CN113512147B - Preparation method of high-performance carboxylic styrene-butadiene latex - Google Patents
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- CN113512147B CN113512147B CN202110725782.5A CN202110725782A CN113512147B CN 113512147 B CN113512147 B CN 113512147B CN 202110725782 A CN202110725782 A CN 202110725782A CN 113512147 B CN113512147 B CN 113512147B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F236/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
- C08F236/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
- C08F236/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
- C08F236/10—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated with vinyl-aromatic monomers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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Abstract
The invention discloses a preparation method of high-performance carboxylic styrene-butadiene latex, and relates to the technical field of carboxylic styrene-butadiene latex. The invention firstly adds initiator into deionized water, modified emulsifier, molecular weight regulator, butadiene, styrene and vinyl pyridine mixture to react to prepare pre-dispersion liquid, then adds initiator into deionized water, pre-dispersion liquid, emulsifier, molecular weight regulator, butadiene, styrene, functional monomer, organic bentonite, beta-carboxyethyl acrylate, unsaturated carboxylic acid, sodium lignin sulfonate and electrolyte mixture to polymerize, then adjusts pH and deaerates to obtain the high-performance carboxylated styrene-butadiene latex. The preparation process is simple, and the obtained carboxylated styrene-butadiene latex has the advantages of concentrated particle size dispersion, good fluidity and moderate viscosity, and has good stability.
Description
Technical Field
The invention belongs to the technical field of carboxyl styrene-butadiene latex, and particularly relates to a preparation method of high-performance carboxyl styrene-butadiene latex.
Background
The carboxyl styrene-butadiene latex is a milky white aqueous dispersion with bluish violet luster, and a terpolymer prepared from butadiene, styrene, unsaturated carboxylic acid and the like through emulsion polymerization has the performance of the styrene-butadiene latex, and has higher conjunctival strength and binding force, large filling amount, good film forming performance, excellent mechanical, chemical and freeze thawing stability, good compatibility with pigments and fillers, and wide application in papermaking, carpets, textiles and building industry due to the introduction of polar groups-carboxyl.
However, in either paper or paint, the latex has relatively high stability and fluidity, and moderate viscosity is required. However, the particle size distribution range of the carboxyl styrene-butadiene latex prepared by the prior art is wide, the size difference is large, the stability and the fluidity of the carboxyl styrene-butadiene latex are affected to a certain extent, and the application of the carboxyl styrene-butadiene latex is limited.
Disclosure of Invention
Aiming at the defects in the background art, the invention provides a preparation method of high-performance carboxyl styrene-butadiene latex, which is realized by the following technical scheme:
a preparation method of high-performance carboxylic styrene-butadiene latex comprises the following steps:
1) Deionized water, a modified emulsifier, a molecular weight regulator, butadiene, styrene and vinyl pyridine are sequentially added into a reaction vessel under the nitrogen atmosphere, the temperature is raised to 50-65 ℃, and an initiator is added for reaction for 6-10 hours, so that a dispersion liquid I is obtained;
2) Sequentially adding deionized water, a dispersion liquid I, an emulsifier, a molecular weight regulator, butadiene, styrene, a functional monomer, organic bentonite, beta-carboxyethyl acrylate, unsaturated carboxylic acid, sodium lignin sulfonate and electrolyte into a reaction container under vacuum condition, heating to 85-100 ℃, adding an initiator, and carrying out heat preservation reaction for 2-3.5 hours to obtain a dispersion liquid II;
3) And adding a pH regulator into the dispersion liquid II to regulate the pH to 7-8, then degassing, cooling to room temperature and discharging to obtain the carboxyl styrene-butadiene latex.
As a further improvement of the technical scheme, in the step 1), the additives are respectively as follows in parts by weight: 100 parts of deionized water, 12-16 parts of modified emulsifier, 0.3-0.5 part of molecular weight regulator, 10-20 parts of butadiene, 20-35 parts of styrene, 5-12 parts of vinylpyridine and 0.8-2.0 parts of initiator.
As a further improvement of the technical scheme, the modified emulsifier is compounded by sodium alkylbenzenesulfonate and fatty alcohol-polyoxyethylene ether, and the mass ratio of the modified emulsifier is (8-11): 3.
the invention adopts an emulsifier compounded by sodium alkylbenzenesulfonate and fatty alcohol polyoxyethylene ether, and firstly prepares butadiene, styrene and vinyl pyridine into a vinyl pyridine modified dispersion liquid, and the dispersion liquid has good polymer stability, and can obviously improve the stability of the prepared latex in the subsequent polymerization process of carboxyl styrene-butadiene latex.
As a further improvement of the technical scheme, in the step 2), the additives are respectively as follows in parts by weight: 100 parts of deionized water, 20-25 parts of dispersion liquid I, 5-8 parts of an emulsifying agent, 0.6-1.0 part of a molecular weight regulator, 15-30 parts of butadiene, 15-25 parts of styrene, 6-12 parts of a functional monomer, 4-8 parts of organic bentonite, 0.2-0.4 part of beta-carboxyethyl acrylate, 10-15 parts of unsaturated carboxylic acid, 1-2 parts of sodium lignin sulfonate, 0.2-0.3 part of an electrolyte and 1.4-2.4 parts of an initiator.
The second step of the invention is to prepare the pre-modified dispersion liquid by adopting the steps, and to prepare the carboxyl styrene-butadiene latex with concentrated particle size range and moderate viscosity by matching with other components such as organic bentonite and the like to participate in the subsequent polymerization of butadiene and styrene.
As a further improvement of the above technical scheme, the molecular weight regulator is tert-dodecyl mercaptan.
The tertiary dodecyl mercaptan is an effective molecular weight regulator, is widely used in the polymerization process of ABS resin, styrene-butadiene rubber and nitrile rubber, and effectively reduces the molecular weight of the polymer, thereby being beneficial to the subsequent processing and application of the polymer.
As a further improvement of the technical scheme, the initiator is tert-butyl peroxybenzoate.
The initiator is a substance capable of initiating the monomer to carry out polymerization reaction, and can directly influence the smooth progress of the polymerization reaction process, and simultaneously influence the reaction rate and the storage period of the product.
As a further improvement of the technical scheme, the emulsifier is alkylphenol ethoxylates.
As a further improvement of the above technical solution, the functional monomer is acrylamide.
The organic bentonite is an organic ammonium compound, can form gel in various organic solvents and liquid resins, and has good thixotropic property, suspension stability, lubricity and film forming property.
As a further improvement of the above technical scheme, the unsaturated carboxylic acid is acrylic acid.
As a further improvement of the above technical scheme, the degassing in the step 3) is carried out for 1-2 hours under the condition of-0.08 MPa to-0.1 MPa.
Compared with the prior art, the invention has the beneficial effects that:
the invention firstly adds initiator into deionized water, modified emulsifier, molecular weight regulator, butadiene, styrene and vinyl pyridine mixture to react to prepare dispersion liquid with good stability, combines functional monomer, organic bentonite, sodium lignin sulfonate and the like to be used in polymerization process of butadiene, styrene and unsaturated carboxylic acid, and obtains carboxyl styrene-butadiene latex by heating and polymerizing mixed phase. The carboxyl styrene-butadiene latex prepared by the invention has the advantages of concentrated particle size distribution, good stability, good fluidity and moderate viscosity.
Detailed Description
In order to make the technical scheme and advantages of the present invention more clear, the technical scheme of the present invention will be more clearly and completely described below with reference to the embodiments. The specific conditions are not noted in the examples, and the reagents or instruments used are conventional products commercially available, which are not noted by the manufacturer, or are recommended by the manufacturer.
Example 1
9 parts of sodium alkyl benzene sulfonate and 3 parts of fatty alcohol polyoxyethylene ether are compounded to obtain the modified emulsifier. 100 parts of deionized water, 15 parts of modified emulsifier, 0.4 part of molecular weight regulator, 12 parts of butadiene, 32 parts of styrene and 8 parts of vinyl pyridine are sequentially added into a reaction vessel according to parts by weight under the nitrogen atmosphere, and the temperature is raised to 60 ℃ and 1.5 parts of initiator is added for reaction for 8 hours, so that a dispersion liquid A is obtained.
Example 2
9 parts of sodium alkyl benzene sulfonate and 1 part of fatty alcohol polyoxyethylene ether are compounded to obtain the modified emulsifier. 100 parts of deionized water, 12 parts of modified emulsifier, 0.4 part of molecular weight regulator, 18 parts of butadiene, 20 parts of styrene and 8 parts of vinyl pyridine are sequentially added into a reaction vessel according to parts by weight under the nitrogen atmosphere, and the temperature is raised to 60 ℃ and 1.5 parts of initiator is added for reaction for 8 hours, so that a dispersion liquid B is obtained.
Example 3
100 parts of deionized water, 22 parts of the dispersion A prepared in the example 1, 6 parts of an emulsifier, 0.8 part of a molecular weight regulator, 24 parts of butadiene, 20 parts of styrene, 8 parts of a functional monomer, 6 parts of organic bentonite, 0.3 part of beta-carboxyethyl acrylate, 12 parts of acrylic acid, 1 part of sodium lignin sulfonate and 0.2 part of electrolyte are sequentially added into a reaction vessel according to the parts by weight under the vacuum condition, and the temperature is raised to 90 ℃, 1.8 parts of an initiator is added for thermal insulation reaction for 3.0 hours, so that the dispersion is obtained. And adding a pH regulator into the dispersion liquid to regulate the pH to 7.5, then degassing, cooling to room temperature and discharging to obtain the carboxyl styrene-butadiene latex.
The performance of the carboxylated styrene-butadiene latex sample prepared in the embodiment is detected (GB/T8301-2008), and the following steps are obtained: the viscosity of the polymer is 242cps, the average particle diameter is 94nm (the particle diameter size is +/-10 percent and exceeds 90 percent), the mechanical stability is 0.025 percent, and the polymer stability is 0.003 percent.
Example 4
100 parts of deionized water, 22 parts of the dispersion B prepared in the example 2, 6 parts of an emulsifier, 0.8 part of a molecular weight regulator, 24 parts of butadiene, 20 parts of styrene, 8 parts of a functional monomer, 6 parts of organic bentonite, 0.3 part of beta-carboxyethyl acrylate, 12 parts of acrylic acid, 1 part of sodium lignin sulfonate and 0.2 part of electrolyte are sequentially added into a reaction vessel according to the parts by weight under the vacuum condition, and the temperature is raised to 90 ℃, 1.8 parts of an initiator is added for thermal insulation reaction for 3.0 hours, so that the dispersion is obtained. And adding a pH regulator into the dispersion liquid to regulate the pH to 7.5, then degassing, cooling to room temperature and discharging to obtain the carboxyl styrene-butadiene latex.
The performance of the carboxylated styrene-butadiene latex sample prepared in the embodiment is detected (GB/T8301-2008), and the following steps are obtained: the viscosity of the polymer is 237cps, the average particle diameter is 98nm (particle diameter size + -10% exceeds 84%), the mechanical stability is 0.024%, and the polymer stability is 0.004%.
Example 5
100 parts of deionized water, 25 parts of the dispersion A prepared in the example 1, 6 parts of an emulsifier, 0.8 part of a molecular weight regulator, 16 parts of butadiene, 15 parts of styrene, 6 parts of a functional monomer, 8 parts of organic bentonite, 0.3 part of beta-carboxyethyl acrylate, 15 parts of acrylic acid, 1 part of sodium lignin sulfonate and 0.3 part of electrolyte are sequentially added into a reaction vessel according to the parts by weight under the vacuum condition, and the temperature is raised to 95 ℃, 2.2 parts of an initiator is added for thermal insulation reaction for 3.0 hours, so that the dispersion is obtained. And adding a pH regulator into the dispersion liquid to regulate the pH to 7.5, then degassing, cooling to room temperature and discharging to obtain the carboxyl styrene-butadiene latex.
The performance of the carboxylated styrene-butadiene latex sample prepared in the embodiment is detected (GB/T8301-2008), and the following steps are obtained: the viscosity of the polymer is 226cps, the average particle diameter is 92nm (the particle diameter size is +/-10 percent and exceeds 90 percent), the mechanical stability is 0.023 percent, and the polymer stability is 0.003 percent.
Comparative example 1
100 parts of deionized water, 15 parts of an unmodified emulsifier (alkylphenol ethoxylate), 0.4 part of a molecular weight regulator, 12 parts of butadiene, 32 parts of styrene and 8 parts of vinylpyridine are sequentially added into a reaction vessel according to parts by weight under a nitrogen atmosphere, and 1.5 parts of an initiator is added to react for 8 hours after the temperature is raised to 60 ℃ to obtain a dispersion liquid C.
100 parts of deionized water, 22 parts of the dispersion C prepared in the comparative example 1, 6 parts of an emulsifier, 0.8 part of a molecular weight regulator, 24 parts of butadiene, 20 parts of styrene, 8 parts of a functional monomer, 6 parts of organic bentonite, 0.3 part of beta-carboxyethyl acrylate, 12 parts of acrylic acid, 1 part of sodium lignin sulfonate and 0.2 part of electrolyte are sequentially added into a reaction vessel according to the parts by weight under the vacuum condition, and the temperature is raised to 90 ℃, 1.8 parts of an initiator is added for thermal insulation reaction for 3.0 hours, so that the dispersion is obtained. And adding a pH regulator into the dispersion liquid to regulate the pH to 7.5, then degassing, cooling to room temperature and discharging to obtain the carboxyl styrene-butadiene latex.
The performance of the carboxylic styrene-butadiene latex sample prepared in the comparative example is detected (GB/T8301-2008), and the following steps are obtained: the viscosity was 294cps, the average particle diameter 136nm (particle size.+ -. 10% of 43%), the mechanical stability 0.057% and the polymer stability 0.018%.
Comparative example 2
100 parts of deionized water, 22 parts of the dispersion A prepared in the example 1, 6 parts of an emulsifier, 0.8 part of a molecular weight regulator, 24 parts of butadiene, 20 parts of styrene, 8 parts of a functional monomer (without adding organic bentonite), 0.3 part of beta-carboxyethyl acrylate, 12 parts of acrylic acid, 1 part of sodium lignin sulfonate and 0.2 part of electrolyte are sequentially added into a reaction vessel according to the parts by weight under the vacuum condition, and the temperature is raised to 90 ℃, 1.8 parts of an initiator is added for thermal insulation reaction for 3.0 hours, so that the dispersion is obtained. And adding a pH regulator into the dispersion liquid to regulate the pH to 7.5, then degassing, cooling to room temperature and discharging to obtain the carboxyl styrene-butadiene latex.
The performance of the carboxylic styrene-butadiene latex sample prepared in the comparative example is detected (GB/T8301-2008), and the following steps are obtained: the viscosity of the polymer is 277cps, the average particle diameter is 118nm (particle diameter size + -10% is 55%), the mechanical stability is 0.041%, and the polymer stability is 0.015%.
Comparative example 3
Under the vacuum condition, 100 parts of deionized water (without adding pre-dispersion liquid), 6 parts of emulsifying agent, 0.8 part of molecular weight regulator, 24 parts of butadiene, 20 parts of styrene, 8 parts of functional monomer, 6 parts of organic bentonite, 0.3 part of beta-carboxyethyl acrylate, 12 parts of acrylic acid, 1 part of sodium lignin sulfonate and 0.2 part of electrolyte are sequentially added into a reaction container according to parts by weight, the temperature is raised to 90 ℃, 1.8 parts of initiator is added, and the reaction is carried out for 3.0 hours under heat preservation, thus obtaining the dispersion liquid. And adding a pH regulator into the dispersion liquid to regulate the pH to 7.5, then degassing, cooling to room temperature and discharging to obtain the carboxyl styrene-butadiene latex.
The performance of the carboxylic styrene-butadiene latex sample prepared in the comparative example is detected (GB/T8301-2008), and the following steps are obtained: the viscosity was 334cps, the average particle size was 145nm (particle size.+ -. 10% of 36%), the mechanical stability was 0.060%, and the polymer stability was 0.023%.
As can be seen from examples 1-5, the carboxylic styrene-butadiene latex prepared by the invention has moderate viscosity, concentrated particle size range and good stability. By adopting the preparation method of the example 3, no modified emulsifier, no organic bentonite and no pre-dispersion liquid are added, and according to the comparative examples 1-3, the stability of the synthesized carboxyl styrene-butadiene latex is reduced, and the prepared latex has dispersed particle size and cannot meet the performance requirement of the coating.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application and not for limiting the same; although the present application has been described in detail with reference to preferred embodiments, those of ordinary skill in the art will appreciate that: modifications may be made to the specific embodiments of the present application or equivalents may be substituted for part of the technical features, which are all included in the scope of the technical solutions claimed herein.
Claims (8)
1. The preparation method of the high-performance carboxylic styrene-butadiene latex is characterized by comprising the following steps of:
1) Deionized water, a modified emulsifier, a molecular weight regulator, butadiene, styrene and vinyl pyridine are sequentially added into a reaction vessel under the nitrogen atmosphere, the temperature is raised to 50-65 ℃, and an initiator is added for reaction for 6-10 hours, so that a dispersion liquid I is obtained; the modified emulsifier is compounded by sodium alkylbenzenesulfonate and fatty alcohol polyoxyethylene ether, and the mass ratio of the modified emulsifier is (8-11): 3, a step of;
2) Sequentially adding deionized water, a dispersion liquid I, an emulsifier, a molecular weight regulator, butadiene, styrene, a functional monomer, organic bentonite, beta-carboxyethyl acrylate, unsaturated carboxylic acid, sodium lignin sulfonate and electrolyte into a reaction container under vacuum condition, heating to 85-100 ℃, adding an initiator, and carrying out heat preservation reaction for 2-3.5 hours to obtain a dispersion liquid II;
3) And adding a pH regulator into the dispersion liquid II to regulate the pH to 7-8, then degassing, cooling to room temperature and discharging to obtain the carboxyl styrene-butadiene latex.
2. The preparation method of the high-performance carboxyl styrene-butadiene latex as claimed in claim 1, wherein the mass parts of the additives in the step 1) are as follows: 100 parts of deionized water, 12-16 parts of modified emulsifier, 0.3-0.5 part of molecular weight regulator, 10-20 parts of butadiene, 20-35 parts of styrene, 5-12 parts of vinylpyridine and 0.8-2.0 parts of initiator.
3. The preparation method of the high-performance carboxyl styrene-butadiene latex as claimed in claim 1, wherein the mass parts of the additives in the step 2) are as follows: 100 parts of deionized water, 20-25 parts of dispersion liquid I, 5-8 parts of an emulsifying agent, 0.6-1.0 part of a molecular weight regulator, 15-30 parts of butadiene, 15-25 parts of styrene, 6-12 parts of a functional monomer, 4-8 parts of organic bentonite, 0.2-0.4 part of beta-carboxyethyl acrylate, 10-15 parts of unsaturated carboxylic acid, 1-2 parts of sodium lignin sulfonate, 0.2-0.3 part of an electrolyte and 1.4-2.4 parts of an initiator.
4. The method for preparing high-performance carboxylated styrene-butadiene latex according to claim 1, wherein the molecular weight regulator is tertiary dodecyl mercaptan.
5. The method for preparing high-performance carboxylated styrene-butadiene latex according to claim 1, wherein the initiator is tert-butyl peroxybenzoate.
6. The method for preparing high-performance carboxylated styrene-butadiene latex according to claim 1, wherein the functional monomer is acrylamide.
7. The method for preparing high-performance carboxylated styrene-butadiene latex according to claim 1, wherein the unsaturated carboxylic acid is acrylic acid.
8. The method for preparing high-performance carboxylated styrene-butadiene latex according to claim 1, wherein the degassing in the step 3) is carried out for 1 to 2 hours under the condition of-0.08 MPa to-0.1 MPa.
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| CN114634586B (en) * | 2022-04-11 | 2022-10-21 | 广西大学 | Modified carboxylic styrene-butadiene latex, and preparation method and application thereof |
| CN114835961B (en) * | 2022-06-17 | 2023-03-17 | 日照锦湖金马化学有限公司 | Preparation process of modified carboxylic styrene-butadiene latex |
| CN116874970B (en) * | 2023-07-26 | 2024-03-08 | 杭州富阳富翔化工有限公司 | Carboxyl styrene-butadiene latex composite material and preparation method thereof |
| CN117551234A (en) * | 2023-12-30 | 2024-02-13 | 珠海金鸡化工有限公司 | Low-odor carboxyl styrene-butadiene latex and preparation method thereof |
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| WO2015030533A1 (en) * | 2013-08-29 | 2015-03-05 | 주식회사 엘지화학 | Carboxylic acid modified nitrile based copolymer latex composition and dip molded product comprising same |
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| CN101891868B (en) * | 2010-07-29 | 2012-05-09 | 浙江长安仁恒科技股份有限公司 | Method for preparing carboxylated styrene-butadiene latex |
| CN102786620B (en) * | 2012-07-18 | 2015-07-15 | 杭州蓝诚实业有限公司 | Small-particle-size carboxylic styrene-butadiene latex and its preparation method |
| CN111234079B (en) * | 2020-01-17 | 2022-05-06 | 日照广大建筑材料有限公司 | Special carboxylic styrene-butadiene latex for lawn and preparation process thereof |
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| WO2015030533A1 (en) * | 2013-08-29 | 2015-03-05 | 주식회사 엘지화학 | Carboxylic acid modified nitrile based copolymer latex composition and dip molded product comprising same |
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| Preparation and properties of styrene butadiene rubber/natural rubber/organo-bentonite nanocomposites prepared from latex dispersions;Zheng Gu,等;Applied Clay Science;第46卷(第3期);241-244 * |
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