CN1037854C - Fluidity improver for crude oil containing wax - Google Patents
Fluidity improver for crude oil containing wax Download PDFInfo
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- CN1037854C CN1037854C CN90105871A CN90105871A CN1037854C CN 1037854 C CN1037854 C CN 1037854C CN 90105871 A CN90105871 A CN 90105871A CN 90105871 A CN90105871 A CN 90105871A CN 1037854 C CN1037854 C CN 1037854C
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- crude oil
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Abstract
The present invention relates to a fluidity improver for crude oil containing wax, which is mainly compounded from a polymer containing acrylic ester or methacrylic ester, a copolymer of the acrylic ester and methacrylic ester, and a surfactant. The present invention can be used for the exploitation, the storage and pipeline systems of crude oil containing wax and, crude oil containing large content of wax (achieving 34%), and crude oil containing water. The present invention has the advantages of little dosage (in general, the dosage is from 20 to 1000 ppm), low cost, wide application range, evident reduction of pour point, viscosity and wax deposition of crude oil containing wax and favorable stability on shearing, standing and repeated heating. When the fluidity improver of the present invention is filled into an oil transporting pipeline, the present invention can realize normal temperature transportation, saves a large quantity of energy sources for country, reduces environment pollution and has obvious economic benefit and social benefit.
Description
The invention belongs to the polymer manufacture field of waxy crude oil, and relate to their preparation and application as the waxy crude oil fluidity improver with fluidity improver.
Owing to contain a large amount of paraffin in the waxy crude oil, when crude oil temperature is reduced to wax precipitation piont, paraffin begins to separate out, continue cooling, paraffin will interconnect, and form three-dimensional net structure, and this structure makes the flowing property variation of crude oil, cause very big difficulty to pipe-line transportation, and in tubing system, storage vessel and oil tanker cabin, generate precipitation of paraffin.It significantly reduces Oil extraction, storage and transport capacity, when serious, cause line clogging and forces to produce or carry and stop.
In order to prevent that paraffin from depositing in Oil extraction, storage and conveying, people once adopted several different methods to handle to waxy crude oil: remove a part of paraffin as solvent extration, can reduce the pour point of waxy crude oil, but solvent recuperation, the removal of wax needs chilling unit, and is wasteful; Also useful light oil dilution method, this method limitation is very big, and only limiting to has existing low pour crude oil available place at those; Also have a kind of heating to carry and the insulation storing method, this method complex process, the consumption of Ministry Of Fuel And Power power is big, and the consumption of oil fuel is up to being transferred 5% of crude oil, and crude oil can not get perfect combustion and contaminate environment.Crude oil heat treating process, this method need crude oil is carried out dynamic and static thermal treatment in advance, and shortcoming is that poor stability, investment are big.
In recent years, in crude oil, add specific polymers, can make the depression of pour point of crude oil, while can also prevent deposition of wax on the one hand.Mainly be that this polymeric additive has changed the wax-crystal structure of separating out, thereby the flowing property of crude oil is improved.Make the improvement of flowing property in the whole processes such as the conveying of waxy crude oil from the oil well to the refinery, storage, and prevent deposition of wax.English Patent G.B2082604 (1981) provides the application of the multipolymer of a kind of positive alkyl acrylate and toxilic acid and derivative thereof as the waxy crude oil crystallization inhibitor, can reduce the pour point of crude oil, viscosity, but the viscosity reduction does not see that implementation result is arranged; U.S. EXXON oil company, CONO CO oil company also have some products to come out.Yet, find that in actual applications many known product all have some limitation and shortcoming.For example, many products can not generally be used for all crude oil; May be invalid to some crude oil.A lot of products have extremely sensitive to shearing, crystallization inhibitor as waxy crude oil, can only just can not play one's part to the full through under the condition of any shearing, in fact, crude oil is normally realized carrying by pump, the influence of the shearing force that applies by pump, completely destroy the effect of many crystallization inhibitors, use is restricted.There is the shortcoming that leaves standstill and repeat to be subjected to poor heat stability in addition.
The purpose of this invention is to provide a kind of waxy crude oil fluidity improver, it has, and cost is low, and consumption is few, and is widely applicable, and the pour point, viscosity and the precipitation of paraffin that reduce waxy crude oil are significantly arranged, and to shearing, leave standstill and repeat to be subjected to Heat stability is good.
Waxy crude oil provided by the invention with the recipe ingredient (by weight) of fluidity improver is:
Polyacrylic ester 1-6 part
Acrylate copolymer 1-5 part
Ethylene-vinyl acetate copolymer 1-6 part
Tensio-active agent (available non-ionic type or anionic and composition thereof, HLB value are 1-40) 1-3 part
The chemical structural formula of the multipolymer of polyacrylic ester and acrylate is:
R
1Be a H atom or a methyl
R
2It is the normal chain alkyl of 6～18 carbon atoms
R
3Be vinylbenzene, maleic anhydride, ethylene vinyl acetate, propenoic acid beta-lignocaine ethyl ester, methacrylic acid β-lignocaine ethyl ester.
N is polymerization degree 33-371
The waxy crude oil provided by the invention manufacture method of fluidity improver:
1. the preparation of acrylate or methacrylic ester
Acrylic or methacrylic acid is carried out esterification with alcohol, acid is 4: 1～1.1: 1 with the ratio (mol ratio) of alcohol, at sulfuric acid or tosic acid as catalyzer, consumption is 1/200～1/20 of an alcohol, with Resorcinol as stopper, consumption is 1/400～1/50 of acid, temperature of reaction is 80～160 ℃ under normal pressure, reaction times is 1.2～1.5 hours, till the water that reaction is deviate from reaches theoretical value, (removing unreacted acid) need do not washed, be distilled to the acrylate or the methacrylate monomer of this method preparation, can directly carry out polyreaction.
2. the preparation of the polymkeric substance of acrylate or methacrylic ester and multipolymer.
Polyreaction can adopt mass polymerization or solution polymerization process; the solvent of solution polymerization can be used benzene toluene xylylene diacetate ethyl ester and kerosene; monomer is 1: 9～1: 1 with the ratio (by weight) of solvent, and initiator can be with dibenzoyl peroxide or Diisopropyl azodicarboxylate, and consumption is monomeric 0.2%～1%; under normal pressure under protection of inert gas; temperature of reaction is 70～90 ℃, and time 3-4 hour, the number-average molecular weight that makes polymkeric substance was 10; 000～100,000.
The preparation method of co-polymer is identical with homopolymer, comonomer can be used vinylbenzene, maleic anhydride, ethylene vinyl acetate, propenoic acid beta-lignocaine ethyl ester and methacrylic acid β-lignocaine ethyl ester, one or more mixture, acrylate or methacrylic ester are 1 with the ratio of comonomer: 0.2-1: 0.6 (mol ratio).
3. the waxy crude oil preparation of fluidity improver
Recipe ingredient by above-mentioned fluidity improver takes by weighing polyacrylic ester 1-6 part, the copolymer 1 of acrylate-5 part, have in the mixing vessel of agitator and heating unit the addings of ethylene-vinyl acetate copolymer 1-6 part and tensio-active agent 1-3 part, under agitation be warming up to 90-110 ℃, continue to stir 1.5 hours, treat that mixing of materials evenly after, cooling, packing, standby.
Waxy crude oil provided by the invention is mainly used in the exploitation of waxy crude oil and the high content of wax (reaching 34%) crude oil and wet oil with fluidity improver, oil tank store and pipe-line transportation system in, generally working concentration is 20-1000ppm, optimum amount is 50-300ppm.
The present invention has following advantage:
1. the used starting material of the present invention are based on domesticly, with short production cycle, and all under normal pressure, temperature is the highest 150 ℃ for whole process, and not high to equipment requirements, technical process is simple, no aftertreatment and three-waste pollution problem.
2. fluidity improver of the present invention, active high, addition is few, and 100ppm can make the pour point of Central Plains, triumph and Qinghai crude oil descend 20 ℃, and viscosity reduces more than 93.5%, yield value reduces by 100%, widely applicable, anti-shearing, dynamically, static and repeat to be subjected to Heat stability is good, Qinghai crude oil is sheared 12 round the clock continuously, its viscosity, pour point do not have rise, also slightly descend, viscosity, pour point do not have rise yet round the clock to leave standstill 7.Its performance index have surpassed the U.S. C-8361 of EXXON oil company, C-8806 and the TLF of Conoco oil company pour point depressant level.
3. the crude oil in China long distance pipeline all adopts the method that heating is carried and insulation stores, this method complex process, transporting resistance is big, burning and power consumption are big, are used to heat about 600,000 tons of the crude oil that conveying burns every year, and power consumption reaches 1,700,000,000 degree, if being added oil pipeline, fluidity improver of the present invention can realize the normal temperature conveying, also reduce pollution simultaneously, can save a large amount of energy, economic benefit and social benefit are significantly arranged for country to environment
4. adopt fluidity improver of the present invention also to can be used for Oil extraction and storage, prevent precipitation of paraffin, improve crude production rate.
Embodiment
1. by the above-mentioned method for preparing waxy crude oil with fluidity improver, stearyl alcohol 270 grams are added in the reactor, add hydroquinone of polymerization retarder 0.75 gram again, acrylic or methacrylic acid 72.72 grams, add catalyzer tosic acid 2.7 grams at last, 150 ℃ of reactions of heating, dehydration under normal pressure, react after 2 hours, 98% water of nearly theoretical amount is deviate from.Need not to reclaim excessive acrylic or methacrylic acid and solvent, can directly carry out polymerization or copolyreaction.
2. with in acrylate or methacrylic ester 25 grams and the toluene 50 gram adding polymerization reaction kettles; under nitrogen protection under normal pressure, add initiator Diisopropyl azodicarboxylate 0.125 gram, 80 ℃ of temperature; reacted 3 hours, the homopolymer that makes acrylate or methacrylic ester is standby.
3. with in acrylate or methacrylic ester 16.2 grams and the propenoic acid beta-lignocaine ethyl ester 0.62 gram adding polymerization reaction kettle; add toluene 40 grams again; under nitrogen protection under normal pressure; add initiator Diisopropyl azodicarboxylate 0.032 gram; 80 ℃ of temperature; reacted 4 hours, the multipolymer that makes acrylate or methacrylic ester and propenoic acid beta-lignocaine ethyl ester is standby.
4. with in acrylate or methacrylic ester 11 grams and the vinyl acetate 13 gram adding polymerization reaction kettles, add toluene 34 grams again, under nitrogen protection under normal pressure, add Diisopropyl azodicarboxylate 0.24 gram, 75 ℃ of temperature were reacted 3 hours, and it is standby to make co-polymer.
5. with acrylate or methacrylic ester 16.2 grams and vinylbenzene 2.6 grams; add in the polymerization reaction kettle; add vinyl acetic monomer 19 grams, under nitrogen protection under normal pressure, add dibenzoyl peroxide 0.1050 gram, 85 ℃ of temperature, reaction 4 hours, it is standby to make multipolymer.
6. with in acrylate or methacrylic ester 15 grams and the maleic anhydride 2.254 gram adding polymerization reaction kettles, add toluene 35 grams, under nitrogen protection under normal pressure, add 85 ℃ of dibenzoyl peroxide 0.117 gram, temperature, reacted 4 hours, it is standby to make multipolymer.
7. the waxy crude oil preparation of fluidity improver
Take by weighing homopolymer 400 grams of acrylate or methacrylic ester by the recipe ingredient of above-mentioned fluidity improver, acrylate copolymer (contain in the multipolymer that embodiment 3 to 6 makes one or more mixture) 200 grams, ethylene-vinyl acetate copolymer 100 grams, surfactivity (available OP-7,10,15, SP-169, the mixture of one or more of nonionic such as Span-80 or anionic) 200 grams, adding has in the mixing vessel of agitator and heating unit successively, and under agitation heat temperature raising continues to stir 1-1.5 hour to 90-110 ℃, after treating that mixing of materials is evenly, cooling, packing, standby.
Waxy crude oil of the present invention carries out the situation of application test to the crude oil in the different places of production of China with fluidity improver:
One, the test character of crude oil
| Central plain oil | Shengli crude | Qinghai crude oil | Daqing crude oil | Renqiu crude oil | |
| Density (gram per centimeter 2) | 0.8487 | 0.9002 | 0.8420 | 0.8604 | 0.8947 |
| Pour point (℃) | 32 | 30.5 | 33.5 | 33 | 36.5 |
| Wax content (%) | 22.25 | 16.79 | 33.41 | 35.70 | 28.53 |
| Colloid+asphalt content (%) | 5.71 | 16.79 | 5.37 | 8.09 | 13.78 |
| Wax precipitation piont (℃) | 56.4 | 55.80 | 57 | ||
| Yield value (Pa) | 46.4 | 126.4 | 22.99 |
Two, test method and effect
A certain amount of crude oil added have in stirring, the heating container, under agitation heat temperature raising to 70 ℃ adds fluidity improver of the present invention, and constant temperature 15 minutes is cooled to 60 ℃, 2 ℃/minute of cooling rates by 70 ℃; 60 ℃ are cooled to 25 ℃ again, 0.5 ℃/minute of cooling rate, and by such processing, the performance of measuring crude oil is as follows:
This fluidity improver of table 1 is to the influence of Central Plains crude oil fluidity
| Addition (ppm) | Zero pour (℃) | Depression of the freezing point amplitude (℃) | 20 ℃ of viscosity (mpas), 20s -1 | Viscosity reduced rate (%) | Yield value reduced rate (%) |
| 0 | 30 | 485.4 | |||
| 50 | 11.5 | 18.5 | 15.4 | 96.8 | 100 |
| 100 | 7.5 | 22.5 | 11.9 | 97.5 | 100 |
This fluidity improver of table 2. is to the influence of Shengli crude flowability
| Additive (ppm) | Zero pour (℃) | Depression of the freezing point amplitude (℃) | Viscosity mpas (20 ℃, 20s -1) | Viscosity reduced rate (%) | Yield value reduced rate (%) |
| 0 | 30.5 | 4935.2 | |||
| 50 | 12.5 | 18 | 250.6 | 94.9 | 100 |
| 100 | 11.5 | 19 | 320.6 | 95.2 | 100 |
This fluidity improver of table 3. is to the influence of Qinghai crude oil fluidity
| Additive (ppm) | Zero pour (℃) | Depression of the freezing point amplitude (℃) | Viscosity mpas (20 ℃, 20s -1) | Rate at the bottom of the viscosity drop (%) | Yield value hangs down rate (%) |
| 0 | 33.5 | 1949 | |||
| 100 | 14.5 | 19 | 126.7 | 93.5 | 100 |
This fluidity improver of table 4. is to the influence of Daqing crude oil zero pour
| Addition (ppm) | Zero pour (℃) | Depression of the freezing point amplitude (℃) |
| 0 | 33 | |
| 100 | 16 | 17 |
| 200 | 13 | 20 |
| 300 | 12 | 21 |
This fluidity improver of table 5. is to the influence of the former oil freezing point of Renqiu
| Addition (ppm) | Zero pour (℃) | Depression of the freezing point amplitude (℃) | Viscosity mpas (20 ℃, 20s -1) | Viscosity reduced rate (%) |
| 0 | 36 | 14764 | ||
| 300 | 15 | 21 | 741.3 | 95 |
This fluidity improver of table 6. is to the influence of triumph octahedral river viscosity of crude
| Addition (ppm) | Viscosity mpas (30 ℃, 3.17s -1) | Viscosity reduced rate (%) |
| 0 | 5804.5 | |
| 200 | 3625.58 | 37.5 |
This fluidity improver of table 7. is to the influence of Central Plains pasty state pour point of crude oils
| Addition (ppm) | Pour point (℃) | The depression of pour point amplitude (℃) |
| 0 | 39 | |
| 300 | 15 | 24 |
Claims (5)
1. waxy crude oil fluidity improver is characterized in that the recipe ingredient (parts by weights meter) of this improving agent is:
Polyacrylic ester 1-6 part
Acrylate copolymer 1-5 part
Ethylene-vinyl acetate copolymer 1-6 part
Tensio-active agent 1-3 part
2. according to the described waxy crude oil fluidity improver of claim 1, it is characterized in that the chemical structural formula of described polyacrylic ester of this properties-correcting agent or acrylate copolymer is:
R
1Be a H atom or a methyl
R
2Normal chain alkyl for 6-18 carbon atom
R
3Be vinylbenzene, maleic anhydride, ethylene-vinyl acetate, propenoic acid beta-lignocaine ethyl ester, methacrylic acid β-lignocaine ethyl ester.
N is polymerization degree 33-371.
3. according to claim 1 or 2 described waxy crude oil stream fluidity improver, it is characterized in that described tensio-active agent is non-ionic type or anionic and composition thereof, the HLB value is 1-40.
4. according to the manufacture method of the described waxy crude oil of claim 1, it is characterized in that with fluidity improver:
(1) preparation of acrylate or methacrylic ester
Acrylic or methacrylic acid is carried out esterification with alcohol, and acid is 4: 1～1.1: 1 with the ratio (mol ratio) of alcohol; As catalyzer, consumption is 1/200～1/20 of an alcohol at sulfuric acid or tosic acid, and as stopper, consumption be sour 1/400～1/50 with Resorcinol.Temperature of reaction is 80-160 ℃ under normal pressure, and the reaction times is 1.2～1.5 hours, till the water that reaction is deviate from reaches theoretical value.The acrylate or the methacrylate monomer of this method preparation need not washed, distill and be removed unreacted acid, can directly carry out polyreaction.
(2) preparation of the polymkeric substance of acrylate or methacrylic ester and multipolymer
Polyreaction can adopt mass polymerization or solution polymerization process; the solvent of solution polymerization can be used benzene, toluene, dimethylbenzene; vinyl acetic monomer and kerosene; monomer is 1: 9～1: 1 with the ratio of solvent, and initiator can be with dibenzoyl peroxide or Diisopropyl azodicarboxylate, and consumption is monomeric 0.2%-1%; under normal pressure under protection of inert gas; temperature of reaction is 70-90 ℃, and time 3-4 hour, the number-average molecular weight that makes polymkeric substance was 10000-100000.
The preparation method of multipolymer is identical with homopolymer, and comonomer can be used vinylbenzene, maleic anhydride, ethylene vinyl acetate, propenoic acid beta-lignocaine ethyl ester, methacrylic acid β-lignocaine ethyl ester.One or more mixture, acrylate or methacrylic ester are 1: 0.2～1: 0.6 mol ratio with the ratio of comonomer.
(3) the waxy crude oil preparation of fluidity improver
Recipe ingredient by above-mentioned fluidity improver takes by weighing polyacrylic ester 1-6 part, the copolymer 1 of acrylate-5 part, have in the mixing vessel of agitator and heating unit the addings of ethylene-vinyl acetate copolymer 1-6 part and tensio-active agent 1-3 part, under agitation be warming up to 90-110 ℃, continue to stir 1.5 hours, treat that mixing of materials evenly after, cooling, packing, standby.
5. according to the purposes of the described waxy crude oil of claim 1 with fluidity improver, it is characterized in that described improving agent can be used for the exploitation that waxy crude oil and the high content of wax reach 34% crude oil and wet oil, in oil tank storage and the pipe-line transportation system, general working concentration is 20-1000ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90105871A CN1037854C (en) | 1990-08-18 | 1990-08-18 | Fluidity improver for crude oil containing wax |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN90105871A CN1037854C (en) | 1990-08-18 | 1990-08-18 | Fluidity improver for crude oil containing wax |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1059157A CN1059157A (en) | 1992-03-04 |
| CN1037854C true CN1037854C (en) | 1998-03-25 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN90105871A Expired - Fee Related CN1037854C (en) | 1990-08-18 | 1990-08-18 | Fluidity improver for crude oil containing wax |
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| Country | Link |
|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11193053B2 (en) | 2017-04-13 | 2021-12-07 | Bl Technologies, Inc. | Wax inhibitors for oil compositions and methods of using wax inhibitors to reduce wax deposition from oil |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100372878C (en) * | 2005-11-11 | 2008-03-05 | 山东大学 | Preparation method of high coagulation high viscosity crude petroleum producing and conveying agent |
| JP5038650B2 (en) * | 2006-04-21 | 2012-10-03 | 東邦化学工業株式会社 | Fluidity improver for crude oil |
| CN101386659B (en) * | 2008-11-05 | 2010-09-15 | 中国海洋石油总公司 | Method for preparing oil soluble crude oil improved flowable agent |
| CN102020982B (en) * | 2009-09-17 | 2012-04-18 | 成都川大金钟科技有限公司 | Multiple-effect viscosity reducer for thickened oil recovery |
| CN102191093A (en) * | 2010-03-10 | 2011-09-21 | 中国石油天然气股份有限公司 | Preparation method of diesel oil low-temperature flow property improver |
| CN106047329B (en) * | 2016-06-06 | 2020-03-06 | 中国石油化工股份有限公司 | High-temperature-resistant pour point depressant and preparation method thereof |
| CN106336480B (en) * | 2016-08-23 | 2018-07-06 | 中国石油化工股份有限公司 | For improving the additive of high-content wax viscous crude low temperature fluidity |
| CN110105942B (en) * | 2018-02-01 | 2021-09-28 | 中国石油天然气股份有限公司 | Wax remover and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85103463A (en) * | 1985-05-11 | 1986-11-05 | 丁杰 | The freeze proof emulsion that contains the polyvinyl acetal product |
| EP0344644A2 (en) * | 1988-05-31 | 1989-12-06 | Röhm Gmbh | Mineral oil with a modified flow rate |
-
1990
- 1990-08-18 CN CN90105871A patent/CN1037854C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85103463A (en) * | 1985-05-11 | 1986-11-05 | 丁杰 | The freeze proof emulsion that contains the polyvinyl acetal product |
| EP0344644A2 (en) * | 1988-05-31 | 1989-12-06 | Röhm Gmbh | Mineral oil with a modified flow rate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11193053B2 (en) | 2017-04-13 | 2021-12-07 | Bl Technologies, Inc. | Wax inhibitors for oil compositions and methods of using wax inhibitors to reduce wax deposition from oil |
| US11261369B2 (en) | 2017-04-13 | 2022-03-01 | Bl Technologies, Inc. | Maleic anhydride copolymer with broadly dispersed ester side chain as wax inhibitor and wax crystallization enhancer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1059157A (en) | 1992-03-04 |
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