CN111701284B - Defoaming agent and preparation method and application thereof - Google Patents
Defoaming agent and preparation method and application thereof Download PDFInfo
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- CN111701284B CN111701284B CN202010581939.7A CN202010581939A CN111701284B CN 111701284 B CN111701284 B CN 111701284B CN 202010581939 A CN202010581939 A CN 202010581939A CN 111701284 B CN111701284 B CN 111701284B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0413—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing N-atoms
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C11/00—Regeneration of pulp liquors or effluent waste waters
- D21C11/04—Regeneration of pulp liquors or effluent waste waters of alkali lye
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Abstract
The invention provides a defoaming agent and a preparation method and application thereof, belonging to the technical field of papermaking chemicals. The defoaming agent provided by the invention comprises the following components in parts by weight: 100-110 parts of silicon paste; 0.5-1 part of stearic acid diethanol amine; 5-8 parts of polyether modified silicone oil; 5-10 parts of a surfactant; 1-3 parts of a fat-soluble auxiliary agent; 0.5-3 parts of a stabilizing synergist; 200 portions and 250 portions of distilled water; based on the weight parts of the silicon paste, the silicon paste is prepared from the following raw materials: 100 parts of organic siloxane; 6-8 parts of silicon dioxide; 1-1.5 parts of a silane coupling agent; 0.3-0.5 part of coupling agent scavenger. The defoaming agent provided by the invention has high stability and defoaming and foam inhibiting performances. The examples show that the defoaming agent provided by the invention is used for defoaming for 3.2 seconds at 10cm, and is used for inhibiting foams for 7 minutes and 54 seconds, and the average dosage is 0.0264 kg/ton pulp.
Description
Technical Field
The invention relates to the technical field of papermaking chemicals, in particular to a defoaming agent and a preparation method and application thereof.
Background
The waste water from the alkaline (soda and sulphate) pulping process of the paper industry contains a large amount of lignin in a dark brown colour called black liquor. The black liquor is easy to foam, mainly because a large amount of organic lignin, especially pine wood, is dissolved in the cooking process, after cooking, because the content of turpentine saponification substances is high, the foaming is especially strong, the generated foam is fine, the alkalinity is strong, the temperature is high, and a defoaming agent is required to be added for defoaming in the recovery treatment, so that the air content in the pulp can be reduced, the cleaning effect is improved, the pulp hanging thickness of the net cage is increased, and the production efficiency is improved.
At present, the commonly used silicone antifoaming agent is generally prepared into an aqueous emulsion type product by emulsifying a compound of simethicone and silicon dioxide by using an emulsifying agent. The action mechanism of the organic silicon defoaming agent is that hydrophobic silicon dioxide is dispersed in dimethyl silicone oil, when the silicon dioxide is contacted with foaming liquid, the dimethyl silicone oil reduces the surface tension, and the silicon dioxide destroys and inhibits the generation of foam, thereby playing the roles of defoaming and inhibiting the foam. However, the papermaking black liquor has the characteristics of high viscosity, high temperature, strong alkalinity, fine bubbles and the like, and the defoaming and foam inhibiting effects of the common organic silicon defoaming agent are very slight, so that the using amount of the defoaming agent is increased during use, and the effect is poor.
Although the novel defoaming agent, such as that provided by patent CN107130459A, can achieve the purpose of quick defoaming and lasting foam inhibition in black liquor, the defoaming agent uses an inorganic acid catalyst, which can accelerate the damage of silicon dioxide to foam and inhibit the generation of foam, thereby improving the defoaming rate and foam inhibition time, but the main components of the inorganic acid catalyst are phosphorous acid and sulfuric acid, both of which have strong corrosivity and toxicity, which can not only damage human body, but also corrode reaction equipment, reduce the service life of the reaction equipment, increase production cost, increase production risk, and is not beneficial to industrial use.
Therefore, the problem to be solved is to provide the defoaming agent which can realize quick defoaming and lasting foam inhibition in the black liquor, and can not generate toxic action on human bodies and corrode equipment.
Disclosure of Invention
The invention aims to provide a defoaming agent, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a defoaming agent which comprises the following components in parts by weight:
100-110 parts of silicon paste;
0.5-1 part of stearic acid diethanol amine;
5-8 parts of polyether modified silicone oil;
5-10 parts of a surfactant;
1-3 parts of a fat-soluble auxiliary agent;
0.5-3 parts of a stabilizing synergist;
200-250 parts of distilled water;
based on the weight parts of the silicon paste, the silicon paste is prepared from the following raw materials:
100 parts of organic siloxane;
6-8 parts of silicon dioxide;
1-1.5 parts of a silane coupling agent;
and 0.3-0.5 part of coupling agent scavenging agent.
Preferably, the organosiloxane comprises dimethicone and hydroxy silicone oil.
Preferably, the mass ratio of the dimethyl silicone oil to the hydroxyl silicone oil is (1.5-2.4): 1.
the invention provides a preparation method of the silicon paste, which comprises the following steps:
mixing organic siloxane, silicon dioxide and a silane coupling agent, and carrying out coupling reaction to obtain a coupling reaction product; and adding a coupling agent remover into the coupling reaction product, and carrying out condensation reaction to obtain the silicon paste.
Preferably, the surfactant comprises one or more of an anionic surfactant, an amphoteric surfactant and a nonionic surfactant.
Preferably, the fat-soluble auxiliary agent comprises a mixture of one or more of fat-soluble fatty acid, animal fat and vegetable fat and C10-C30 fatty alcohol.
Preferably, the coupling agent scavenger comprises one or more of tert-butyl dimethyl monohydrosilane, dimethyl ethyl silane, dimethyl isopropyl silane, triisopropyl silane, trimethyl silane and tert-butyl dimethyl silanol.
Preferably, the stabilizing synergist comprises one or more of triphenylmonohydroxysilane, triphenylmethylsilane, triphenylethoxysilane, N-trimethylsilylacetamide, tribenzylsilane and dimethylmethoxy (3,3, 3-trifluoropropyl) silane.
The invention provides a preparation method of the defoaming agent in the technical scheme, which comprises the following steps:
mixing the silicon paste with stearic acid diethanol amine, polyether modified silicone oil, a surfactant, a fat-soluble auxiliary agent and a stabilizing synergist to obtain a primary mixture; and then mixing the primary mixture with distilled water at the temperature of 60-70 ℃ to obtain the defoaming agent.
The invention provides the application of the defoaming agent in the technical scheme or the defoaming agent prepared by the preparation method in the technical scheme in defoaming treatment of papermaking black liquor.
The invention provides a defoaming agent, which comprises the following components in parts by weight: 100-110 parts of silicon paste; 0.5-1 part of stearic acid diethanol amine; 5-8 parts of polyether modified silicone oil; 5-10 parts of a surfactant; 1-3 parts of a fat-soluble auxiliary agent; 0.5-3 parts of a stabilizing synergist; and distilled water 200 and 250 portions; based on the weight parts of the silicon paste, the silicon paste is prepared from the following raw materials: 100 parts of organic siloxane; 6-8 parts of silicon dioxide; 1-1.5 parts of a silane coupling agent; and 0.3-0.5 part of coupling agent scavenging agent. The silicon paste in the defoaming agent provided by the invention takes silicon dioxide as a raw material, can be fully dispersed and fused with organic siloxane, so that the silicon dioxide is not easy to precipitate, has stable property under alkaline conditions and is not easy to decompose, and the alkali resistance of the silicon dioxide is improved; the silane coupling agent is used as a raw material to play a bridging role, can improve the binding force between organic siloxane and silicon dioxide, enables the silicon dioxide not to be easily precipitated, has stable property under an alkaline condition, is not easily decomposed, is beneficial to improving the alkali resistance of the silicon dioxide, and further improves the using effect of the defoaming agent; the coupling agent remover can remove the residual silicon hydroxyl in the coupling agent reaction, so that the defoaming agent is not precipitated due to excessive crosslinking, and the problem that the defoaming agent is difficult to emulsify due to excessive crosslinking is avoided; the stabilizing synergist in the defoaming agent can ensure that the defoaming agent is stable, does not precipitate or crosslink in an emulsion state, and further improves the stability and defoaming and foam inhibiting performance of the defoaming agent; no inorganic acid catalyst is added, and the used raw materials have no corrosiveness and toxicity, do not produce toxic and harmful effects on human bodies, and do not corrode production equipment. The results of the examples show that the paper mill black liquor 100mL is used as foaming material, the circulation foaming is carried out by a bubbling machine, the foaming height is 20cm, 5 μ L of the defoaming agent provided by the invention is added, the time for eliminating the 10cm height foam is 3.2 seconds, and the foam inhibition time is 7 minutes and 54 seconds, which is superior to the commercial defoaming agent. The defoaming agent provided by the invention is applied to the actual pulp boiling production process of a paper mill, and particularly, the defoaming agent is added in the extraction and rinsing working section of the paper-making black liquor, and under the condition of equivalent defoaming and foam inhibition effects, the average dosage of the paper-making black liquor defoaming agent provided by the invention is 0.0264 kg/ton pulp, which is superior to that of the commercial defoaming agent.
Detailed Description
The invention provides a defoaming agent which comprises the following components in parts by weight:
100-110 parts of silicon paste;
0.5-1 part of stearic acid diethanol amine;
5-8 parts of polyether modified silicone oil;
5-10 parts of a surfactant;
1-3 parts of a fat-soluble auxiliary agent;
0.5-3 parts of a stabilizing synergist;
200-250 parts of distilled water;
based on the weight parts of the silicon paste, the silicon paste is prepared from the following raw materials:
100 parts of organic siloxane;
6-8 parts of silicon dioxide;
1-1.5 parts of a silane coupling agent;
and 0.3-0.5 part of coupling agent scavenging agent.
The defoaming agent provided by the invention comprises 100-110 parts by weight of silicon paste, preferably 105.5-108.5 parts by weight, more preferably 106-108 parts by weight, more preferably 106.5-107.5 parts by weight, and most preferably 107 parts by weight.
In the invention, the silicon paste is prepared from the following raw materials in parts by weight:
100 parts of organic siloxane;
6-8 parts of silicon dioxide;
1-1.5 parts of a silane coupling agent;
0.3-0.5 part of coupling agent scavenger.
The raw materials for preparing the silicon paste comprise 100 parts by weight of organic siloxane. In the present invention, the organosiloxane preferably includes dimethylsilicone oil and hydroxysilicone oil. In the invention, the mass ratio of the dimethyl silicone oil to the hydroxyl silicone oil in the organic siloxane is preferably (1.5-2.4): 1, more preferably (1.8 to 2.2): 1, most preferably (2.0-2.1): 1. according to the invention, the mass ratio of the dimethyl silicone oil to the hydroxyl silicone oil is limited within the range, and the silicon dioxide can be fully dispersed and fused with the organic siloxane, so that the silicon dioxide is not easy to precipitate, has stable properties under alkaline conditions, is not easy to decompose, and improves the alkali resistance of the silicon dioxide.
In the present invention, the dimethylsilicone oil preferably includes low-viscosity dimethylsilicone oil and high-viscosity dimethylsilicone oil; the viscosity of the low-viscosity dimethyl silicone oil is preferably 300-500 cst, and more preferably 350-450 cst; the viscosity of the high-viscosity dimethyl silicone oil is preferably 3000-10000 cst, and more preferably 5000-8000 cst. In the invention, the mass ratio of the low-viscosity dimethyl silicone oil to the high-viscosity dimethyl silicone oil in the dimethyl silicone oil is preferably (1.5-8.5): 1, more preferably (3-7): 1, most preferably (4-6): 1. the source of the dimethylsilicone fluid used in the present invention is not particularly limited, and commercially available dimethylsilicone fluids known to those skilled in the art may be used.
In the invention, the viscosity of the hydroxyl silicone oil is preferably 50-100000 cst, more preferably 10000-80000 cst, and most preferably 30000-60000 cst; the hydroxyl silicone oil is preferably hydroxyl terminated polysiloxane and/or dihydroxyl terminated polysiloxane; the hydroxyl content of the hydroxyl silicone oil is preferably 3-8%. The source of the hydroxyl silicone oil in the present invention is not particularly limited, and commercially available hydroxyl silicone oils known to those skilled in the art may be used. The viscosity of the dimethyl silicone oil and the hydroxyl silicone oil is limited in the range, the obtained defoaming agent is in an emulsion state, the viscosity is moderate, other dispersing agents and solvents are not required to be added for adjusting the viscosity, and the production cost is reduced.
The silicon paste is prepared from 6-8 parts of silicon dioxide, preferably 6.5-7.5 parts of silicon dioxide, and more preferably 7 parts of organic siloxane by mass of 100 parts of silicon dioxide. In the invention, the silicon dioxide can be fully dispersed and fused with the organic siloxane, so that the silicon dioxide is not easy to precipitate, has stable property under alkaline conditions and is not easy to decompose, and the alkali resistance of the silicon dioxide is improved. The source of the silica in the present invention is not particularly limited, and commercially available silica known to those skilled in the art may be used.
The raw materials for preparing the silicon paste comprise 1-1.5 parts, preferably 1.1-1.4 parts and more preferably 1.2-1.3 parts of silane coupling agent by taking the mass of the organic siloxane as 100 parts. In the present invention, the silane coupling agent preferably includes a silane coupling agent KH550 and/or KH 560. When the silane coupling agent comprises silane coupling agents KH550 and KH560, the adding proportion of the silane coupling agents KH550 and KH560 is not specially limited, and any adding proportion can be adopted; in the present invention, the silane coupling agents KH550 and KH560 are preferably added in a ratio of 1: 2-2: 1, more preferably 1: 1. in the invention, the silane coupling agent plays a bridging role in the process of preparing the silicon paste, can improve the binding force between organic siloxane and silicon dioxide, enables the silicon dioxide not to be easily precipitated, has stable property under alkaline conditions, is not easily decomposed, is beneficial to improving the alkali resistance of the silicon dioxide, and further improves the use effect of the defoaming agent. The source of the silane coupling agent in the present invention is not particularly limited, and commercially available silica known to those skilled in the art may be used.
The raw materials for preparing the silicon paste comprise 0.3-0.5 part of coupling agent remover, preferably 0.35-0.4 part of coupling agent remover, by taking the mass of the organic siloxane as 100 parts. In the invention, the coupling agent scavenger comprises one or more of tert-butyl dimethyl monohydrosilane, dimethyl ethyl silane, dimethyl isopropyl silane, triisopropyl silane, trimethyl silane and tert-butyl dimethyl silanol, and preferably dimethyl isopropyl silane and/or trimethyl silanol. According to the invention, silicon hydroxyl which is not completely reacted after the silane coupling agent is hydrolyzed can be eliminated through the coupling agent eliminating agent, so that the problem that the silane coupling agent is difficult to emulsify due to excessive crosslinking is avoided. The source of the coupling agent scavenger is not particularly limited in the present invention, and commercially available silica known to those skilled in the art may be used.
In the present invention, the method for preparing the silicon paste preferably includes the steps of:
mixing organic siloxane, silicon dioxide and a silane coupling agent, and carrying out coupling reaction to obtain a coupling reaction product; and adding a coupling agent remover into the coupling reaction product, and carrying out condensation reaction to obtain the silicon paste.
The apparatus used in the process of the present invention for producing the silicon paste is not particularly limited, and an apparatus known to those skilled in the art may be used.
In the invention, the organic siloxane and the silicon dioxide are preferably mixed to obtain a mixed product; and then mixing the mixed product with a silane coupling agent for coupling reaction to obtain a coupling reaction product.
In the invention, the mixing temperature of the organic siloxane and the silicon dioxide is preferably 80-110 ℃, and the mixing time of the organic siloxane and the silicon dioxide is preferably 1-2 h. In the present invention, the mixing of the organosiloxane and silica is preferably carried out under stirring conditions; the stirring speed is preferably 60-120 rpm, more preferably 80-100 rpm, and most preferably 90 rpm. According to the invention, by adopting the mixing mode, in the mixing process, the silicon dioxide and the organic siloxane can be fully dispersed and fused, so that the silicon dioxide is not easy to precipitate, has stable property under an alkaline condition and is not easy to decompose, the alkali resistance of the silicon dioxide is improved, and then the silane coupling agent is added for coupling reaction, so that the silicon oil and the silicon dioxide are better combined, and the defoaming and foam inhibiting effects are improved.
In the invention, the organic siloxane is preferably heated before being mixed with the silicon dioxide, and the heating temperature is preferably 50-60 ℃, more preferably 52-58 ℃, and most preferably 55 ℃.
After obtaining the mixed product, the invention preferably mixes the mixed product with a silane coupling agent to perform a coupling reaction to obtain a coupling reaction product. In the present invention, the coupling reaction is preferably carried out under stirring conditions; the stirring speed is preferably 60-120 rpm, more preferably 80-100 rpm, and most preferably 90 rpm. In the invention, the temperature of the coupling reaction is preferably 80-110 ℃, more preferably 90-105 ℃, and most preferably 95-100 ℃; the time of the coupling reaction is preferably 0.5-1.5 h, and more preferably 1 h.
After the coupling reaction product is obtained, the invention preferably adds the coupling agent remover under the stirring condition to carry out condensation reaction to obtain the silicon paste. In the invention, the condensation reaction temperature is preferably 80-110 ℃, more preferably 90-105 ℃, and most preferably 95-100 ℃; the time of the condensation reaction is preferably 1h to 1.5h, and more preferably 1.2 h; the stirring speed is preferably 60-120 rpm, more preferably 80-100 rpm, and most preferably 90 rpm. The invention eliminates active silicon hydroxyl by adding a coupling agent elimination agent, thereby ensuring the stability of the product.
According to the invention, the silicon paste is preferably cooled after being obtained; the cooling end point temperature is preferably 50-70 ℃, more preferably 55-65 ℃, and most preferably 60 ℃. The manner of cooling and the rate of cooling are not particularly limited in the present invention and may be by any cooling scheme known in the art.
The defoaming agent provided by the invention comprises 0.5-1 part of stearic acid diethanol amine, preferably 0.6-0.9 part, and more preferably 0.7-0.8 part by mass of silicon paste of 100-110 parts. The source of the stearic acid diethanolamine is not particularly limited in the present invention, and commercially available stearic acid diethanolamine known to those skilled in the art may be used. In the invention, the stearic acid diethanol amine can play a role in assisting in breaking bubbles.
The defoaming agent provided by the invention comprises 5-8 parts of polyether modified silicone oil, preferably 6-7.5 parts, and more preferably 7 parts by mass of silicon paste of 100-110 parts. The polyether modified silicone oil of the present invention is not particularly limited in kind or type, and may be one known to those skilled in the art. In the embodiment of the invention, polyether modified silicone oil with Dow Corning brand OFX-0190 model is specifically adopted. In the invention, the polyether modified silicone oil can improve the foam inhibition effect of the defoaming agent.
The defoaming agent provided by the invention comprises 5-10 parts of surfactant, preferably 6-9 parts, more preferably 6.5-8.5 parts, and most preferably 8 parts by mass of silicon paste of 100-110 parts. In the present invention, the surfactant preferably includes one or more of an anionic surfactant, an amphoteric surfactant and a nonionic surfactant, and more preferably a mixture of an anionic surfactant, an amphoteric surfactant and a nonionic surfactant. In the invention, the mass ratio of the anionic surfactant, the amphoteric surfactant and the nonionic surfactant in the surfactant is preferably (0.5-1): (0.5-1): (4-7), more preferably (0.6-0.9): (0.6-0.9): (4.5-6.5), most preferably (0.7-0.8): (0.7-0.8): (5-6).
The kind of the anionic surfactant is not particularly limited in the present invention, and anionic surfactants known to those skilled in the art may be used. In the present invention, the anionic surfactant is preferably sodium di-sec-octyl maleate sulfonate (fast penetrant T). In the present invention, the anionic surfactant contributes to increase the defoaming speed of the defoaming agent.
The amphoteric surfactant used in the present invention is not particularly limited in kind, and those known to those skilled in the art can be used. In the present invention, the amphoteric surfactant is preferably lecithin. In the invention, the amphoteric surfactant can assist the fusion of all components in the papermaking black liquor defoamer, so that all components are not easy to stratify, and the use effect of the defoamer is favorably improved.
The type of the nonionic surfactant is not particularly limited in the present invention, and nonionic surfactants known to those skilled in the art may be used. In the present invention, the nonionic surfactant is preferably a polyether nonionic surfactant, and more preferably a mixture of fatty alcohol-polyoxyethylene ether and fatty alcohol-polyoxypropylene ether. In the invention, the mass ratio of the fatty alcohol-polyoxyethylene ether to the fatty alcohol-polyoxypropylene ether is preferably (2-3): (2-4), more preferably (2.2-2.8): (2.5-3.5), most preferably 2.5: 3.
the types of the fatty alcohol-polyoxyethylene ether and the fatty alcohol-polyoxypropylene ether are not particularly limited, and the fatty alcohol-polyoxyethylene ether and the fatty alcohol-polyoxypropylene ether which are well known to those skilled in the art can be used. In the invention, the fatty alcohol-polyoxyethylene ether is preferably isomeric dodecyl alcohol-polyoxyethylene ether. In the present invention, the fatty alcohol polyoxypropylene ether is preferably cetostearyl alcohol polyoxypropylene ether. In the invention, the nonionic surfactant can assist the fusion of all components in the defoaming agent, so that all components are not easy to layer, and the use effect of the defoaming agent is improved; and meanwhile, the foam inhibition effect of the defoaming agent can be improved.
The defoaming agent provided by the invention comprises 1-3 parts of fat-soluble auxiliary agent, preferably 1.5-2.5 parts, more preferably 2.0-2.4 parts, and most preferably 2.2 parts by mass of silicon paste of 100-110 parts. In the invention, the fat-soluble auxiliary agent preferably comprises a mixture of one or more of fat-soluble fatty acid, animal fat and vegetable fat and C10-C30 fatty alcohol. In the fat-soluble auxiliary agent, the mass ratio of the C10-C30 fatty alcohol to other components is preferably (2-4): (1-2), more preferably (2.5-3.5): (1.2 to 1.8), most preferably 3: (1.4-1.6). In the invention, the fat-soluble auxiliary agent can form an oil film on the surface of the papermaking black liquor, and plays a role in assisting in breaking bubbles; in addition, the fatty alcohol of C10-C30 in the fat-soluble auxiliary agent can aggregate small foams in the black paper-making liquid, so that the black paper-making liquid is degassed in the black paper-making liquid, and the foam breaking is assisted.
The invention has no special limitation on the types of the fat-soluble fatty acid, the animal fat and the vegetable fat, and can be prepared by adopting the fat-soluble fatty acid, the animal fat and the vegetable fat which are well known by the technical personnel in the field; in an embodiment of the present invention, the fat soluble auxiliary is preferably oleic acid. In the present invention, the fatty alcohol of C10 to C30 is preferably a fatty alcohol of C10 to C18, and more preferably a fatty alcohol of C12 to C14.
The defoaming agent provided by the invention comprises 0.5-3 parts of stabilizing synergist by mass of 100-110 parts of silicon paste, preferably 1.0-2.8 parts of stabilizing synergist, and more preferably 1.5-2.0 parts of stabilizing synergist. In the invention, the stabilizing synergist comprises one or more of triphenylmonohydrosilane, triphenylmethylsilane, triphenylethoxysilane, N-trimethylsilylacetamide, tribenzylsilane and dimethylmethoxy (3,3, 3-trifluoropropyl) silane. In the invention, the stabilizing synergist is beneficial to further improving the stability of the defoamer emulsion, so that the defoamer emulsion is not precipitated and demulsified due to crosslinking, the defoaming and foam inhibiting effects are improved, and the using effect of the papermaking black liquor defoamer is improved.
The invention provides a preparation method of the defoaming agent in the technical scheme, which comprises the following steps:
mixing the silicon paste with stearic acid diethanol amine, polyether modified silicone oil, a surfactant, a fat-soluble auxiliary agent and a stabilizing synergist to obtain a primary mixture; and then mixing the primary mixture with distilled water at the temperature of 60-70 ℃ to obtain the defoaming agent.
The silicon paste is mixed with stearic acid diethanol amine, polyether modified silicone oil, a surfactant, a fat-soluble auxiliary agent and a stabilizing synergist to obtain a primary mixture. In the invention, the silicon paste is mixed with stearic acid diethanol amine, polyether modified silicone oil, surfactant, fat-soluble auxiliary agent and stabilizing synergist preferably under the condition of stirring; the stirring speed is preferably 60-120 rpm, more preferably 80-100 rpm, and most preferably 90 rpm; the stirring time is preferably 1-3 h, and more preferably 2 h.
The mixing sequence of the silicon paste, the stearic acid diethanol amine, the polyether modified silicone oil, the surfactant, the fat-soluble auxiliary agent and the stabilizing synergist is not specially limited, and any mixing sequence can be adopted.
After the primary mixture is obtained, the primary mixture is mixed with distilled water at the temperature of 60-70 ℃ to obtain the defoaming agent. In the present invention, the temperature of mixing the primary mixture with distilled water is preferably 65 ℃. In the present invention, the mixing of the primary mixture with distilled water is preferably performed under stirring conditions; the stirring speed is preferably 60-120 rpm, more preferably 80-110 rpm, and most preferably 100 rpm; the stirring time is preferably 1-2 h, and more preferably 1.5 h.
The invention provides application of the defoaming agent in the technical scheme or the defoaming agent prepared by the preparation method in the technical scheme in defoaming treatment of papermaking black liquor. The application mode of the defoaming agent in the defoaming treatment of the papermaking black liquor is not particularly limited, and the application mode known by the technical personnel in the field can be adopted. In the invention, preferably, during the pulp boiling production process of a paper mill, a defoaming agent is added in the extraction and rinsing section of the paper-making black liquor to realize defoaming treatment of the paper-making black liquor.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Heating 100 parts of organic siloxane (including 50 parts of dimethyl silicone oil with the viscosity of 350-450 cst, 15 parts of dimethyl silicone oil with the viscosity of 5000-8000 cst and 35 parts of hydroxyl silicone oil with the viscosity of 30000 cst) to 50 ℃, mixing with 6 parts of silicon dioxide and 5601 parts of silane coupling agent under the stirring of 60rpm, continuously heating to 100 ℃, and carrying out coupling reaction for 2 hours to obtain a coupling reaction product;
(2) mixing the coupling reaction product obtained in the step (1) with 0.3 part of coupling agent remover (dimethyl ethyl silane) under stirring of 60rpm, carrying out condensation reaction for 1.5h at 100 ℃, and cooling to 55 ℃ to obtain 107.3 parts of silicon paste;
(3) mixing 107.3 parts of the silicon paste obtained in the step (2) with 1 part of stearic diethanol amine, 6 parts of polyether modified silicone oil (Dow Corning brand OFX-0190 type), 9 parts of surfactant (comprising 5 parts of cetostearyl alcohol polyoxypropylene ether and 4 parts of isomeric decyl alcohol polyoxyethylene ether), 3 parts of fat-soluble auxiliary agent (comprising 1 part of oleic acid and 2 parts of fatty alcohol of C20-C26) and 1.5 parts of stabilizing synergist (N-trimethylsilyl acetamide) for the first time, and stirring for 1.5 hours at 60rpm to obtain a first mixture;
(4) and (4) adjusting the temperature of the primary mixture in the step (3) to 60 ℃, adding 200 parts of distilled water for secondary mixing, and stirring at 60rpm for 1.5 hours to obtain the defoaming agent.
Example 2
(1) Heating 100 parts of organosiloxane (comprising 45 parts of dimethyl silicone oil with the viscosity of 350-500 cst, 25 parts of dimethyl silicone oil with the viscosity of 5000-6000 cst and 30 parts of hydroxyl silicone oil with the viscosity of 10000 cst) to 50 ℃, mixing with 7 parts of silicon dioxide and 7 parts of silane coupling agent KH5501.5 under stirring at 60rpm, continuously heating to 110 ℃, and carrying out coupling reaction for 1 hour to obtain a coupling reaction product;
(2) mixing the coupling reaction product obtained in the step (1) with 0.4 part of coupling agent remover (trimethylsilanol) under stirring at 100rpm, carrying out condensation reaction for 0.5h at 110 ℃, and cooling to 65 ℃ to obtain 108.9 parts of silicon paste;
(3) mixing 108.9 parts of the silicon paste obtained in the step (2) with 0.5 part of stearic diethanol amine, 8 parts of polyether modified silicone oil (Dow Corning brand OFX-0190 type), 8 parts of surfactant (comprising 0.5 part of rapid penetrating agent T, 0.5 part of lecithin, 4 parts of cetostearyl alcohol polyoxypropylene ether and 3 parts of isomeric lauryl alcohol polyoxyethylene ether), 1 part of fat-soluble auxiliary agent (fatty alcohol of C12-C18) and 2.5 parts of stabilizing synergist (dimethyl methoxyl (3,3, 3-trifluoropropyl)) for the first time, and stirring for 0.5h at 100rpm to obtain a first mixture;
(4) and (4) adjusting the temperature of the primary mixture in the step (3) to 70 ℃, adding 240 parts of distilled water for secondary mixing, and stirring at 100rpm for 1h to obtain the defoaming agent.
Example 3
(1) Heating 100 parts of organic siloxane (including 55 parts of dimethyl silicone oil with the viscosity of 350-450 cst, 5 parts of dimethyl silicone oil with the viscosity of 5000-8000 cst and 40 parts of hydroxyl silicone oil with the viscosity of 50000 cst) to 50 ℃, mixing with 8 parts of silicon dioxide and 8 parts of silane coupling agent KH5601.5 under stirring at 60rpm, continuously heating to 100 ℃, and carrying out coupling reaction for 2 hours to obtain a coupling reaction product;
(2) mixing the coupling reaction product obtained in the step (1) with 0.5 part of coupling agent remover (triisopropylsilane) under the stirring of 120rpm, carrying out condensation reaction for 1.5h at the temperature of 100 ℃, and cooling to 55 ℃ to obtain 110 parts of silicon paste;
(3) mixing 110 parts of silicon paste obtained in the step (2) with 1 part of stearic acid diethanol amine, 8 parts of polyether modified silicone oil (Dow Corning brand OFX-0190 type), 10 parts of surfactant (comprising 0.5 part of rapid penetrating agent T, 0.5 part of lecithin, 5 parts of cetostearyl alcohol polyoxypropylene ether and 4 parts of isomeric decyl alcohol polyoxyethylene ether), 2 parts of fat-soluble auxiliary agent (comprising 1 part of oleic acid and 1 part of fatty alcohol of C20-C26) and 1.0 part of stable synergist (triphenyl monohydrogen silane) for the first time, and stirring for 1 hour at 120rpm to obtain a first mixture;
(4) and (4) adjusting the temperature of the primary mixture in the step (3) to 70 ℃, adding 250 parts of distilled water for secondary mixing, and stirring at 120rpm for 1.5 hours to obtain the defoaming agent.
Comparative example 1
Amazon 5865 antifoaming agent
Comparative example 2
Amazon 5814 defoaming
Comparative example 3
Patent CN107130459A example 4 provides an antifoaming agent
The performance of the papermaking black liquor defoamer prepared in the embodiments 1 to 3 of the invention is tested, and compared with the commercial defoamer product, the results are shown in table 1, and the specific steps are as follows:
the method comprises the steps of taking 100mL of paper mill black liquor as a foaming substance, circularly foaming by a bubbling machine, wherein the foaming height is 20cm, adding 5 μ L of defoaming agent (the defoaming agent is the paper mill black liquor defoaming agent, the Amazon 5865 defoaming agent and the Amazon 5814 defoaming agent in the embodiments 1-3 of the invention and the defoaming agent provided in the embodiment 4 of the patent CN107130459A respectively), and recording the time for eliminating 10 cm-height foam and the foam inhibition time of the defoaming agent.
TABLE 1 comparison of the Performance of inventive examples 1-3 with comparative examples 1-3
In order to further verify the use effect of the defoaming agent, the defoaming agent in example 3 and comparative examples 1 to 3 is applied to the actual pulp boiling production process of a paper mill, specifically, the defoaming agent is added in the extraction and rinsing section of the paper making black liquor, and under the condition of equivalent defoaming and foam inhibition effects, the average dosage of the defoaming agent (kg/ton pulp, mass of the defoaming agent consumed for producing 1 ton pulp) is recorded. The results show that example 3 of the present invention provides an average amount of the defoaming agent of 0.0264 kg/ton of pulp, while the defoaming agent of comparative example 1 provides an average amount of 0.0417 kg/ton of pulp, the defoaming agent of comparative example 2 provides an average amount of 0.0353 kg/ton of pulp, and the defoaming agent of comparative example 3 provides an average amount of 0.03283 kg/ton of pulp, with comparable defoaming and foam suppressing effects.
The test results show that the defoaming agent provided by the invention has the advantages of quick defoaming, lasting foam inhibition and small using amount when defoaming treatment is carried out on the papermaking black liquor, and is superior to commercial defoaming agents.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. The defoaming agent is prepared from the following components in parts by weight:
100-110 parts of silicon paste;
0.5-1 part of stearic acid diethanol amine;
5-8 parts of polyether modified silicone oil;
5-10 parts of a surfactant;
1-3 parts of a fat-soluble auxiliary agent;
0.5-3 parts of a stabilizing synergist;
200-250 parts of distilled water;
based on the weight parts of the silicon paste, the silicon paste is prepared from the following raw materials:
100 parts of organic siloxane;
6-8 parts of silicon dioxide;
1-1.5 parts of a silane coupling agent;
and 0.3-0.5 part of coupling agent scavenger;
the coupling agent scavenger comprises one or more of tert-butyl dimethyl monohydrogen silane, dimethyl ethyl silane, dimethyl isopropyl silane, triisopropyl silane, trimethyl silanol and tert-butyl dimethyl silanol.
2. The defoamer of claim 1, wherein said organosiloxane comprises dimethicone and hydroxy silicone oil.
3. The antifoaming agent according to claim 2, wherein the mass ratio of the dimethyl silicone oil to the hydroxyl silicone oil is (1.5-2.4): 1.
4. the defoamer according to claim 1, wherein the preparation method of the silicon paste comprises the following steps:
mixing organic siloxane, silicon dioxide and a silane coupling agent, and carrying out coupling reaction to obtain a coupling reaction product; and adding a coupling agent remover into the coupling reaction product, and carrying out condensation reaction to obtain the silicon paste.
5. The defoamer of claim 1, wherein the surfactant comprises one or more of an anionic surfactant, an amphoteric surfactant, and a nonionic surfactant.
6. The antifoaming agent according to claim 1, wherein the fat-soluble auxiliary comprises a mixture of one or more of fat-soluble fatty acid, animal fat and vegetable fat and fatty alcohol of C10-C30.
7. The defoamer of claim 1, wherein said stabilizer synergist comprises one or more of triphenylmonohydroxysilane, triphenylmethylsilane, triphenylethoxysilane, N-trimethylsilylacetamide, tribenzylsilane, and dimethylmethoxy (3,3, 3-trifluoropropyl) silane.
8. A method for preparing the defoaming agent according to any one of claims 1 to 7, comprising the steps of:
mixing the silicon paste with stearic acid diethanol amine, polyether modified silicone oil, a surfactant, a fat-soluble auxiliary agent and a stabilizing synergist to obtain a primary mixture; and then mixing the primary mixture with distilled water at the temperature of 60-70 ℃ to obtain the defoaming agent.
9. The use of the defoaming agent according to any one of claims 1 to 7 or the defoaming agent prepared by the preparation method according to claim 8 in defoaming treatment of papermaking black liquor.
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