers Close potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or compound zirconium, aluminium base or clad aluminum and polyureas The reaction for closing object, is added without bentonite and silica gel；(ii) lithium base or complex lithium, sodium base or compound are only carried out before step (2) Sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or compound zirconium, aluminium base or multiple It closes one of aluminium, polyurea compound or a variety of reactions, and/or bentonite and/or silica gel is added, i.e., it is first compound to convert again； (iii) lithium base or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base or composite calcium, strontium are carried out before step (2) Base or compound strontium, barium base or compound barium, zirconium base or one of compound zirconium, aluminium base or clad aluminum, polyurea compound are a variety of anti- It answers, and/or bentonite and/or silica gel is added, also, also carry out lithium base or complex lithium, sodium base or compound after step (2) Sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or compound zirconium, aluminium base or multiple It closes one of aluminium, polyurea compound or a variety of reactions, and/or bentonite and/or silica gel is added, i.e., it is first compound to convert again again again It closes；(iv) lithium base or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base or compound are only carried out after step (2) Calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or one of compound zirconium, aluminium base or clad aluminum, polyurea compound or more Kind reaction, and/or bentonite and/or silica gel is added, i.e., it first converts again compound.

This field is generally transforming agent to be first added to be converted, then carry out recombination reaction, such as makes when preparing lubricating grease When standby complex calcium sulfonate grease.But the present inventor has found under study for action, according to above situation (ii) or (iii) into Row method of the invention, than carrying out method of the invention according to situation (i) and (iv), i.e., first carry out it is all or part of compound, It is converted again, can further improve the performance of lubricating grease obtained.This may be it is compound due to first carrying out, can be more preferable Ground converts the newton body sulfurized alkylphenol calcium of oily to the non-newtonian fluid sulfurized alkylphenol calcium of smectic.It is therefore preferred that in step Suddenly lithium base or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound are carried out before (2) Strontium, barium base or compound barium, zirconium base or one of compound zirconium, aluminium base or clad aluminum, polyurea compound or a variety of reactions, and/or Bentonite and/or silica gel is added；Or, carrying out lithium base or complex lithium, sodium base or compound sodium, potassium base before and after step (2) Or it is compound potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or compound zirconium, aluminium base or clad aluminum, poly- One of carbamide compound or a variety of reactions, and/or bentonite and/or silica gel is added.

For lithium base or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound strontium, Barium base or compound barium, zirconium base or compound zirconium, aluminium base or the respective preparation method of clad aluminum can use this field without particular/special requirement Conventional preparation method, this is known to those skilled in the art, and details are not described herein.For bentonite and silica gel, Ke Yizhi Commercially available from connecing, it is directly added into.

For polyurea compound preparation method without particular/special requirement, single polyureas can be prepared, it is poly- that mixing can also be prepared Urea.Can using the common various methods of those skilled in the art, such as can using CN103060069A as described above, The method preparation that CN103060070A, CN103060068A, CN103060067A, US3243372 are recorded.Preferably, addition portion After point base oil, monoamine, optional diamines, diisocyanate, 100-120 DEG C constant temperature 10-30 minutes, wherein monoamine, optionally Diamines, diisocyanate the amount of substance meet following relationship: the amount of the substance of diisocyanate × 2=monoamine substance Amount × 2 of amount+diamines substance, or, diisocyanate is excessive, excessive amount≤10%.

The structure of the diisocyanate is OCN-R³- NCO, R³Can be carbon number is 6-30, preferably 6-20 arlydene, Alkylidene or cycloalkylidene, preferably -(CH₂)₆Etc..For example, the diisocyanate can be toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate (MDI), two isocyanide of six hexylidene diisocyanates (HDI), dicyclohexyl methyl hydride diisocyanate (HMDI) and xyxylene At least one of acid esters (XDI) etc..

The monoamine can be fatty amine, aliphatic cyclic amine or arylamine, structural formula R¹–NH₂、R⁴–NH₂, R therein¹、R⁴It can be with It is alkyl, naphthenic base or aryl, the carbon number of alkyl or cycloalkyl can be 8-24, preferably 10-18, and aryl can be phenyl or take The phenyl that the phenyl in generation, preferably phenyl or C1-C3 alkyl or halogen replace.Preferred monoamine can be selected from aniline, chlorobenzene The arylamine of amine, parachloroanilinum and/or para-totuidine, and/or selected from lauryl amine, tetradecy lamine, cetylamine, octadecylamine fatty amine.

The diamines can be fatty amine or arylamine, structural formula NH₂–R²–NH₂, wherein R²It can be alkylidene or Asia Aryl, the carbon number of alkylidene can be 2-12, preferably 2-8, and arlydene can be phenylene or biphenylene.Preferred diamines can Be selected from p-phenylenediamine, o-phenylenediamine, 4,4 '-benzidines aromatic amine and/or selected from ethylenediamine, propane diamine, 1,6-oneself The straight-chain fatty amine of diamines.

In step (2) of the present invention, it is preferable that at 50-80 DEG C, required transforming agent is added in preferred constant temperature 10-30 minutes It is reacted, is stirred 8-12 minutes after preferably adding every kind of transforming agent, after all transforming agents add, in 80-100 DEG C of constant temperature 60- 90 minutes.

The transforming agent be preferably selected from fatty alcohol, fatty acid, aliphatic ketone, fatty aldehyde, fatty amine, ether, calcium carbonate, boric acid, In phosphonic acids, carbon dioxide, phenol, aromatic alcohol, aromatic amine, C8-C20 alkyl benzene sulphonate, aphthenic acids, C16-C24 alkyl phenol and water At least one；Be more preferably selected from the fatty alcohol of C1-C5, the fatty acid of C1-C5, the aliphatic ketone of C1-C5, C1-C5 fatty aldehyde, The fatty amine of C1-C5, the ether of C1-C5, boric acid, the alkyl phosphonic acid of C1-C10, the di alkyl phosphonic acid of C2-C16, C6-C20 virtue Base phosphonic acids, the diaryl phosphonic acids of C12-C24, the aromatic alcohol of C7-C20, the aromatic amine of C7-C20, C8-C20 alkyl benzene sulphonate, ring At least one of alkanoic acid, C16-C22 alkyl phenol and water；Still more preferably it is selected from dodecyl benzene sulfonic acid, aphthenic acids, 18 At least one of alkyl phenol, methanol, isopropanol, butanol, boric acid, acetic acid and water.The additional amount of transforming agent is preferably high base number The 2-30% of material total weight, the more preferably 6-22% of high base number material total weight.

In the present invention, fatty alcohol includes straight chain, branch and cricoid fatty alcohol, fatty acid, aliphatic ketone, fatty aldehyde, fat Amine is similarly.

In step (3) of the present invention, it is preferable that be warming up to 100-130 DEG C, preferably remain 30-60 minutes to realize dehydration.

In step (4) of the present invention, it is preferable that be warming up to 180-230 DEG C of constant temperature 5-30 minutes；Surplus base oil is added, to Temperature is cooled to 100-120 DEG C, and necessary additive is added, stirring, circulating filtration, homogenizing, degassing.

In the present invention, the weight ratio of base oil used is preferably 1:0.1- in base oil used and step (4) in step (1) 5。

Fourth aspect, the present invention also provides grease compositions made from the preparation method provided as third aspect present invention Object.

Compared with the lubricant composition made from the preparation method provided as second aspect, preparation side that the third aspect provides Lubricant composition made from method has better viscous resistance, mechanical stability, water-resistance, colloid stability, storage stability And abrasion resistance.

Embodiment

The present invention is further illustrated for embodiment below, but is not intended to limit the present invention.

In the following Examples and Comparative Examples:

Non-newtonian fluid sulfurized alkylphenol calcium, non-newtonian fluid sulfoacid calcium, non-newtonian fluid ring in lubricant composition obtained The total content of alkanoic acid calcium, non-newtonian fluid calcium salicylate and non-newtonian fluid calcium oleate uses non-newtonian fluid sulfurized alkylphenol calcium % table Show, that is,

Non-newtonian fluid sulfurized alkylphenol calcium %=(overbased or SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER raw material weight+superelevation alkali Value or calcium sulfonate with high base number raw material weight+overbased or overbased calcium alkyl-salicylate raw material weight+overbased or high base number water Poplar acid calcium raw material weight+overbased or high base number calcium oleate raw material weight+transforming agent total weight)/lubricating grease total weight × 100%.Transforming agent is included in non-newtonian fluid sulfurized alkylphenol calcium %.

Overbased and SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER is prepared according to patent CN101423483.

Overbased and calcium sulfonate with high base number is prepared according to the method for patent CN101928239A.

Overbased and overbased calcium alkyl-salicylate raw material is purchased from Xinjiang Land Fine Petrochemical Co., Ltd.

Aphthenic acids is purchased from Jinzhou Tie Chen petrochemical industry Co., Ltd.

High base number calcium salicylate is prepared according to the method for patent CN1345921.

High base number calcium oleate is prepared according to document (NLGI Spokeman, 2009,73 (2): 1-17) method.

Embodiment 1

The present embodiment is for illustrating lubricant composition prepared by the present invention.

Raw material components: overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 20kg)；HVI150BS lubrication (100 DEG C of kinematic viscosity are 31mm to base oil²/ s, 15kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；One hydration Lithium hydroxide (1.63kg)；12-hydroxy stearic acids (5.6kg)；Decanedioic acid (1.86kg)；(100 DEG C of HVI500SN lubricating base oil Kinematic viscosity is 11mm²/ s, 10kg).

It in a volume is 160L and with 20kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the overbased sulfurized alkylphenol calcium of 400mgKOH/g and the HVI150BS lubricating base oil of 15kg, stirring；It heats to 90 DEG C, 12-hydroxy stearic acid of 5.6kg and 1.86kg decanedioic acid is added, stirs 10 minutes, is slowly added to be hydrated containing 1.63kg mono- The aqueous solution of lithium hydroxide stirs 10 minutes；50 DEG C are cooled to, constant temperature 10 minutes, 4-octadecylphenol of 2.8kg, temperature is added Degree control is stirred 10 minutes at 50 DEG C, and the aqueous acetic acid that 2.8kg concentration is 20 weight % is added, stirs 10 minutes；It is warming up to 80 DEG C, constant temperature 90 minutes, material retrogradation；It is warming up to 120 DEG C under stirring, is kept for 45 minutes, dehydration；It is warming up to 200 DEG C of constant temperature 10 Minute, it is 11mm that 10kg100 DEG C of kinematic viscosity, which is added,²The HVI500SN lubricating base oil of/s.110 DEG C are cooled to temperature, is followed Ring filtering, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 41.7 weight %；44.6 weight % of lubricating base oil；10.2 weight % of 12- hydroxy lithium stearate；3.5 weight % of decanedioic acid lithium.

Embodiment 2

Raw material components: overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 20kg)；Calcium sulfonate with high base number (total base number 320mgKOH/g, 10kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil²/ s, 30kg)；4– Octadecylphenol (2.8kg)；Acetic acid (0.56kg)；Calcium hydroxide (1.8kg)；12-hydroxy stearic acids (2kg)；Terephthaldehyde Sour (3.5kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil²/ s, 17kg).

It in a volume is 160L and with 20kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle Calcium sulfonate with high base number that overbased sulfurized alkylphenol calcium, 10kg total base number for 400mgKOH/g are 320mgKOH/g and The HVI150BS lubricating base oil of 30kg, stirring；85 DEG C are heated to, it is outstanding that the calcium hydroxide that solid content is 20 weight % is added Turbid 0.9kg is stirred 10 minutes, and 12-hydroxy stearic acid of 0.2kg is added, and is stirred 10 minutes, and 0.35kg terephthaldehyde is added Acid stirs 10 minutes；80 DEG C are cooled to, constant temperature 10 minutes, 4-octadecylphenol of 2.8kg is added, temperature is controlled at 80 DEG C, Stirring 10 minutes is added the aqueous acetic acid that 2.8kg concentration is 20 weight %, stirs 10 minutes, be warming up to 90 DEG C, constant temperature 60 divides Clock, material retrogradation；85 DEG C are cooled to, the calcium hydroxide suspension 8.1kg that solid content is 20 weight % is added, stirs 10 minutes, 12-hydroxy stearic acid of 1.8kg is added, stirs 10 minutes, 3.15kg terephthalic acid (TPA) is added, stirs 10 minutes；The lower heating of stirring It to 110 DEG C, is kept for 60 minutes, dehydration；Being warming up to 230 DEG C, constant temperature for 5 minutes.Then, 160 DEG C are cooled to, is added 17kg's HVI500SN lubricating base oil；120 DEG C are cooled to temperature, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1。

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 38.4 weight %；54.2 weight % of lubricating base oil；2.4 weight % of 12- hydroxy stearic acid calcium；5.0 weight of terephthalic acid (TPA) calcium Measure %.

Embodiment 3

Raw material components: SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total base number 320mgKOH/g, 10kg)；Naphthenate with superhigh base number calcium (total base number 420mgKOH/g, 10kg)；(100 DEG C of kinematic viscosity are 10mm to PAO10 lubricating base oil²/ s, 10kg)；Aphthenic acids (2.8kg)；Acetic acid (0.56kg)；Aluminium isopropoxide (2.2kg)；Stearic acid (2.8kg)；Benzoic acid (1.2kg)；HVI500SN (100 DEG C of kinematic viscosity are 11mm to lubricating base oil²/ s, 10kg).

It in a volume is 160L and with 10kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 320mgKOH/g, 10kg total base number be 420mgKOH/g naphthenate with superhigh base number calcium and The PAO10 lubricating base oil of 10kg, stirring；100 DEG C are heated to, 2.8kg stearic acid and 1.2kg benzoic acid, stirring is added Uniformly, 2.2kg aluminium isopropoxide is added, reacts 30min, water 0.3kg is added, reacts 15min；65 DEG C are cooled to, constant temperature 10 Minute, 2.8kg aphthenic acids is added, temperature is controlled at 65 DEG C, stirred 10 minutes, and the acetic acid that 2.8kg concentration is 20 weight % is added Aqueous solution stirs 10 minutes, is warming up to 100 DEG C, and constant temperature 70 minutes, material retrogradation；It is warming up to 130 DEG C under stirring, is kept for 30 points Clock, dehydration；It is warming up to 180 DEG C of constant temperature 20 minutes, 10kgHVI500SN is added.100 DEG C are cooled to temperature, circulating filtration, Change, degassing obtains finished product.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 48.9 weight %；41.8 weight % of lubricating base oil；9.3 weight % of clad aluminum.

Embodiment 4

Raw material components: overbased sulfurized alkylphenol calcium (total base number 420mgKOH/g, 22kg)；High base number calcium oleate (total base number 360mgKOH/g, 8kg)；(100 DEG C of kinematic viscosity are 31mm to HVI150BS lubricating base oil²/ s, 30kg)；4-ten Eight alkylphenols (2.8kg)；Acetic acid (0.56kg)；Calcium hydroxide (1.8kg)；12-hydroxy stearic acids (2kg)；Terephthalic acid (TPA) (3.5kg)；Aluminium isopropoxide (2.41kg)；Stearic acid (2.8kg)；Benzoic acid (1.2kg)；4# ethyl silicon oil (10kg).

It in a volume is 160L and with 22kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle The high base number calcium oleate and 30kg that overbased sulfurized alkylphenol calcium, 8kg total base number for 420mgKOH/g are 360mgKOH/g HVI150BS lubricating base oil, stirring；100 DEG C are heated to, 2.8kg stearic acid and 1.2kg benzoic acid is added, stirring is equal It is even, 2.41kg aluminium isopropoxide is added in 100 DEG C of reaction 30min, water 0.3kg is added, reacts 30min；50 DEG C are cooled to, Constant temperature 10 minutes, 4-octadecylphenol of 2.8kg is added, temperature is controlled at 50 DEG C, stirred 10 minutes, and 2.8kg concentration is added and is The aqueous acetic acid of 20 weight % stirs 10 minutes, is warming up to 80 DEG C, and constant temperature 90 minutes, material retrogradation；It is 20 that solid content, which is added, The calcium hydroxide suspension 9kg of weight % is stirred 10 minutes, and 12-hydroxy stearic acid of 2kg is added, and is stirred 10 minutes, is added 3.5kg terephthalic acid (TPA) stirs 10 minutes；It is warming up to 110 DEG C under stirring, is kept for 45 minutes, dehydration；It is warming up to 200 DEG C of constant temperature 10 minutes.Then, 160 DEG C are cooled to, the 4# ethyl silicon oil lubricating base oil of 10kg is added, is cooled to 110 DEG C to temperature, circulation Filtering, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 39.6 weight %；47.5 weight % of lubricating base oil；13.1 weight % of clad aluminum calcium.

Embodiment 5

Raw material components: overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 10kg)；Overbased sulfoacid calcium (total base number 400mgKOH/g, 10kg)；Naphthenate with superhigh base number calcium (total base number 400mgKOH/g, 10kg)；HVI150BS (100 DEG C of kinematic viscosity are 31 mm to lubricating base oil²/ s, 15kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)； Acetone (5kg)；Organobentonite (15kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil²/ s, 25kg).

It in a volume is 160L and with 10kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle Overbased sulfoacid calcium that overbased sulfurized alkylphenol calcium, 10kg total base number for 400mgKOH/g are 400mgKOH/g, 10kg total base number is the naphthenate with superhigh base number calcium of 400mgKOH/g and the HVI150BS lubricating base oil of 15kg, is stirred, heating It is warming up to 50 DEG C, constant temperature 10 minutes；4-octadecylphenol of 2.8kg is added, temperature is controlled at 50 DEG C, stirred 10 minutes；Add Enter the aqueous acetic acid that 2.8kg concentration is 20 weight %, stirs 10 minutes；It is warming up to 80 DEG C, constant temperature 90 minutes, material retrogradation； 120 DEG C of constant temperature 1h dehydrations are warming up to, it is 11mm that 25kg100 DEG C of kinematic viscosity, which is added,²The HVI500SN lubricating base oil of/s, drop Temperature is added 15kg organobentonite and 5kg acetone, 1h is sufficiently stirred to 40 DEG C, is warming up to 85 DEG C of removing acetone, circulating filtration, Homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 37.7 weight %；45.3 weight % of lubricating base oil；17.0 weight % of organobentonite.

Embodiment 6

Raw material components: overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 8kg)；High base number calcium salicylate (total base number 320mgKOH/g, 12kg)；High base number calcium oleate (total base number 360mgKOH/g, 10kg)；HVI150BS lubrication (100 DEG C of kinematic viscosity are 31mm to base oil²/ s, 15kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；Hard charcoal Black (12kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil²/ s, 25kg).

It in a volume is 160L and with 8kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle High base number calcium salicylate that overbased sulfurized alkylphenol calcium, 12kg total base number for 400mgKOH/g are 320mgKOH/g, 10kg total base number is the high base number calcium oleate of 360mgKOH/g and the HVI150BS lubricating base oil of 15kg, stirring, heat temperature raising To 50 DEG C, constant temperature 10 minutes；4-octadecylphenol of 2.8kg is added, temperature is controlled at 50 DEG C, stirred 10 minutes；It is added 2.8kg concentration is the aqueous acetic acid of 20 weight %, is stirred 10 minutes；It is warming up to 80 DEG C, constant temperature 90 minutes, material retrogradation；It rises Temperature is dehydrated to 120 DEG C of constant temperature 1h, and it is 11 mm that 25kg100 DEG C of kinematic viscosity, which is added,²The HVI500SN lubricating base oil of/s, cooling To 40 DEG C, 12kg white carbon black is added, stirs evenly, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 39.0 weight %；46.9 weight % of lubricating base oil；14.1 weight % of white carbon black.

Embodiment 7

Raw material components: SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total base number 360mgKOH/g, 5kg)；Non-newtonian fluid high base number sulphur Sour calcium (15kg)；High base number calcium oleate (total base number 320mgKOH/g, 10kg)；HVI150BS lubricating base oil (100 DEG C of fortune Kinetic viscosity is 31mm²/ s, 15kg)；4-octadecylphenols (2.8kg)；Acetic acid (0.56kg)；Zr(OH)₄(3.9kg)；12-hydroxyls Base stearic acid (2kg)；Terephthalic acid (TPA) (3.5kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil²/ s, 32kg)。

The preparation of non-newtonian fluid calcium sulfonate with high base number: in a volume being 30L and with heating, stirring, circulation, cooling 100 DEG C of kinematic viscosity of calcium sulfonate with high base number and 5kg that 8kg total base number is 350mgKOH/g are added in normal-pressure reaction kettle is 31mm²The HVI150BS lubricating base oil of/s, stirring, heats to 80 DEG C, constant temperature 10 minutes；1.7kg dodecyl is added Benzene sulfonic acid, temperature are controlled at 80 DEG C or so, are stirred 10 minutes；The acetic acid and 4 times of acetic acid weight of aqueous solution of 0.33kg is added, stirs It mixes 10 minutes；85 DEG C are warming up to, constant temperature 90 minutes, it is spare to obtain non-newtonian fluid sulfoacid calcium at smectic for material retrogradation.

Lubricant composition is prepared according to the method for embodiment 1, unlike, sulfurized alkylphenol calcium is using total base number The SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 320mgKOH/g, and increase non-newtonian fluid calcium sulfonate with high base number and high base number calcium oleate；With Zr(OH)₄Instead of a hydronium(ion) lithia, decanedioic acid is replaced with terephthalic acid (TPA), the dosage of each ingredient is as above.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 37.7 weight %；53.2 weight % of lubricating base oil；12-hydroxy stearic acid oxygen zirconium, 2.6 weight %；Terephthalic acid (TPA) oxygen zirconium 6.5 Weight %.

Embodiment 8

Raw material components: overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 15kg)；High base number calcium salicylate (total base number 320mgKOH/g, 15kg)；(100 DEG C of kinematic viscosity are 41mm to full synthetic oil poly & Alpha ,-olefin oil PAO 40²/ s, 15kg)；Dodecyl benzene sulfonic acid (2.8kg)；Acetic acid (0.56kg)；Boric acid (2.32kg)；Octadecylamine (1.08kg)；Ethylenediamine (0.12kg)；MDI(1kg)；(100 DEG C of kinematic viscosity are 11mm to full synthetic oil poly & Alpha ,-olefin oil PAO 10²/ s, 26kg)；Two fourths Base zinc dithiophosphate (2kg)；Dibutyl dithiocaarbamate molybdenum (1kg)；Tungsten disulfide (2kg)；Two tungsten selenides (2kg)； It is right, right '-di-iso-octyldiphenylamine (0.2kg).

It in a volume is 160L and with 15kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle High base number calcium salicylate that overbased sulfurized alkylphenol calcium, 15kg total base number for 400mgKOH/g are 320mgKOH/g and 40 lubricating base oil of PAO of 15kg, stirring are warming up to 120 DEG C, and 1kgMDI is added, and stir 10 minutes, are added with stirring 1.08kg octadecylamine and 0.12kg ethylenediamine, the molar ratio of added MDI, ethylenediamine and octadecylamine are 2:1:2,120 DEG C of constant temperature 20 minutes；It is cooled at 50 DEG C, constant temperature 10 minutes, 2.8kg dodecyl benzene sulfonic acid is added, temperature controls the stirring 10 at 50 DEG C Minute, the acetic acid and 4 times of acetic acid weight of aqueous solution of 0.56kg is added, stirs 10 minutes, 2.32kg boric acid is added and with 6 times The boric acid solution that hot water is completely dissolved, stirring, 80 DEG C constant temperature 90 minutes, material retrogradation is warming up to 120 under stirring at smectic DEG C, it is kept for 45 minutes, dehydration；It is warming up to 200 DEG C of constant temperature 10 minutes.Then, 160 DEG C are cooled to, the PAO10 profit of 26kg is added Sliding base oil；110 DEG C are cooled to temperature, the zinc dibutyl dithiophosphate of 2kg is added, stirs 10 minutes, is added 1kg's Dibutyl dithiocaarbamate molybdenum stirs 10 minutes, and the tungsten disulfide of 2kg is added, and stirs 10 minutes, two selenium of 2kg are added Change tungsten, stir 10 minutes, be added pair of 0.2kg, right '-di-iso-octyldiphenylamine stirs 10 minutes, then circulating filtration, Change, degassing obtains finished product；The dosage of each ingredient is as above.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 41.3 weight %；2.6 weight % of polyureas；44.0 weight % of lubricating base oil；Two thio 3.4 weight % of dibutylphosphoric acid zinc；Two 1.7 weight % of butyl molybdenum dithiocarbamate；3.4 weight % of tungsten disulfide；Two tungsten selenides, 3.4 weight %；It is right, right '-two 0.2 weight % of di-iso-octyldiphenylamine.

Embodiment 9

The present embodiment is for illustrating composite sulfuration alkyl phenol calcium-base grease prepared by the present invention.

Raw material components: overbased sulfurized alkylphenol calcium (total base number 400mgKOH/g, 8kg)；Calcium sulfonate with high base number is (total Base number is 320mgKOH/g, 5kg)；High base number calcium salicylate (total base number 360mgKOH/g, 5kg)；Naphthenate with superhigh base number Calcium (total base number 420mgKOH/g, 6kg)；High base number calcium oleate (total base number 320mgKOH/g, 6kg)；HVI150BS lubrication (100 DEG C of kinematic viscosity are 31mm to base oil²/ s, 40kg)；4- octadecylphenol (2.8kg)；Acetic acid (0.56kg)；Hydrogen-oxygen Change calcium (1.8kg)；12- hydroxy stearic acid (2kg)；Terephthalic acid (TPA) (3.5kg)；HVI500SN lubricating base oil (100 DEG C of fortune Kinetic viscosity is 11mm²/ s, 7kg).

It in a volume is 160L and with 8kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle Calcium sulfonate with high base number that overbased sulfurized alkylphenol calcium, 5kg total base number for 400mgKOH/g are 320mgKOH/g, 5kg are total Naphthenate with superhigh base number calcium that high base number calcium salicylate that base number is 360mgKOH/g, 6kg total base number are 420mgKOH/g, 6kg Total base number is the high base number calcium oleate of 320mgKOH/g and the HVI150BS lubricating base oil of 20kg, and stirring is warming up to 95 DEG C, The calcium hydroxide suspension 9kg that solid content is 20 weight % is added, stirs 10 minutes；2kg 12- hydroxy stearic acid, stirring is added 10 minutes；3.5kg terephthalic acid (TPA) is added, stirs 10 minutes.The HVI150BS lubricating base oil that 20kg is added is down to material 50 DEG C, constant temperature 10 minutes, 2.8kg 4- octadecylphenol is added, temperature is controlled at 50 DEG C, stirred 10 minutes；2.8kg is added Concentration is the aqueous acetic acid of 20 weight %, is stirred 10 minutes；It is warming up to 80 DEG C, constant temperature 90 minutes, material retrogradation；It is risen under stirring Temperature is kept for 45 minutes to 120 DEG C, dehydration.It is warming up to 200 DEG C of constant temperature 10 minutes, then, is cooled to 160 DEG C, is added 7kg's HVI500SN lubricating base oil；110 DEG C are cooled to temperature, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1。

Embodiment 10

Raw material components: SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total base number 360mgKOH/g, 30kg)；HVI150BS lubricates base (100 DEG C of kinematic viscosity are 31mm to plinth oil²/ s, 30kg)；4- octadecylphenol (2.6kg)；Acetic acid (1.0kg)；Boric acid (2kg)；12- hydroxy stearic acid (2.5kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil²/ s, 15kg).

It in a volume is 160L and with 30kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 360mgKOH/g and the HVI150BS lubricating base oil of 30kg, stir evenly, at 60 DEG C Under, 1.8kg 4- octadecylphenol is added, stirs 20 minutes；The aqueous acetic acid that 2.8kg concentration is 20 weight % is added, Stirring 20 minutes；The boric acid aqueous solution that 10kg concentration is 20 weight % is added, stirs 30 minutes；2kg 12- hydroxy stearate is added Acid stirs 30 minutes；It is warming up to 95 DEG C, constant temperature 120 minutes, material retrogradation；It is warming up to 110 DEG C under stirring, is kept for 60 minutes, Dehydration.It is warming up to 180 DEG C of constant temperature 20 minutes.Then, the HVI500SN lubricating base oil of 15kg is added；100 are cooled to temperature DEG C, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 44.7 weight %；55.3 weight % of lubricating base oil.

Embodiment 11

Raw material components: SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER (total base number 360mgKOH/g, 10kg)；High base number calcium salicylate (total base number 360mgKOH/g, 10kg)；High base number calcium oleate (total base number 360mgKOH/g, 10kg)；HVI150BS lubrication (100 DEG C of kinematic viscosity are 31mm to base oil²/ s, 15kg)；Dodecyl benzene sulfonic acid (2.8kg)；Acetic acid (0.56kg)；Hydrogen-oxygen Change sodium (1.2kg)；12-hydroxy stearic acids (5.6kg)；Decanedioic acid (1.86kg)；Benzoic acid (1.1kg)；Barium hydroxide octahydrate (3.0kg)；(100 DEG C of kinematic viscosity are 11mm to HVI500SN lubricating base oil²/ s, 10kg).

It in a volume is 160L and with 10kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the SULFURIZED CALCIUM ALKYL PHENATE WITH HIGH BASE NUMBER of 360mgKOH/g, 10kg total base number be 360mgKOH/g high base number calcium salicylate, 10kg Total base number is the high base number calcium oleate of 360mgKOH/g and the HVI150BS lubricating base oil of 15kg, stirring；Heat to 95 DEG C, 12-hydroxy stearic acid of 2.8kg and 1.86kg decanedioic acid is added, stirs 10 minutes, the water-soluble of the sodium hydroxide containing 1.2kg is added Liquid stirs 10 minutes；50 DEG C are cooled to, constant temperature 10 minutes, 4-octadecylphenol of 2.8kg is added, temperature is controlled at 50 DEG C, Stirring 10 minutes is added the aqueous acetic acid that 2.8kg concentration is 20 weight %, stirs 10 minutes；80 DEG C are warming up to, constant temperature 90 divides Clock, material retrogradation；1.1kg benzoic acid and 2.8kg12-hydroxy stearic acid is added, stirs 10 minutes, is added and is hydrated containing 3.0kg eight The aqueous solution of barium hydroxide stirs 30 minutes；It is warming up to 120 DEG C under stirring, is kept for 45 minutes, dehydration；It is warming up to 200 DEG C of perseverances Temperature 10 minutes, it is 11mm that 10kg100 DEG C of kinematic viscosity, which is added,²The HVI500SN lubricating base oil of/s.110 are cooled to temperature DEG C, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.

In the lubricating grease that the present embodiment obtains, on the basis of lubricating grease weight, composition are as follows: non-newtonian fluid sulfurized alkylphenol calcium 48.5 weight %；36.3 weight % of lubricating base oil；Compound 15.2 weight % of sodium barium.

Embodiment 12

It in a volume is 160L and with 20kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the overbased sulfurized alkylphenol calcium of 400mgKOH/g and the HVI150BS lubricating base oil of 15kg, stirring is warming up to 50 DEG C, constant temperature 10 minutes, 4-octadecylphenol of 2.8kg is added, temperature is controlled at 50 DEG C, stirred 10 minutes, and it is dense that 2.8kg is added Degree is the aqueous acetic acid of 20 weight %, is stirred 10 minutes；It is warming up to 80 DEG C, constant temperature 90 minutes, material retrogradation；

It in another volume is 30L and with being added 100 DEG C of 5kg in heating, stirring, circulation, cooling normal-pressure reaction kettle Kinematic viscosity is 11mm²The HVI500SN lubricating base oil of/s, is warming up to 90 DEG C, be added 12-hydroxy stearic acid of 5.6kg and 1.86kg decanedioic acid stirs 10 minutes, is slowly added to the aqueous solution of the mono- hydronium(ion) lithia containing 1.63kg, stirs 30 minutes；? To 12- hydroxy lithium stearate and decanedioic acid lithium.

Gained 12- hydroxy lithium stearate and decanedioic acid lithium are all squeezed into a upper kettle, 120 DEG C are warming up under stirring, It is kept for 45 minutes, dehydration；It is warming up to 200 DEG C of constant temperature 10 minutes, addition 100 DEG C of kinematic viscosity of surplus are 11mm²/ s's HVI500SN lubricating base oil.110 DEG C are cooled to temperature, circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1。

Embodiment 13

It in a volume is 160L and with 20kg total base number is added in heating, stirring, circulation, cooling normal-pressure reaction kettle For the overbased sulfurized alkylphenol calcium of 400mgKOH/g and the HVI150BS lubricating base oil of 15kg, stirring；It heats to 50 DEG C, constant temperature 10 minutes, 4-octadecylphenol of 2.8kg is added, temperature is controlled at 50 DEG C, stirred 10 minutes, and 2.8kg is added Concentration is the aqueous acetic acid of 20 weight %, is stirred 10 minutes；It is warming up to 80 DEG C, constant temperature 90 minutes, material retrogradation；It is warming up to 90 DEG C, 12-hydroxy stearic acid of 5.6kg and 1.86kg decanedioic acid is added, stirs 10 minutes, is slowly added to mono- hydronium(ion) containing 1.63kg The aqueous solution of lithia stirs 10 minutes；It is warming up to 120 DEG C under stirring, is kept for 45 minutes, dehydration；It is warming up to 200 DEG C of constant temperature 10 minutes, it was 11mm that 10kg100 DEG C of kinematic viscosity, which is added,²The HVI500SN lubricating base oil of/s.110 DEG C are cooled to temperature, Circulating filtration, homogenizing, degassing obtain finished product.Inspection result is shown in Table 1.

Embodiment 14

Lubricant composition is prepared according to the method for embodiment 1, unlike, 4-octadecylphenols are replaced with 18 Acetic acid is replaced with methyl ethyl ketone by amine.Inspection result is shown in Table 1.

Comparative example 1

Lubricant composition is prepared according to the method for embodiment 1, unlike, overbased sulfurized alkylphenol calcium total alkali Value is replaced by the overbased sulfoacid calcium of 400mgKOH/g, and obtained each performance data of lubricating grease finished product is shown in Table 1.

In the lubricating grease that this comparative example obtains, on the basis of lubricating grease weight, composition are as follows: 41.7 weight of non-newtonian fluid sulfoacid calcium Measure %；44.6 weight % of lubricating base oil；10.2 weight % of 12- hydroxy lithium stearate；3.5 weight % of decanedioic acid lithium.

Each lubricating grease properties of sample data of table 1

Each indication test method: dropping point: GB/T 3498；Work cone penetration and extension work cone penetration: GB/T 269；It is rotten Erosion: GB/T 7326；Anticorrosive property: GB/T 5018；Water drenches number of dropouts: SH/T 0109；Salt spray test: SH/T 0081；Water resistant It is spraying: SH/T0643；Stencil oil-dividing: SH/T 0324；Surface hardened layer value: 0370 appendix A of SH/T；Coefficient of friction: SH/T 0721；Tetra-ball machine test: SH/T 0202.

Each lubricating grease properties of sample data of 1 (Continued) of table

It will be understood by those skilled in the art that work cone penetration is smaller, grease thickening performance is better；Extend work The difference for making cone penetration and the cone penetration that works is smaller, and the mechanical stability of lubricating grease can be better；Water leaching number of dropouts is smaller, lubricating grease Water-resistance it is better；Salt spray test higher grade, and the antirust and anticorrosive property of lubricating grease are better；Water resistant is worth smaller, lubrication by spraying The adhesiveness and water-resistance of rouge are better；Stencil oil-dividing value is smaller, and the colloid stability of lubricating grease is better；Surface hardened layer value it is absolute It is worth smaller, the storage stability of lubricating grease is better；The coefficient of friction of lubricating grease is smaller, and the abrasion resistance of lubricating grease is better；PB,PD Value is bigger, and the extreme pressure anti-wear of lubricating grease is better.

Embodiment 1 and comparative example 1 are compared to antirust and anticorrosion as can be seen that lubricant composition of the invention Property, storage stability be substantially better than complex calcium sulfonate grease.Moreover, lubricant composition of the invention has better than compound Viscous resistance, mechanical stability, water-resistance, colloid stability, abrasion resistance and the extreme pressure anti-wear of calcium sulfonate grease.And And lubricant composition of the invention also has excellent heat-resisting quantity.

Embodiment 1 and embodiment 11 are compared the lubricant composition as can be seen that being prepared in situ, had better Viscous resistance, mechanical stability, water-resistance, colloid stability, storage stability and abrasion resistance；By embodiment 1 and embodiment 11, Embodiment 12 is compared as can be seen that first carry out compound, then is converted, lubricant composition obtained has preferably thick The property changed, mechanical stability, water-resistance, colloid stability, storage stability and abrasion resistance；By embodiment 1 and embodiment 13 into Row is relatively as can be seen that transforming agent is selected from dodecyl benzene sulfonic acid, aphthenic acids, octadecyl phenol, methanol, isopropanol, butanol, boron At least one of acid, acetic acid and water, lubricant composition obtained have better viscous resistance, mechanical stability, water resistant Property, colloid stability, storage stability and abrasion resistance.

The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this A little simple variants all belong to the scope of protection of the present invention.

It is further to note that specific technical features described in the above specific embodiments, in not lance In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can No further explanation will be given for the combination of energy.

In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims

1. a kind of lubricant composition, the lubricant composition contains base oil and thickening agent, which is characterized in that the thickening Agent contains non-newtonian fluid sulfurized alkylphenol calcium, and the thickening agent also optionally contains non-newtonian fluid sulfoacid calcium, non-newtonian fluid cycloalkanes One of sour calcium, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate are a variety of, and the weight with the lubricant composition is Benchmark, the content of base oil are 10-80 weight %, and the content of non-newtonian fluid sulfurized alkylphenol calcium is 10-70 weight %, non newtonian The content of body sulfoacid calcium is 0-70 weight %, and the content of non-newtonian fluid calcium naphthenate is 0-70 weight %, non-newtonian fluid salicylic acid The content of calcium is 0-70 weight %, and the content of non-newtonian fluid calcium oleate is 0-70 weight %.

2. lubricant composition according to claim 1, wherein on the basis of the weight of the lubricant composition, base The content of plinth oil is 20-70 weight %, and the content of non-newtonian fluid sulfurized alkylphenol calcium is 20-65 weight %, non-newtonian fluid sulfonic acid The content of calcium is 0-50 weight %, and the content of non-newtonian fluid calcium naphthenate is 0-50 weight %, and non-newtonian fluid calcium salicylate contains Amount is 0-50 weight %, and the content of non-newtonian fluid calcium oleate is 0-50 weight %.

3. lubricant composition according to claim 1 or 2, wherein the thickening agent also optionally contains higher aliphatic Acid, aromatic acid, small molecule inorganic acid, the lithium salts of lower fatty acid, sodium salt, sylvite, calcium salt, strontium salt, barium salt, zirconates, aluminium salt and One of polyurea compound, bentonite and silica gel are a variety of.

4. lubricant composition according to claim 1 or 2, wherein the non-newtonian fluid sulfurized alkylphenol calcium is by ox Pause what body sulfurized alkylphenol calcium converted, the total base number of the non-newtonian fluid sulfurized alkylphenol calcium is 250-450mgKOH/g； The non-newtonian fluid sulfoacid calcium is converted by newton body sulfoacid calcium, and the total base number of the non-newtonian fluid sulfoacid calcium is 250- 450mgKOH/g；The non-newtonian fluid calcium naphthenate is converted by newton body calcium naphthenate, the non-newtonian fluid cycloalkanes The total base number of sour calcium is 250-450mgKOH/g；The non-newtonian fluid calcium salicylate is to convert to obtain by newton body calcium salicylate , the total base number of the non-newtonian fluid calcium salicylate is 250-450mgKOH/g；The non-newtonian fluid calcium oleate is by newton body What calcium oleate converted, the total base number of the non-newtonian fluid calcium oleate is 250-450mgKOH/g.

5. lubricant composition according to claim 3, wherein the higher fatty acids is the fat that carbon number is 8-20 Acid.

6. lubricant composition according to claim 3, wherein the higher fatty acids is the hydroxyl rouge that carbon number is 8-20 Fat acid.

7. lubricant composition according to claim 3, wherein the higher fatty acids is selected from lauric acid, palmitinic acid, hard At least one of resin acid, 12- hydroxy stearic acid, eicosyl carboxylic acid.

8. lubricant composition according to claim 3, wherein the aromatic acid is substituted or unsubstituted aromatic acid, is taken At least one of Dai Jiwei alkyl, alkenyl, alkynyl, aryl and halogenated alkyl or aryl, the molecular weight of the aromatic acid is less than Equal to 550.

9. lubricant composition according to claim 8, wherein the halogenated alkyl or aryl is the alkyl of perhalogeno Or aryl.

10. lubricant composition according to claim 8, wherein the aromatic acid is selected from unsubstituted or C₁-C₅Alkyl takes At least one of the phthalic acid in generation, M-phthalic acid, terephthalic acid (TPA), biphenyl dicarboxylic acid, multi-joint phthalic acid.

11. lubricant composition according to claim 3, wherein the small molecule inorganic acid and the lower fatty acid Molecular weight be less than or equal to 250.

12. lubricant composition according to claim 11, wherein the small molecule inorganic acid is selected from boric acid, phosphoric acid, sulphur At least one of acid, the lower fatty acid be selected from acetic acid, ethanedioic acid, propionic acid, malonic acid, butyric acid, succinic acid, adipic acid, At least one of azelaic acid, decanedioic acid.

13. lubricant composition according to claim 3, wherein the structural formula of the polyurea compound is

Wherein, n is 0-3 integer, R¹、R⁴It is alkyl, naphthenic base or aryl, R²It is alkylidene or arlydene, R³It is arlydene, Asia Alkyl or cycloalkylidene.

14. lubricant composition according to claim 13, wherein polyurea compound is two polyurea compounds, four polyureas At least one of compound, six polyurea compounds and eight polyurea compounds.

15. lubricant composition according to claim 13, wherein R¹、R⁴It is phenyl or substituted phenyl or carbon number is 8-24 alkyl or cycloalkyl；R²It is the alkylidene that phenylene or biphenylene or carbon number are 2-12；R³Be carbon number be 6-30 Arlydene, alkylidene or cycloalkylidene.

16. lubricant composition according to claim 15, wherein R¹、R⁴It is phenyl or C₁–C₃Alkyl or halogen The alkyl or cycloalkyl that substituted phenyl or carbon number is 10-18；R²It is the Asia that phenylene or biphenylene or carbon number are 2-8 Alkyl；R³It is With-(CH₂)₆At least one of.

17. the preparation method of lubricant composition described in any one of claim 1-16, this method comprises: by thickening agent It is uniformly mixed with part basis oil, is refined in 180-230 DEG C of constant temperature, surplus base oil is added, necessary additive is added, obtains Finished product, which is characterized in that the thickening agent contains non-newtonian fluid sulfurized alkylphenol calcium, and the thickening agent also optionally contains non-ox Pause one of body sulfoacid calcium, non-newtonian fluid calcium naphthenate, non-newtonian fluid calcium salicylate, non-newtonian fluid calcium oleate or a variety of.

18. a kind of preparation method of lubricant composition, which is characterized in that this method comprises:

(1) newton body sulfurized alkylphenol calcium, optional newton body and/or non-newtonian fluid sulfoacid calcium, optional newton body will be contained And/or non-newtonian fluid calcium naphthenate, optional newton body and/or non-newtonian fluid calcium salicylate and optional newton body and/or non- The high base number material and part basis oil of newton body calcium oleate mix, and obtain mixture；

(2) transforming agent is added, heats up to material retrogradation；

(3) heating dehydration；

(4) it is warming up to 180-230 DEG C of constant temperature refining, surplus base oil is added, necessary additive is added, obtains finished product；

On the basis of the weight of the lubricant composition, the content of base oil is 10-80 weight %, non-newtonian fluid alkyl monosulfide The content of phenol calcium is 10-70 weight %, and the content of non-newtonian fluid sulfoacid calcium is 0-70 weight %, and non-newtonian fluid calcium naphthenate contains Amount is 0-70 weight %, and the content of non-newtonian fluid calcium salicylate is 0-70 weight %, and the content of non-newtonian fluid calcium oleate is 0-70 Weight %.

19. preparation method according to claim 18, wherein optionally carry out lithium base before or after step (2) Or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium Base or one of compound zirconium, aluminium base or clad aluminum, polyurea compound or a variety of reactions, and/or be optionally added into bentonite and/ Or silica gel.

20. preparation method according to claim 19, wherein carry out before the step (2) lithium base or complex lithium, sodium base or Compound sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound strontium, barium base or compound barium, zirconium base or compound zirconium, aluminium base Or one of clad aluminum, polyurea compound or a variety of reactions, and/or bentonite and/or silica gel is added；Or, step (2) it It is preceding and carry out later lithium base or complex lithium, sodium base or compound sodium, potassium base or compound potassium, calcium base or composite calcium, strontium base or compound strontium, Barium base or compound barium, zirconium base or one of compound zirconium, aluminium base or clad aluminum, polyurea compound or a variety of reactions, and/or be added Bentonite and/or silica gel.

21. preparation method described in any one of 8-20 according to claim 1, wherein in step (2), at 50-80 DEG C, Be added needed for transforming agent reacted, after all transforming agents add, 80-100 DEG C constant temperature 60-90 minutes.

22. preparation method described in any one of 8-20 according to claim 1, wherein in step (3), be warming up to 100-130 DEG C dehydration.

23. preparation method described in any one of 8-20 according to claim 1, wherein in step (4), be warming up to 180-230 DEG C constant temperature 5-30 minutes, surplus base oil is added, is cooled to 100-120 DEG C to temperature, necessary additive is added, stirs, follow Ring filtering, homogenizing, degassing.

24. preparation method described in any one of 8-20 according to claim 1, wherein the newton body sulfurized alkylphenol calcium It is synthesis sulfurized alkylphenol calcium, the total base number of the newton body sulfurized alkylphenol calcium is 250-450mgKOH/g；The newton body Sulfoacid calcium is calcium mahogany sulfonate and/or calcium alkylbenzenesulfonate, and the total base number of the newton body sulfoacid calcium is 250-450mgKOH/g；Institute Stating newton body calcium naphthenate is petroleum naphthenic acid calcium and/or synthesis calcium naphthenate, and the total base number of the newton body calcium naphthenate is 250-450mgKOH/g；The newton body calcium salicylate is salicylate calcium, and the total base number of the newton body calcium salicylate is 250-450mgKOH/g；The newton body calcium oleate be natural calcium oleate and/or synthesis calcium oleate, the newton body calcium oleate Total base number is 250-450mgKOH/g.

25. preparation method described in any one of 8-20 according to claim 1, wherein the transforming agent is selected from fatty alcohol, rouge Fat acid, aliphatic ketone, fatty aldehyde, fatty amine, ether, calcium carbonate, boric acid, phosphonic acids, carbon dioxide, phenol, aromatic alcohol, aromatic amine, C₈- C₂₀Alkyl benzene sulphonate, aphthenic acids, C₁₆-C₂₄At least one of alkyl phenol and water, the additional amount of transforming agent are the high base number object Expect the 2-30% of total weight.

26. preparation method according to claim 25, wherein the transforming agent be selected from dodecyl benzene sulfonic acid, aphthenic acids, At least one of octadecyl phenol, methanol, isopropanol, butanol, boric acid, acetic acid and water, the additional amount of transforming agent are the height The 6-22% of base number material total weight.

27. lubricant composition made from the method as described in any one of claim 18-26.