CN114146455B - Defoaming composition - Google Patents
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- CN114146455B CN114146455B CN202111095860.4A CN202111095860A CN114146455B CN 114146455 B CN114146455 B CN 114146455B CN 202111095860 A CN202111095860 A CN 202111095860A CN 114146455 B CN114146455 B CN 114146455B
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- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
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Abstract
The invention introduces a defoaming composition with acrylate polymer as an active substance, which has excellent defoaming performance and good compatibility in a foaming system; the defoaming composition is synthesized by a solution polymerization method, and the specific preparation method comprises the following steps: 1) Preparing a polymer X by using a methyl/acrylic acid alkyl ester (alkyl number is 1-8) monomer A and/or methyl/acrylic acid hydroxyalkyl ester B, an organic solvent S and an initiator I according to a solution polymerization method known in the industry; 2) Preparing a polymer Y by using a methyl/acrylic acid alkyl ester (the alkyl number is 9-18) monomer D and/or an olefin monomer O, an organic solvent S and an initiator I according to a solution polymerization method known in the industry; 3) Preparing a polymer Z from all monomers used by the polymer X and the polymer Y, a cross-linking agent monomer C, hydrophobic particles K, an organic solvent S and an initiator I according to a solution polymerization method known in the industry; 4) The polymer X, Y, Z was uniformly mixed by a shearing apparatus to obtain a defoaming composition.
Description
Technical Field
The invention belongs to the technical field of fine chemical preparations, relates to a fine chemical preparation, in particular to a defoaming composition, and more particularly relates to a defoaming composition taking an acrylic ester polymer as a main active substance and application of the defoaming composition in a system rich in anionic surfactants, such as papermaking, water treatment, textile industry and the like.
Background
Defoamers are compositions used in industrial production to control foam in various processes. In industrial production, especially in the industries of papermaking, water treatment, textile and the like, various chemical auxiliary agents are added into a water system due to specific requirements, and foam formation is extremely easy to be caused along with large mechanical energy, such as stirring, washing, thickening processes and the like. Liquid media (e.g., water), chemical aids (e.g., surfactants), air sources, and mechanical energy are the primary sources of foam generation in industrial processes.
Defoamers have been developed to eliminate unwanted foam generated in industrial production. The defoamers are classified into two categories according to active ingredients, namely, non-silicon defoamers and organic silicon defoamers, wherein the common non-silicon defoamers take mineral oil, polyether, amide or fatty alcohol as active substances, and the organic silicon defoamers take polyorganosiloxane as active substances.
The defoamer introduced in the patent CN102120106A consists of mineral oil, polyol stearate, white carbon black and an emulsifier, and has good defoaming performance in the industries of papermaking and water-based paint. The defoamer introduced in the patent CN104069653A consists of mineral oil, fatty acid/fatty acid metal soap, fatty acid amide, tributyl citrate, octanol, triethanolamine and an emulsifier, and is widely used in the fields of ink production, paint production, sewage treatment and latex production. The defoamer referred in the above patent belongs to mineral oil defoamer, namely, mineral oil defoamer using mineral oil as carrier, and the mineral oil hydrocarbon oil substances can generate tetrachlorodibenzo-p-dioxin (TCDD) harmful substances when encountering high temperature, which causes harm to the environment and human health, and has insufficient capability of inhibiting foam in a system rich in anionic surfactant.
Alkylimides as the main active substance of mineral oil defoamers, usually EBS, other diamides or mixtures of diamides can also be used in such defoamers. Patent application CN101362063a describes a defoamer consisting of vegetable oil, EBS and other types of amides, mainly for textile printing industry. An antifoaming agent for water treatment introduced in patent CN102976429B mainly consists of EBS, liquid paraffin, engine oil, kerosene, simethicone and white carbon black. In the use process, EBS in the mineral oil defoamer is easier to deposit due to stronger hydrophobicity, thereby influencing the production efficiency and the product quality.
The patent CN102343165a improves the foam eliminating and inhibiting performance, dispersibility and compatibility by mixing a silicone grease mixture as an active substance with a polyether silicone oil emulsifier and the like. The patent CN107638718A improves the high-temperature stability of emulsion through polysiloxane silicone grease and ethoxyalkynol emulsifier, the polysiloxane silicone grease improves the compatibility of products, and the emulsifier with a gemini structure improves the compatibility of the emulsifier and a water phase. The defoamers described in the above patents all adopt silicone grease as defoaming active substances, however, due to the characteristics of the silicone grease, the silicone grease can be gradually precipitated in the use process of the defoamer, and under the condition that the defoamer accumulates for a long time, the silicone grease can be precipitated in a large amount, so that on one hand, the product quality can be influenced, and on the other hand, the silicone grease can be deposited on equipment to be difficult to clean and even cause equipment blockage. Thus, although silicone grease is generally considered to have the characteristics of rapid defoaming and long-lasting foam inhibition, the use of silicone grease-containing defoamer products is avoided in many industrial processes.
Thus, there is an increasing need for defoamers that do not contain hydrocarbon oils, EBS, or silicone grease. Patent 101045880 discloses a defoaming agent compounded by high molecular block polyether, fatty alcohol and solvent, wherein the high molecular block polyether is polyethylene glycol with molecular weight of 10000-20000, the high molecular block polyether is a block copolymer of ethylene oxide and propylene oxide as an initiator, the fatty alcohol is isooctyl alcohol, and the solvent is ethanol and water. The defoamer does not contain any silicon element, does not affect the downstream hydrogenation process and the quality of final light oil products, but has the defects of insufficient active components, slow permeation and diffusion in a tower, large addition amount, higher cost than the organosilicon defoamer, poor high temperature resistance and low defoaming efficiency at high temperature. . Patent CN102126763a describes a defoamer consisting of polyether and lower alcohols, mainly for garbage permeate treatment. The above patent does not use mineral oil, avoids the damage of mineral oil to the environment, but the defoaming performance of the non-silicon defoamer taking polyether or fatty alcohol as a main active substance in a system rich in anionic surfactant is not satisfactory, and the capability of inhibiting foam cannot meet the industrial production requirement. So researchers improve on the one hand on the basis of the existing type of defoamer to alleviate the problems, and on the other hand, develop a novel defoamer to fundamentally solve the problems, and the acrylic defoamer is a research hot spot.
Patent US5152925a describes an antifoaming agent with an acrylic resin as the main antifoaming active substance, wherein the acrylic polymer is mainly an acrylic resin prepared from an acrylic monomer containing hydroxyl groups in diisodecyl phthalate (DIDP) as the organic diluent, and is used for brown stock washing and other papermaking processes. The patent CN102428142B also mentions that an acrylic ester polymer is used as a main active substance to prepare a defoaming agent, wherein the acrylic ester polymer is prepared from monomers such as isooctyl acrylate, hydroxyalkyl acrylate, acrylic acid and the like in an organic diluent diisooctyl adipate (DIOA), the prepared acrylic ester polymer is used as a main active ingredient of the defoaming agent, and is compounded with defoaming aids such as white carbon black and alkyl silicone oil, and the defoaming agent is applied to industries such as petroleum industry, water treatment, pigment and coating, food and beverage processing, mining industry, textile industry, agriculture and papermaking and the like. The appearance of the defoamer can solve the problems of environmental injury and silicon precipitation residue, but the defoaming performance of the defoamer prepared by the prior art still has a great improvement space. Therefore, it would be of great importance to improve the foam inhibition performance of acrylate polymer defoamers.
Disclosure of Invention
The invention discloses an antifoaming composition with acrylate polymer as main active substance, which has excellent defoaming performance in a foaming system and good compatibility. The defoaming composition is synthesized by a solution polymerization method, and the specific preparation method comprises the following steps: 1) Preparing a polymer X by using a methyl/alkyl acrylate (alkyl number 1-8) monomer A and/or methyl/hydroxyalkyl acrylate B, an organic solvent S and an initiator I according to a solution polymerization method well known in the industry; 2) Preparing a polymer Y by using a methyl/acrylic acid alkyl ester (the alkyl number is 9-18) monomer D and/or an olefin monomer O, an organic solvent S and an initiator I according to a solution polymerization method known in the industry; 3) Preparing a polymer Z from all monomers used by the polymer X and the polymer Y, a cross-linking agent monomer C, hydrophobic particles K, an organic solvent S and an initiator I according to a solution polymerization method known in the industry; 4) The polymer X, Y, Z was uniformly mixed by a shearing apparatus to obtain a polymer defoamer composition P. The polymer X obtained by singly polymerizing or mixing and copolymerizing methyl/acrylic acid alkyl ester A and methyl/acrylic acid hydroxyalkyl ester B serving as monomers has lower glass transition temperature and lower molecular weight and mainly plays roles of rapid spreading and rapid dispersion; the polymer Y obtained by singly polymerizing or mixing and copolymerizing methyl/acrylic acid alkyl ester D and olefin O serving as monomers has proper molecular weight and mainly plays a role in inhibiting bubbles; the polymer Z obtained by mixing and copolymerizing all monomers used by the polymer X and the polymer Y and the crosslinking monomer C has the function of solvent by containing the structures of the polymer X and the polymer Y at the same time so as to fully mix the polymer X and the polymer Y, and has the function of foam inhibition by the network structure of macromolecules.
The invention aims at realizing the following technical scheme:
a defoaming composition comprises a methyl/acrylic acid alkyl ester (the alkyl number is 1-8), a methyl/acrylic acid hydroxyalkyl ester monomer B, a methyl/acrylic acid alkyl ester (the alkyl number is 9-18), an olefin monomer O, a cross-linking agent monomer C, an organic solvent S, hydrophobic particles K and an initiator I; the amount of the methyl/acrylic acid alkyl ester (the alkyl number is 1-8) monomer A accounts for 10-25% of the total mass of the defoamer composition, the amount of the methyl/acrylic acid hydroxyalkyl ester monomer B accounts for 5-15% of the total mass of the defoamer composition, the amount of the methyl/acrylic acid alkyl ester (the alkyl number is 9-18) monomer D accounts for 10-25% of the total mass of the defoamer composition, the amount of the olefin monomer O accounts for 0.5-5% of the total mass of the defoamer composition, the amount of the cross-linking agent monomer C accounts for 0.5-5% of the total mass of the defoamer composition, the amount of the organic solvent S accounts for 30-60% of the total mass of the defoamer composition, the amount of the hydrophobic particles K accounts for 1-8% of the total mass of the defoamer composition, and the amount of the initiator I accounts for 0.1-1% of the total mass of the defoamer composition.
Preferably, the amount of the methyl/acrylic acid alkyl ester (the alkyl number is 1-8) monomer A accounts for 15-20% of the total mass of the defoamer composition, the amount of the methyl/acrylic acid hydroxyalkyl ester monomer B accounts for 8-12% of the total mass of the defoamer composition, the amount of the methyl/acrylic acid alkyl ester (the alkyl number is 9-18) monomer D accounts for 15-20% of the total mass of the defoamer composition, the amount of the olefin monomer O accounts for 2-4% of the total mass of the defoamer composition, the amount of the cross-linking agent monomer C accounts for 2-4% of the total mass of the defoamer composition, the amount of the organic solvent S accounts for 40-50% of the total mass of the defoamer composition, the amount of the hydrophobic particles K accounts for 3-6% of the total mass of the defoamer composition, and the amount of the initiator I accounts for 0.4-0.8% of the total mass of the defoamer composition.
The preparation method of the defoaming composition provided by the invention comprises the following steps:
1) Preparing a polymer X by using a methyl/alkyl acrylate (alkyl number 1-8) monomer A and/or methyl/hydroxyalkyl acrylate B, an organic solvent S and an initiator I according to a solution polymerization method well known in the industry;
2) Preparing a polymer Y by using a methyl/acrylic acid alkyl ester (the alkyl number is 9-18) monomer D and/or an olefin monomer O, an organic solvent S and an initiator I according to a solution polymerization method known in the industry;
3) Preparing a polymer Z from all monomers used by the polymer X and the polymer Y, a cross-linking agent monomer C, hydrophobic particles K, an organic solvent S and an initiator I according to a solution polymerization method known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the defoaming composition P
A. Methyl/acrylic acid alkyl ester (alkyl number 1-8) monomer
The methyl/alkyl acrylate (alkyl number 1-8) monomer can be used singly or in a plurality of mixed mode; selected from the group consisting of acrylic esters, methacrylic esters, and in particular, but not limited to, methyl acrylate, ethyl acrylate, butyl acrylate, isooctyl acrylate, methyl methacrylate, ethyl methacrylate, butyl methacrylate, isooctyl methacrylate.
Preferably, the methyl/alkyl acrylate (alkyl number 1-8) monomer is butyl acrylate, isooctyl acrylate or isooctyl methacrylate.
B. Hydroxyalkyl methacrylate monomers
The hydroxyalkyl methacrylate monomer may be used singly or in combination of plural ones; selected from hydroxyalkyl acrylates, hydroxyalkyl methacrylates, specifically but not limited to hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate.
Preferably, the methyl/acrylic acid hydroxyalkyl ester monomer is hydroxyethyl acrylate or hydroxypropyl acrylate.
D. Methyl/acrylic acid alkyl ester (alkyl number 9-18) monomer
The methyl/alkyl acrylate (the alkyl number is 9-18) monomer can be used singly or in a plurality of mixed mode; selected from alkyl acrylates, alkyl methacrylates, specifically but not limited to dodecyl acrylate, stearyl acrylate, dodecyl methacrylate, stearyl methacrylate.
Preferably, the methyl/alkyl acrylate (the alkyl number is 9-18) monomer is dodecyl methacrylate or octadecyl methacrylate.
O, olefin monomer
The olefin monomer is any one or a mixture of a plurality of linear alpha-olefins, alpha-aromatic olefins or branched alpha-olefins, and comprises alpha-octene, alpha-decene, alpha-dodecene, alpha-tetradecene, alpha-hexadecene, alpha-octadecene, alpha-eicosene, C20-C24 linear alpha-olefin mixture, C24-C28 linear alpha-olefin mixture, alpha-triacontene, alpha-methylstyrene and alpha-styrene, which can be used singly or in any proportion.
Preferably, the olefin monomer is alpha-dodecene, alpha-tetradecene, alpha-hexadecene, alpha-octadecene, alpha-methyl styrene, alpha-styrene.
C. Crosslinking agent monomer
The cross-linking agent monomer refers to a monomer which contains at least two or more vinyl groups in one molecule and can form a polymer soluble in an organic solvent; selected from allyl methacrylate, polyol methacrylate (ethylene glycol dimethacrylate, diethylene glycol dimethacrylate, 1, 3-butylene glycol dimethacrylate), divinylbenzene, double-end vinyl end-capped polysiloxane, tetra-vinyl tetramethyl cyclotetrasiloxane and vinyl MQ silicone resin, can be used singly or mixed in any proportion.
Preferably, the cross-linking agent monomer is allyl methacrylate, ethylene glycol dimethacrylate, double-end vinyl end-capped polysiloxane, vinyl MQ silicon resin.
I. Initiator(s)
Examples of free radical generating initiators useful in the present invention are selected from, but not limited to, 2' -azobis (2-methylpropanenitrile), 2' -azobis (2, 4-dimethylvaleronitrile), 2' -azobis (2-methylbutanenitrile), benzoyl peroxide; preferably, the initiator is benzoyl peroxide.
S, organic solvent
Examples of suitable organic solvents for use in the present invention may be selected from, but are not limited to, diisodecyl phthalate, diisooctyl adipate, diisooctyl phthalate, dioctyl adipate, 2-ethyl-1-hexanol, isooctyl alcohol, polyethylene glycol, polypropylene glycol, polytetramethylene glycol, liquid polybutene, liquid polyisobutene, fatty alcohol polyoxyethylene ether, polyether esters, polyether amines, alone or in combination; preferably, the organic solvent is polypropylene glycol or fatty alcohol polyoxyethylene ether.
K. Hydrophobic particles
The hydrophobic particles are inorganic hydrophobic particles, and specific examples are, but not limited to, fatty acid magnesium salt, fatty acid calcium salt, fatty acid aluminum salt, fatty acid zinc salt, particle polyisobutene, particle polymethacrylic acid resin, particle polyacrylic acid resin, particle organic silicon resin and white carbon black, and can be used singly or in a mixed mode; preferably, the hydrophobic particles are particle polyisobutene, particle polymethacrylic acid resin, particle polyacrylic acid resin, particle organic silicon resin and white carbon black.
The defoamer composition provided by the invention is applied to defoaming and foam inhibition in a system rich in anionic surfactant, such as defoaming and foam inhibition in industries of papermaking, water treatment, textile and the like.
Detailed Description
Example 1
1) 5g of butyl acrylate, 15g of polypropylene glycol and 0.03g of benzoyl peroxide are taken, and polymer X is prepared according to a solution polymerization method well known in the industry;
2) 12g of dodecyl acrylate, stearyl acrylate, 20g of polypropylene glycol and 0.03g of benzoyl peroxide are taken, and polymer Y is prepared according to a solution polymerization method well known in the industry;
3) Polymer Z was prepared by solution polymerization methods well known in the industry from 5g of butyl acrylate, 12g of dodecyl and stearyl acrylate, 5g of a double-ended vinyl-terminated polysiloxane, 6.9g of a particulate polyisobutylene, 19g of polypropylene glycol, and 0.04g of benzoyl peroxide;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 2
1) 12.5g of isooctyl acrylate, 16g of isooctyl alcohol and 0.33g of 2,2' -azobis (2-methylbutyronitrile) are taken and used for preparing a polymer X according to a solution polymerization method known in the industry;
2) 9g of octadecyl acrylate, 16g of isooctyl alcohol and 0.33g of 2,2' -azobis (2-methylbutyronitrile) are taken, and polymer Y is prepared according to a solution polymerization method well known in the industry;
3) 12.5g of isooctyl acrylate, 9g of stearyl acrylate, 3g of diethylene glycol dimethacrylate, 5g of granular polymethacrylic resin, 16g of isooctyl alcohol and 0.34g of 2,2' -azobis (2-methylbutyronitrile) are taken, and a polymer Z is prepared according to a solution polymerization method well known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 3
1) 12.5g of isooctyl methacrylate, 15g of polyethylene glycol and 0.33g of 2,2' -azobis (2-methylpropanenitrile) are taken and used for preparing a polymer X according to a solution polymerization method known in the industry;
2) 2.5g of alpha-dodecene, 25g of polyethylene glycol and 0.33g of 2,2' -azobis (2-methylpropanenitrile) are taken and used for preparing a polymer Y according to a solution polymerization method known in the industry;
3) 12.5g of isooctyl methacrylate, 2.5g of alpha-dodecene, 4.9g of divinylbenzene, 4.1g of particulate polymethacrylic resin, 20g of polyethylene glycol and 0.34g of 2,2' -azobis (2-methylpropanenitrile) are taken and used for preparing a polymer Z according to a solution polymerization method well known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 4
1) 10.5g of methyl acrylate, 20g of polytetramethylene glycol and 0.33g of 2,2' -azobis (2, 4-dimethyl valeronitrile) are taken and used for preparing a polymer X according to a solution polymerization method well known in the industry;
2) 2.5g of alpha-tetradecene, 20g of polytetramethylene glycol and 0.33g of 2,2' -azobis (2, 4-dimethyl valeronitrile) are taken, and polymer Y is prepared according to a solution polymerization method well known in the industry;
3) 10.5g of methyl acrylate, 2.5g of alpha-tetradecene, 5g of 1, 3-butanediol dimethacrylate, 8g of granular polyacrylic resin, 20g of polytetramethylene glycol and 0.34g of 2,2' -azobis (2, 4-dimethyl valeronitrile) are taken and prepared into a polymer Z according to a solution polymerization method known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 5
1) 2.5g of hydroxyethyl acrylate, 19g of 2-ethyl-1-hexanol, 0.26g of 2,2 '-azobis (2-methylpropanenitrile) and 2,2' -azobis (2-methylbutanenitrile) were taken and polymer X was prepared according to the solution polymerization method known in the industry;
2) Polymer Y was prepared by solution polymerization methods well known in the industry from 12.5g of stearyl acrylate and methacrylate, 19.6g of polypropylene glycol, and 0.26g of 2,2' -azobis (2-methylpropanenitrile);
3) 2.5g of hydroxyethyl acrylate, 12.5g of stearyl acrylate and stearyl methacrylate, 3.6g of vinyl MQ silicone resin, 8g of granular polyacrylic resin, 19g of polypropylene glycol and 0.28g of 2,2' -azobis (2-methylbutyronitrile) are taken, and polymer Z is prepared according to a solution polymerization method known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 6
1) 7.5g of hydroxypropyl acrylate, 19.4g of fatty alcohol polyoxyethylene ether and 0.3g of benzoyl peroxide are taken, and polymer X is prepared according to a solution polymerization method well known in the industry;
2) 7.8g of lauryl methacrylate, 2.5g of alpha-hexadecene, 15.4g of fatty alcohol polyoxyethylene ether and 0.3g of 2,2' -azobis (2, 4-dimethyl valeronitrile) are taken, and polymer Y is prepared according to a solution polymerization method well known in the industry;
3) 7.5g of hydroxypropyl acrylate, 7.8g of dodecyl methacrylate, 2.5g of alpha-hexadecene, 3.3g of ethylene glycol dimethacrylate, 8g of white carbon black, 17.4g of fatty alcohol polyoxyethylene ether and 0.3g of benzoyl peroxide are taken, and a polymer Z is prepared according to a solution polymerization method well known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 7
1) 7.5g of butyl methacrylate, 4g of hydroxypropyl acrylate, 19g of diisodecyl phthalate and 0.2g of 2,2' -azobis (2-methylpropanenitrile) are taken and used for preparing a polymer X according to a solution polymerization method known in the industry;
2) 2.3g of alpha-styrene, 10g of stearyl methacrylate, 16g of diisodecyl phthalate and 0.2g of 2,2' -azobis (2-methylpropanenitrile) are taken and used for preparing a polymer Y according to a solution polymerization method known in the industry;
3) 7.5g of butyl methacrylate, 4g of hydroxypropyl acrylate, 2.3g of alpha-styrene, 5g of stearyl methacrylate, 1.8g of allyl methacrylate, 3g of granular polyacrylic resin and white carbon black, 17g of diisodecyl phthalate and 0.2g of 2,2' -azobis (2-methylpropanenitrile) are taken and used for preparing a polymer Z according to a solution polymerization method well known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 8
1) 9g of butyl acrylate, 6g of hydroxyethyl methacrylate and hydroxypropyl methacrylate, 17.7. 17.7 g diisooctyl adipate and 0.3g of 2,2' -azobis (2, 4-dimethylvaleronitrile) are taken and prepared into a polymer X according to a solution polymerization method well known in the industry;
2) 2.6g of alpha-octene, 17.7. 17.7 g of diisooctyl adipate and 0.3g of 2,2' -azobis (2, 4-dimethylvaleronitrile) are taken and prepared into a polymer Y according to a solution polymerization method known in the industry;
3) 9g of butyl acrylate, 6g of hydroxyethyl methacrylate and hydroxypropyl methacrylate, 2.6g of alpha-octene, 4.8g of tetravinyl tetramethyl cyclotetrasiloxane, 6g of granular polyacrylic resin and white carbon black, 17.7. 17.7 g diisooctyl adipate and 0.3g of 2,2' -azobis (2, 4-dimethyl valeronitrile) are taken and prepared into a polymer Z according to a solution polymerization method well known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 9
1) 12.5g of isooctyl acrylate and isooctyl methacrylate, 4g of hydroxyethyl acrylate, 8g of diisooctyl phthalate, 0.2g of 2,2 '-azobis (2-methylpropanenitrile) and 2,2' -azobis (2-methylbutanenitrile) are taken and the polymer X is prepared according to the solution polymerization method known in the industry;
2) Polymer Y was prepared by solution polymerization methods known in the industry from 12.5g of stearyl acrylate and lauryl methacrylate, 12g of diisooctyl phthalate, 0.2g of 2,2 '-azobis (2-methylpropanenitrile) and 2,2' -azobis (2-methylbutanenitrile);
3) Polymer Z was prepared by solution polymerization methods well known in the industry from 12.5g of isooctyl acrylate and isooctyl methacrylate, 4g of hydroxyethyl acrylate, 12.5g of a mixture of stearyl acrylate and dodecyl methacrylate, 4.4g of allyl methacrylate and ethylene glycol dimethacrylate, 7g of magnesium fatty acid, 10g of diisooctyl phthalate, 0.2g of 2,2 '-azobis (2-methylpropanenitrile) and 2,2' -azobis (2-methylbutanenitrile);
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 10
1) Polymer X was prepared by solution polymerization methods known in the industry from 5.2g of ethyl methacrylate, 18g of dioctyl adipate, 0.05g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide;
2) 10g of stearyl methacrylate, 2.5g of alpha-eicose, 22g of dioctyl adipate, 0.05g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide are taken and prepared into a polymer Y according to a solution polymerization method well known in the industry;
3) Polymer Z was prepared by solution polymerization methods well known in the industry from 5.2g of ethyl methacrylate, 9.95g of stearyl methacrylate, 2.5g of alpha-eicosene, 3.5g of divinylbenzene and double-ended vinyl-terminated polysiloxane, 1.00g of fatty acid aluminum and particulate polyisobutylene, 20g of dioctyl adipate, 0.05g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 11
1) 7.5g of ethyl acrylate and methyl methacrylate, 7.5g of hydroxypropyl acrylate, 20g of liquid polybutene and 0.22g of benzoyl peroxide are taken and used for preparing a polymer X according to a solution polymerization method well known in the industry;
2) 1.17g of C20-alpha olefin, 24g of liquid polybutene and 0.22g of benzoyl peroxide are taken and prepared into a polymer Y according to a solution polymerization method well known in the industry;
3) 7.5g of ethyl acrylate and methyl methacrylate, 7.5g of hydroxypropyl acrylate, 1.17g of C20-alpha olefin, 4.6g of a mixture of diethylene glycol dimethacrylate and vinyl MQ silicone, 2.4g of granular polyacrylic resin and white carbon black, 16g of liquid polybutene and 0.22g of benzoyl peroxide are taken, and polymer Z is prepared according to the solution polymerization method well known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 12
1) Polymer X was prepared by solution polymerization methods well known in the industry from 12.5g of ethyl methacrylate, 5.5g of hydroxyethyl methacrylate, 16.6g of liquid polyisobutylene, 0.3g of 2,2' -azobis (2-methylbutyronitrile);
2) 2.4g of alpha-dodecene and alpha-octadecene, 16.8g of liquid polyisobutene and 0.3g of 2,2' -azobis (2-methylbutyronitrile) are taken and the polymer Y is prepared according to the solution polymerization method known in the industry;
3) Polymer Z was prepared by solution polymerization methods well known in the industry from 12.5g of ethyl methacrylate, 5.5g of hydroxyethyl methacrylate, 2.4g of alpha-dodecene and alpha-octadecene, 4.5g of double-ended vinyl-terminated polysiloxane, 3.8g of calcium and zinc fatty acids, 16.6g of liquid polyisobutylene, 0.3g of 2,2' -azobis (2-methylbutyronitrile);
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 13
1) Polymer X was prepared by solution polymerization of 11.5g of butyl acrylate and butyl methacrylate, 19g of polypropylene glycol and fatty alcohol polyoxyethylene ether, 0.15g of 2,2' -azobis (2-methylpropanenitrile) according to the well-known method of industry;
2) Polymer Y was prepared by solution polymerization methods well known in the industry from 5g of stearyl methacrylate, 0.25g of alpha-decene, 19g of polypropylene glycol and fatty alcohol-polyoxyethylene ether, and 0.15g of 2,2' -azobis (2-methylpropanenitrile);
3) Polymer Z was prepared by solution polymerization procedures known in the industry from 11.5g of butyl acrylate and butyl methacrylate, 5g of stearyl methacrylate, 0.25g of alpha-decene, 3.2g of vinyl MQ silicone resin, 5.85g of white carbon black, 19g of polypropylene glycol and fatty alcohol polyoxyethylene ether, and 0.15g of 2,2' -azobis (2-methylpropanenitrile);
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 14
1) 4g of hydroxypropyl acrylate, hydroxybutyl acrylate, 19g of fatty alcohol polyoxyethylene ether and 0.18g of 2,2' -azobis (2-methylpropanenitrile) are taken, and polymer X is prepared according to a solution polymerization method well known in the industry;
2) 12.5g of dodecyl acrylate, 2.5g of alpha-octadecene, 19g of fatty alcohol polyoxyethylene ether and 0.18g of 2,2' -azobis (2-methyl propionitrile) are taken to prepare a polymer Y according to a solution polymerization method well known in the industry;
3) 4g of hydroxypropyl acrylate and hydroxybutyl acrylate, 12.5g of dodecyl acrylate, 2.5g of alpha-octadecene, 0.5g of ethylene glycol dimethacrylate, 3.96g of fatty acid zinc, 19g of fatty alcohol polyoxyethylene ether and 0.18g of 2,2' -azobis (2-methylpropanenitrile) are taken, and a polymer Z is prepared according to a solution polymerization method known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 15
1) 12g of butyl acrylate, 4.7g of hydroxyethyl acrylate, 14.12g of diisooctyl adipate and polypropylene glycol, and 0.08g of 2,2' -azobis (2, 4-dimethylvaleronitrile) were taken and prepared according to the solution polymerization method known in the industry;
2) 7.5g of dodecyl methacrylate, 1g of alpha-methylstyrene, 14.12g of diisooctyl adipate and polypropylene glycol, and 0.08g of 2,2' -azobis (2, 4-dimethylvaleronitrile) were taken and prepared into a polymer Y by a solution polymerization method known in the industry;
3) Polymer Z was prepared by solution polymerization methods well known in the industry from 12g of butyl acrylate, 4.7g of hydroxyethyl acrylate, 7.5g of dodecyl methacrylate, 1g of alpha-methylstyrene, 5g of allyl methacrylate, 2g of aluminum fatty acid, 14.12g of diisooctyl adipate and polypropylene glycol, and 0.08g of 2,2' -azobis (2, 4-dimethylvaleronitrile);
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 16
1) 10g of isooctyl acrylate, 6.41g of hydroxypropyl methacrylate, 13.3g of dioctyl adipate, 0.13g of 2,2 '-azobis (2-methylpropanenitrile) and 2,2' -azobis (2-methylbutanenitrile) are taken and polymer X is prepared according to the solution polymerization method known in the industry;
2) 10g of octadecyl acrylate, 2g of alpha-dodecene, 13.3g of isooctyl alcohol, 0.13g of 2,2 '-azobis (2-methylpropanenitrile) and 2,2' -azobis (2-methylbutanenitrile) are taken and prepared into a polymer Y according to a solution polymerization method well known in the industry;
3) 10g of isooctyl acrylate, 6.3g of hydroxypropyl methacrylate, 10g of stearyl acrylate, 2g of alpha-dodecene, 2g of allyl methacrylate and ethylene glycol dimethacrylate, 1g of fatty acid calcium, 13.3g of dioctyl adipate and isooctyl alcohol, 0.13g of 2,2 '-azobis (2-methylpropanenitrile) and 2,2' -azobis (2-methylbutanenitrile) are taken, and a polymer Z is prepared according to a solution polymerization method well known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Example 17
1) 7.5g of hydroxyethyl acrylate and hydroxypropyl acrylate, 19.2g of polyether ester, 0.3g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide are taken, and polymer X is prepared according to a solution polymerization method well known in the industry;
2) 8g of octadecyl acrylate, 2.5g of alpha-triacontene and alpha-tetradecene, 18g of polyetheramine, 0.3g of 2,2' -azobis (2, 4-dimethyl valeronitrile) and benzoyl peroxide are taken, and polymer Y is prepared according to a solution polymerization method well known in the industry;
3) 7.5g of hydroxyethyl acrylate and hydroxypropyl acrylate, 8g of stearyl acrylate, 2.5g of alpha-triacontene and alpha-tetradecene, 4g of divinylbenzene and double-ended vinyl-terminated polysiloxane, 3.9g of fatty acid aluminum and granular silicone resin, 18g of polyether ester, 0.3g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide are taken, and polymer Z is prepared according to a solution polymerization method well known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Comparative example 1
Mineral oil defoamer prepared according to example 1 in patent CN102120106 a.
Comparative example 2
A silicone defoamer prepared according to example 1 in patent CN102343165 a.
Comparative example 3
Polyether defoamer prepared according to example 1 in patent CN102126763 a.
Comparative example 4
EBS defoamer prepared according to example 1 in patent CN101362063 a.
Comparative example 5
1) 21g of ethyl methacrylate, 10.6g of hydroxyethyl methacrylate, 29g of liquid polyisobutene, 1.9g of 2,2' -azobis (2-methylbutanenitrile) are taken and the polymer X is prepared according to the solution polymerization method known in the industry;
2) 6.6g of alpha-dodecene and alpha-octadecene, 29g of liquid polyisobutene, 1.9g of 2,2' -azobis (2-methylbutyronitrile) are taken and the polymer Y is prepared according to the solution polymerization method known in the industry;
3) Uniformly mixing the polymer X, Y by a shearing device to obtain the polymer defoamer composition P
Comparative example 6
1) 16.1g of butyl methacrylate, 4g of hydroxypropyl acrylate, 26g g of diisodecyl phthalate and 1.5g of 2,2' -azobis (2-methylpropanenitrile) are taken and used for preparing a polymer X according to a solution polymerization method known in the industry;
2) 16.1g of butyl methacrylate, 4g of hydroxypropyl acrylate, 1.8g of allyl methacrylate, 3g of granular polyacrylic resin and white carbon black, 26g of diisodecyl phthalate and 1.5g of 2,2' -azobis (2-methylpropanenitrile) are taken, and a polymer Z is prepared according to a solution polymerization method well known in the industry;
3) Uniformly mixing the polymer X, Z by a shearing device to obtain the polymer defoamer composition P
Comparative example 7
1) 9g of alpha-tetradecene, 29g of polytetramethylene glycol and 1.5g of 2,2' -azobis (2, 4-dimethyl valeronitrile) are taken, and polymer Y is prepared according to a solution polymerization method known in the industry;
2) 13g of alpha-tetradecene, 9g of double-end vinyl end-capped polysiloxane, 8g of granular polyacrylic resin, 29g of polytetramethylene glycol and 1.5g of 2,2' -azobis (2, 4-dimethyl valeronitrile) are taken, and polymer Z is prepared according to a solution polymerization method well known in the industry;
3) Uniformly mixing the polymer Y, Z by a shearing device to obtain the polymer defoamer composition P
Comparative example 8
1) 15g of hydroxyethyl acrylate and hydroxypropyl acrylate, 18.4g of polyether ester, 0.3g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide are taken and used for preparing a polymer X according to a solution polymerization method well known in the industry;
2) 8g of octadecyl acrylate, 2.5g of alpha-triacontene and alpha-tetradecene, 18.4g of polyether ester, 0.3g of 2,2' -azobis (2, 4-dimethyl valeronitrile) and benzoyl peroxide are taken, and polymer Y is prepared according to a solution polymerization method well known in the industry;
3) 8g of octadecyl acrylate, 2.5g of alpha-triacontene and alpha-tetradecene, 4g of divinylbenzene and double-ended vinyl-terminated polysiloxane, 3.9g of fatty acid aluminum and particulate polyisobutylene, 18.4g of polyether ester, 0.3g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide are taken, and polymer Z is prepared according to a solution polymerization method known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Comparative example 9
1) 12g of butyl acrylate, 4.7g of hydroxyethyl acrylate, 14.12g of diisooctyl adipate and polypropylene glycol, and 0.08g of 2,2' -azobis (2, 4-dimethylvaleronitrile) were taken and prepared according to the solution polymerization method known in the industry;
2) Polymer Y was prepared by solution polymerization methods well known in the industry from 11.5g of dodecyl methacrylate, 5.5g of alpha-methylstyrene, 14.12g of diisooctyl adipate and polypropylene glycol, and 0.08g of 2,2' -azobis (2, 4-dimethylvaleronitrile);
3) Polymer Z was prepared by solution polymerization methods well known in the industry from 12g of butyl acrylate, 4.7g of hydroxyethyl acrylate, 5g of allyl methacrylate, 2g of fatty acid aluminum, 14.12g of diisooctyl adipate and polypropylene glycol, and 0.08g of 2,2' -azobis (2, 4-dimethylvaleronitrile);
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Comparative example 10
1) 10.2g of ethyl methacrylate, 20g of dioctyl adipate, 0.05g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide were taken and prepared according to the solution polymerization method known in the industry;
2) Polymer Y was prepared by solution polymerization methods well known in the industry from 15.7g of stearyl methacrylate, 9.5g of alpha-eicose, 20g of dioctyl adipate, 0.05g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide;
3) 3.5g of divinylbenzene and double-end vinyl-terminated polysiloxane, 0.95g of fatty acid aluminum and granular polyisobutene, 20g of dioctyl adipate, 0.05g of 2,2' -azobis (2, 4-dimethylvaleronitrile) and benzoyl peroxide were taken and prepared according to the solution polymerization method known in the industry;
4) Uniformly mixing the polymer X, Y, Z by a shearing device to obtain the polymer defoamer composition P
Bubble eliminating and inhibiting performance test
Papermaking black liquor system testing method
600mL of papermaking pulping black liquor is added into a circulation bubbling instrument with a glass tube with a scale of 0-500 mL and an inner diameter of 5cm, so that the liquid level of the papermaking pulping black liquor reaches the position of the lowest scale of 0mL, the temperature is set to be 80 ℃, the flow is 6L/min, the voltage is 220V, a temperature control switch is turned on, a circulation pump is turned on after the papermaking pulping black liquor is heated to the set temperature, impact bubbling is started, when the foam rises to the position of 350mL, 0.2mL of defoaming agent is added, and the change of the foam height along with time is recorded. The shorter the time the foam reaches the lowest scale, the lower the scale is, which means that the instant defoaming performance of the defoamer is better; the longer the time elapsed at which the foam re-reached 350mL, the better the foam inhibition of the defoamer
Claims (9)
1. An antifoaming composition, characterized by the following composition:
a: alkyl methyl/acrylate monomer
The alkyl methyl/acrylic acid ester monomer has 1-8 alkyl number, is one or a mixture of acrylic acid ester and methacrylic acid ester, and is specifically selected from methyl acrylate, ethyl acrylate, butyl acrylate, isooctyl acrylate, methyl methacrylate, ethyl methacrylate, butyl methacrylate and isooctyl methacrylate, and the dosage of the alkyl methyl/acrylic acid ester monomer is 10-25% of the total mass of the defoaming composition;
b: hydroxyalkyl methacrylate monomers
The methyl/hydroxyalkyl acrylate monomer is one or a mixture of a plurality of hydroxyalkyl acrylate and hydroxyalkyl methacrylate, is specifically selected from hydroxyalkyl acrylate and hydroxyalkyl methacrylate, is specifically but not limited to hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate, and the dosage of the methyl/hydroxyalkyl acrylate monomer accounts for 5-15% of the total mass of the defoaming composition;
c: crosslinking agent monomer
The cross-linking agent monomer refers to a monomer which contains at least two or more vinyl groups in one molecule and can form a polymer soluble in an organic solvent; the foam-removing composition is selected from allyl methacrylate, methacrylic polyol esters, divinylbenzene, double-end vinyl end-capped polysiloxane, tetravinyl tetramethyl cyclotetrasiloxane and vinyl MQ silicone resin, can be used singly or mixed in any proportion, and the dosage of the foam-removing composition accounts for 0.5-5% of the total mass of the foam-removing composition;
d: alkyl methyl/acrylate monomer
The alkyl number of the methyl/acrylic acid alkyl ester is 9-18, the methyl/acrylic acid alkyl ester is one or more of alkyl acrylate and methyl acrylic acid alkyl ester, and the methyl/acrylic acid alkyl ester is one or more of dodecyl acrylate, octadecyl acrylate, dodecyl methacrylate and octadecyl methacrylate, and the dosage of the methyl/acrylic acid alkyl ester is 10-25% of the total mass of the defoaming composition;
o: olefin monomer
The olefin monomer is any one or a mixture of a plurality of linear alpha-olefins, alpha-aromatic olefins or branched alpha-olefins, and is specifically selected from one or a plurality of alpha-octenes, alpha-decenes, alpha-dodecenes, alpha-tetradecenes, alpha-hexadecenes, alpha-octadecenes, alpha-eicosenes, C20-C24 linear alpha-olefin mixtures, C24-C28 linear alpha-olefin mixtures, alpha-triacontenes, alpha-methyl styrene and alpha-styrene; the dosage is 0.5-5% of the total mass of the defoaming composition;
i: initiator(s)
The initiator is selected from 2,2' -azobis (2-methylpropanenitrile), 2' -azobis (2, 4-dimethyl valeronitrile), 2' -azobis (2-methylbutanenitrile) and benzoyl peroxide; the dosage is 0.1-1% of the total mass of the defoaming composition;
s: organic solvents
The organic solvent is selected from diisodecyl phthalate, diisooctyl adipate, diisooctyl phthalate, dioctyl adipate, 2-ethyl-1-hexanol, isooctanol, polyethylene glycol, polypropylene glycol, polytetramethylene glycol, liquid polybutene, liquid polyisobutene, fatty alcohol polyoxyethylene ether, polyether ester and polyether amine, and can be used singly or in a mixed mode; the dosage accounts for 30-60% of the total mass of the defoaming composition;
k: hydrophobic particles
The hydrophobic particles are inorganic hydrophobic particles, are selected from fatty acid magnesium salt, fatty acid calcium salt, fatty acid aluminum salt, fatty acid zinc salt, particle polyisobutene, particle polymethacrylic resin, particle polyacrylic resin, particle organic silicon resin and white carbon black, and can be used singly or in a mixed mode; the dosage is 1-8% of the total mass of the defoaming composition;
the preparation method of the defoaming composition comprises the following steps:
1) Preparing a polymer X by using a methyl/acrylic acid alkyl ester monomer A, methyl/acrylic acid hydroxyalkyl ester B, an organic solvent S and an initiator I according to a solution polymerization method known in the industry;
2) Preparing a polymer Y by using a methyl/acrylic acid alkyl ester monomer D, an olefin monomer O, an organic solvent S and an initiator I according to a solution polymerization method known in the industry;
3) Preparing a polymer Z from all monomers used by the polymer X and the polymer Y, a cross-linking agent monomer C, hydrophobic particles K, an organic solvent S and an initiator I according to a solution polymerization method known in the industry;
4) The polymer X, Y, Z was uniformly mixed by a shearing apparatus to obtain a defoamer composition.
2. The defoaming composition according to claim 1, wherein the amount of the methyl/alkyl acrylate monomer A is 15 to 20% of the total mass of the defoaming composition, the amount of the methyl/hydroxyalkyl acrylate monomer B is 8 to 12% of the total mass of the defoaming composition, the amount of the methyl/alkyl acrylate monomer D is 15 to 20% of the total mass of the defoaming composition, the amount of the olefin monomer O is 2 to 4% of the total mass of the defoaming composition, the amount of the crosslinking agent monomer C is 2 to 4% of the total mass of the defoaming composition, the amount of the organic solvent S is 40 to 50% of the total mass of the defoaming composition, the amount of the hydrophobic particles K is 3 to 6% of the total mass of the defoaming composition, and the amount of the initiator I is 0.4 to 0.8% of the total mass of the defoaming composition.
3. The defoaming composition according to claim 1, wherein said methyl/alkyl acrylate monomer a is selected from butyl acrylate, isooctyl methacrylate.
4. The defoamer composition of claim 1, wherein said methyl/alkyl acrylate monomer B is selected from the group consisting of hydroxyethyl acrylate and hydroxypropyl acrylate.
5. The defoaming composition according to claim 1, wherein said olefinic monomer O is selected from the group consisting of α -dodecene, α -tetradecene, α -hexadecene, α -octadecene, α -methylstyrene, α -styrene.
6. The defoamer composition of claim 1, wherein the crosslinker monomer C is selected from the group consisting of allyl methacrylate, ethylene glycol dimethacrylate, double-ended vinyl-terminated polysiloxanes, vinyl MQ silicone.
7. The defoaming composition according to claim 1, wherein said initiator I is benzoyl peroxide.
8. The defoaming composition according to claim 1, wherein the organic solvent S is selected from the group consisting of polypropylene glycol and fatty alcohol-polyoxyethylene ether.
9. The defoaming composition according to claim 1, wherein said hydrophobic particles K are selected from the group consisting of particulate polyisobutylenes, particulate polymethacrylic resins, particulate polyacrylic resins, particulate silicone resins, white carbon black.
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| CN202111095860.4A CN114146455B (en) | 2021-09-18 | 2021-09-18 | Defoaming composition |
| PCT/CN2021/132745 WO2023040045A1 (en) | 2021-09-18 | 2021-11-24 | Defoaming composition |
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| CN202111095860.4A CN114146455B (en) | 2021-09-18 | 2021-09-18 | Defoaming composition |
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| CN103272411B (en) * | 2013-06-07 | 2015-03-18 | 南京四新科技应用研究所有限公司 | Foam inhibitor and preparation method thereof |
| CN103641195B (en) * | 2013-12-13 | 2016-02-10 | 深圳市安品有机硅材料有限公司 | A kind of silicone antifoam agent and preparation method thereof |
| CN108786188B (en) * | 2017-05-05 | 2020-04-07 | 江苏四新科技应用研究所股份有限公司 | Non-silicon defoaming agent |
| WO2019000339A1 (en) * | 2017-06-29 | 2019-01-03 | Kemira Oyj | Aqueous emulsion and use thereof |
| CN110201427A (en) * | 2019-05-09 | 2019-09-06 | 江苏四新科技应用研究所股份有限公司 | A kind of polymer defoaming agent and preparation method thereof |
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