CN115819808A - Water-resistant redispersible latex powder and preparation method thereof - Google Patents

Water-resistant redispersible latex powder and preparation method thereof Download PDF

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Publication number
CN115819808A
CN115819808A CN202310032084.6A CN202310032084A CN115819808A CN 115819808 A CN115819808 A CN 115819808A CN 202310032084 A CN202310032084 A CN 202310032084A CN 115819808 A CN115819808 A CN 115819808A
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water
latex powder
resistant
redispersible latex
polyvinyl alcohol
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Inventor
单云
范厚能
杨军
张明良
王大莲
李春雏
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ANHUI WANWEI HUASHAN NEW MATERIAL CO LTD
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ANHUI WANWEI HUASHAN NEW MATERIAL CO LTD
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Publication of CN115819808A publication Critical patent/CN115819808A/en
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Abstract

The invention discloses a water-resistant redispersible latex powder and a preparation method thereof, wherein the raw materials comprise polymer emulsion, polyvinyl alcohol aqueous solution, an anti-caking agent and organic siloxane grafted polyvinyl formal. The redispersible latex powder has excellent dispersibility, flowability and water resistance, is an environment-friendly product which can be used in high-performance building materials, can promote the application of the redispersible latex powder in building mortar, special waterproof materials and the like, and has wide market prospect.

Description

Water-resistant redispersible latex powder and preparation method thereof
Technical Field
The invention relates to the field of dry-mixed mortar additives, in particular to water-resistant redispersible latex powder and a preparation method thereof.
Background
The redispersible latex powder is a redispersible powder obtained by modifying a polymer emulsion by adding other substances and performing spray drying. After the mortar is mixed with the mortar, the curing reaction of the polymer and the hydration reaction of the cement are carried out simultaneously, so that an interpenetrating network structure of the polymer and the cement gel is formed. The structure can connect aggregate more firmly, thereby improving the performance of cement mortar. Redispersible latex powder prepared from vinyl acetate/ethylene copolymer (VAE) emulsion occupies the main dry-mixed mortar market all over the world, but the waterproof performance of the latex powder is generally poor.
Patent CN110684307A describes a water-resistant redispersible latex powder which is resistant to water for 8h without falling off. But the method used by the invention is to add an organic silicon cross-linking agent to increase the water resistance of the rubber powder. The organosilicon cross-linking agent has low surface tension, is easy to adhere to the surface of a cement hydration product in the mortar hardening process, influences the cement hydration reaction rate, and causes the early strength of the mortar to be too low.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a water-resistant redispersible latex powder and a preparation method thereof, so as to effectively overcome the defects of low early strength and poor water resistance of the product in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a water-resistant redispersible latex powder comprises polymer emulsion, aqueous solution of polyvinyl alcohol, anti-blocking agent and organic siloxane grafted polyvinyl formal.
Further, the polymer emulsion is a mixture of vinyl acetate-versatic acid ethylene copolymer emulsion and at least one of vinyl acetate-ethylene copolymer emulsion and polyacrylate emulsion, and the mass percentage of the vinyl acetate-versatic acid ethylene copolymer emulsion accounts for 30-40% of the total mass of the polymer emulsion.
Further, the solid content of the polymer emulsion is 45% -60%, and the viscosity is 2300mPa.s-5400mPa.s.
Further, the polymerization degree of the polyvinyl alcohol is 500-2400, and the alcoholysis degree is 78-90%.
Further, the solid content of the polyvinyl alcohol aqueous solution is 15% -30%, and the mass ratio of the polyvinyl alcohol aqueous solution to the polymer emulsion is 1.
Further, the addition amount of the anti-caking agent accounts for 1% -4% of the mass of solids in the polymer emulsion, the polyvinyl alcohol aqueous solution and the organosiloxane grafted polyvinyl formal; the addition amount of the organosiloxane grafted polyvinyl formal accounts for 0.5-1.5% of the mass of solids in the polymer emulsion and the polyvinyl alcohol aqueous solution.
Further, the anti-caking agent is at least one of heavy calcium powder, talcum powder, kaolin, bentonite and fumed silica.
The preparation method of the water-resistant redispersible latex powder comprises the following steps:
step 1, adding water into polyvinyl alcohol, heating and stirring to prepare a polyvinyl alcohol aqueous solution;
step 2, mixing the polyvinyl alcohol aqueous solution, the polymer emulsion and the organic siloxane grafted polyvinyl formal according to a ratio, and uniformly stirring to obtain a spray solution;
and 3, conveying the prepared spray liquid into drying equipment for spray drying, carrying out high-speed centrifugal atomization to form micro droplets, adding an anti-caking agent from a feeding port above the drying equipment through compressed air to prevent bonding, and then cooling and separating the obtained rubber powder particles to obtain the water-resistant redispersible latex powder.
Compared with the prior art, the invention has the beneficial effects that:
1. the redispersible latex powder has excellent dispersibility, flowability and water resistance, is an environment-friendly product which can be used in high-performance building materials, can promote the application of the redispersible latex powder in building mortar, special waterproof materials and the like, and has wide market prospect.
2. In the formula system of the redispersible latex powder, the organic siloxane grafted polyvinyl formal can improve the water resistance of the redispersible latex powder, and the annular structure of the organic siloxane grafted polyvinyl formal can show stronger bonding force to an EPS (expandable polystyrene) plate due to the similarity and intermiscibility principle.
3. In the formula system of the redispersible latex powder, under the alkaline condition of cement mortar, the organic siloxane grafted polyvinyl formal has better chemical stability compared with an organic silicon cross-linking agent, is not easy to decompose, has higher surface tension than the organic silicon cross-linking agent, and cannot interfere the hydration action of cement to influence the early strength of the mortar.
4. The preparation process of the redispersible latex powder of the invention uses the original production conditions, and does not need to add new process equipment.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The polyvinyl alcohols and organosiloxane-grafted polyvinyl formals used in the examples below, each having a degree of polymerization and alcoholysis, are commercially available, as follows: available from Anhui Uygur, anhui, uygur, inc.
Each of the polymer emulsions used in the following examples is commercially available as follows: the vinyl acetate-ethylene copolymer emulsion can be purchased from Guangxi Anhui vitamin materials science and technology Limited, model 705; vinyl acetate-vinyl versatate copolymer emulsions are available from Shandong Haoyao New materials, inc.; polyacrylate emulsions are available from Minde chemical Co., ltd, of Jinan.
Example 1
The preparation method of the water-resistant redispersible latex powder of this example is as follows:
step 1: adding water into polyvinyl alcohol with the polymerization degree of 1200 and the alcoholysis degree of 80%, heating and stirring to prepare a polyvinyl alcohol aqueous solution with the solid content of 18%.
Step 2: mixing a polyvinyl alcohol aqueous solution with a vinyl acetate-ethylene copolymer emulsion (with the viscosity of 2400Pa & s and the solid content of 48%) and a vinyl acetate-tertiary carboxylic acid ethylene copolymer emulsion (with the viscosity of 2400Pa & s and the solid content of 48%) according to a mass ratio of 1:3.1:1.4, adding the organic siloxane grafted polyvinyl formal, mixing, and uniformly stirring to obtain the spray solution. Wherein, the addition amount of the organic siloxane grafted polyvinyl formal accounts for 1.5 percent of the solid mass in the polymer emulsion and the polyvinyl alcohol aqueous solution.
And step 3: and (3) conveying the prepared spray liquid to drying equipment for spray drying, and controlling the air inlet temperature of the drying equipment to be 120 ℃ and the air outlet temperature to be 80 ℃. And when the inlet air temperature reaches the set temperature, feeding is started, the feeding speed must be gradually adjusted from low to high, the flow is properly adjusted until the outlet temperature meets the requirement and is stable, and meanwhile, an anti-caking agent is added from a feeding port above the drying equipment through compressed air to prevent bonding, so that the water-resistant re-dispersible latex powder is obtained. Wherein: the anti-caking agent is prepared from heavy calcium powder and gas-phase silicon dioxide according to the mass ratio of 2:1, the addition amount of the anti-caking agent accounts for 2 percent of the solid content of the spray liquid.
The latex powder obtained in this example was subjected to the following performance tests:
1. water resistance
The rubber powder is dispersed into regenerated emulsion when meeting water, and the regenerated emulsion is subjected to film forming again and drying, so that the rubber powder does not fall off after being resistant to water for 8 hours.
2. Adhesive strength
The water resistance strength of the redispersible emulsion powder obtained in the embodiment is tested according to the GB/T29906-2013 molded polyphenyl board thin plastered exterior wall external thermal insulation system material standard, and the result is as follows: the bonding strength between the polystyrene board and the molded polystyrene board is 0.12MPa, and the bonding strength between the polystyrene board and the concrete board is 0.80MPa.
3. Early strength
The redispersible latex powder obtained in this example was tested for three-day strength according to the GBT17671-1999 cement mortar strength test method, and the results showed that the redispersible latex powder of this example had a compressive strength of 12.5MPa.
Example 2
The preparation method of the water-resistant redispersible latex powder of this example is as follows:
step 1: adding water into polyvinyl alcohol with the polymerization degree of 1400 and the alcoholysis degree of 84%, heating and stirring to prepare a polyvinyl alcohol aqueous solution with the solid content of 21%.
Step 2: mixing a polyvinyl alcohol aqueous solution with a vinyl acetate-ethylene copolymer emulsion (the viscosity is 3200 Pa.s, the solid content is 48%) and a vinyl acetate-tertiary carboxylic acid ethylene copolymer emulsion (the viscosity is 3000 Pa.s, the solid content is 45%) according to a mass ratio of 1:2.8:1.7, adding the organic siloxane grafted polyvinyl formal, mixing, and uniformly stirring to obtain the spray solution. Wherein the addition of the organosiloxane-grafted polyvinyl formal accounts for 1.5% of the mass of the solids in the polymer emulsion and the aqueous polyvinyl alcohol solution.
And step 3: and (3) conveying the prepared spray liquid to drying equipment for spray drying, and controlling the air inlet temperature of the drying equipment to be 120 ℃ and the air outlet temperature to be 80 ℃. And when the inlet air temperature reaches the set temperature, feeding is started, the feeding speed must be gradually adjusted from low to high, the flow is properly adjusted until the outlet temperature meets the requirement and is stable, and meanwhile, an anti-caking agent is added from a feeding port above the drying equipment through compressed air to prevent bonding, so that the water-resistant re-dispersible latex powder is obtained. Wherein: the anti-caking agent is prepared from heavy calcium powder and gas-phase silicon dioxide according to the mass ratio of 2:1, the addition amount of the anti-caking agent accounts for 2 percent of the solid content of the spray liquid.
The latex powder obtained in this example was subjected to the following performance tests:
1. water resistance
The rubber powder is dispersed into regenerated emulsion when meeting water, and the regenerated emulsion is subjected to film forming again and drying, so that the rubber powder does not fall off after being resistant to water for 8 hours.
2. Adhesive strength
The water resistance strength of the redispersible emulsion powder obtained in the embodiment is tested according to the GB/T29906-2013 molded polyphenyl board thin plastered exterior wall external thermal insulation system material standard, and the result is as follows: the bonding strength between the polystyrene board and the molded polystyrene board is 0.13MPa, and the bonding strength between the polystyrene board and the concrete board is 0.82MPa.
3. Early strength
The redispersible latex powder obtained in this example was tested for three-day strength according to the GBT17671-1999 cement mortar strength test method, and the results showed that the redispersible latex powder of this example had a compressive strength of 12.9MPa.
Example 3
The preparation method of the water-resistant redispersible latex powder of this example is as follows:
step 1: adding water into polyvinyl alcohol with the polymerization degree of 2200 and the alcoholysis degree of 86%, heating and stirring to prepare a polyvinyl alcohol aqueous solution.
Step 2: mixing a polyvinyl alcohol aqueous solution with a vinyl acetate-ethylene copolymer emulsion (viscosity is 4400Pa & s, solid content is 56%), and a vinyl acetate-tertiary carboxylic acid ethylene copolymer emulsion (viscosity is 5200Pa & s, solid content is 58%) according to a mass ratio of 1:2.7:1.8, adding organic siloxane grafted polyvinyl formal, mixing, and uniformly stirring to obtain a spray solution. Wherein the addition amount of the organic siloxane grafted polyvinyl formal accounts for 1.5 percent of the mass of the solid in the polymer emulsion and the polyvinyl alcohol aqueous solution.
And step 3: and (3) conveying the prepared spray solution to drying equipment for spray drying, and controlling the air inlet temperature of the drying equipment to be 120 ℃ and the air outlet temperature to be 80 ℃. And when the inlet air temperature reaches the set temperature, feeding is started, the feeding speed must be gradually adjusted from low to high, the flow is properly adjusted until the outlet temperature meets the requirement and is stable, and meanwhile, an anti-caking agent is added from a feeding port above the drying equipment through compressed air to prevent bonding, so that the water-resistant re-dispersible latex powder is obtained. Wherein: the anti-caking agent is prepared from heavy calcium powder and gas-phase silicon dioxide according to the mass ratio of 2:1, the addition amount of the anti-caking agent accounts for 2 percent of the solid content of the spray liquid.
The latex powder obtained in this example was subjected to the following performance tests:
1. water resistance
The rubber powder is dispersed into regenerated emulsion when meeting water, and the regenerated emulsion is subjected to film forming again and drying, so that the rubber powder does not fall off after being resistant to water for 8 hours.
2. Adhesive strength
The redispersible latex powder obtained in the embodiment is tested according to the GB/T29906-2013 molded polyphenyl board thin plastered external thermal insulation system material standard, and the result is that: the adhesive strength between the polystyrene board and the molded polystyrene board is 0.14MPa, and the adhesive strength between the polystyrene board and the concrete board is 0.84MPa.
3. Early strength
The three-day strength of the redispersible latex powder obtained in the embodiment is tested according to the GBT17671-1999 cement mortar strength test method, and the results show that the redispersible latex powder has a compressive strength of 13.1MPa.
Example 4
The preparation method of the water-resistant redispersible latex powder of this example is as follows:
step 1: adding water into polyvinyl alcohol with polymerization degree of 2000 and alcoholysis degree of 82%, heating and stirring to obtain polyvinyl alcohol aqueous solution.
Step 2: mixing a polyvinyl alcohol aqueous solution, a vinyl acetate-ethylene copolymer emulsion (viscosity is 4400 Pa.s, solid content is 56%), a vinyl acetate-tertiary carboxylic acid ethylene copolymer emulsion (viscosity is 5200 Pa.s, solid content is 58%), a polyacrylate emulsion according to a mass ratio of 1:2.9:1.5:0.1, adding organic siloxane grafted polyvinyl formal, mixing, and uniformly stirring to obtain a spray solution. Wherein the addition amount of the organic siloxane grafted polyvinyl formal accounts for 1.5 percent of the mass of the solid in the polymer emulsion and the polyvinyl alcohol aqueous solution.
And 3, step 3: and (3) conveying the prepared spray liquid to drying equipment for spray drying, and controlling the air inlet temperature of the drying equipment to be 120 ℃ and the air outlet temperature to be 80 ℃. And when the inlet air temperature reaches the set temperature, feeding is started, the feeding speed must be gradually adjusted from low to high, the flow is properly adjusted until the outlet temperature meets the requirement and is stable, and meanwhile, an anti-caking agent is added from a feeding port above the drying equipment through compressed air to prevent bonding, so that the water-resistant re-dispersible latex powder is obtained. Wherein: the anti-caking agent is prepared from heavy calcium powder and gas-phase silicon dioxide according to the mass ratio of 2:1, wherein the addition amount of the anti-caking agent accounts for 2 percent of the solid content of the spray liquid.
The latex powder obtained in this example was subjected to the following performance tests:
1. water resistance
The rubber powder is dispersed into regenerated emulsion when meeting water, and the regenerated emulsion is subjected to film forming again and drying, so that the rubber powder does not fall off after being resistant to water for 8 hours.
2. Adhesive strength
The water resistance strength of the redispersible emulsion powder obtained in the embodiment is tested according to the GB/T29906-2013 molded polyphenyl board thin plastered exterior wall external thermal insulation system material standard, and the result is as follows: the adhesive strength between the polystyrene board and the molded polystyrene board is 0.13MPa, and the adhesive strength between the polystyrene board and the concrete board is 0.81MPa.
3. Early strength
The redispersible latex powder obtained in this example was tested for three-day strength according to the GBT17671-1999 cement mortar strength test method, and the results showed that the redispersible latex powder of this example had a compressive strength of 12.7MPa.
Comparative example 1
The redispersible latex powder is prepared in the same manner as in comparative example 1, except that: in step 2, the amount of organosiloxane-grafted polyvinyl butyral added was 0.5% of the mass of the solids in the polymer emulsion and the aqueous polyvinyl alcohol solution.
The latex powder obtained in the comparative example is subjected to the following performance tests:
1. water resistance
The rubber powder is dispersed into regenerated emulsion when meeting water, and the regenerated emulsion is subjected to film forming again and drying, so that the rubber powder does not fall off after being resistant to water for 8 hours.
2. Adhesive strength
The water resistance strength of the redispersible latex powder obtained in the comparative example is tested according to the GB/T29906-2013 molded polyphenyl board thin plastered external thermal insulation system material standard, and the result is as follows: the adhesive strength between the polystyrene board and the molded polystyrene board is 0.09MPa, and the adhesive strength between the polystyrene board and the concrete board is 0.74MPa.
3. Early strength
The three-day strength of the redispersible latex powder obtained in the comparative example is tested according to the GBT17671-1999 cement mortar strength test method, and the results show that the redispersible latex powder of the embodiment has a compressive strength of 12.3MPa.
Comparative example 2
The redispersible latex powder is prepared in the same manner as in comparative example 1, except that: in step 2, the amount of organosiloxane-grafted polyvinyl butyral added was 2% of the mass of the solids in the polymer emulsion and the aqueous polyvinyl alcohol solution.
The latex powder obtained in the comparative example is subjected to the following performance tests:
1. water resistance
The rubber powder is dispersed into regenerated emulsion when meeting water, and the regenerated emulsion is subjected to film forming again and drying, so that the rubber powder does not fall off after being resistant to water for 8 hours.
2. Adhesive strength
According to the GB/T29906-2013 molded polyphenyl board thin plastered exterior wall external thermal insulation system material standard, the water resistance strength of the redispersible emulsion powder obtained in the comparative example is tested, and the result is as follows: the adhesive strength between the polystyrene board and the molded polystyrene board is 0.09MPa, and the adhesive strength between the polystyrene board and the concrete board is 0.75MPa.
3. Early strength
The three-day strength of the redispersible latex powder obtained in the comparative example is tested according to the GBT17671-1999 cement mortar strength test method, and the results show that the redispersible latex powder of the embodiment has a compressive strength of 12.1MPa.
Comparative example 3
The redispersible latex powder is prepared in the same manner as in comparative example 1, except that: the organosiloxane-grafted polyvinyl butyral from step 2 was replaced with an organosilicon crosslinker (hydrogen-containing silicone oil).
The latex powder obtained in the comparative example is subjected to the following performance tests:
1. water resistance
The rubber powder is dispersed into regenerated emulsion when meeting water, and the regenerated emulsion is subjected to film forming again and drying, so that the rubber powder does not fall off after being resistant to water for 8 hours.
2. Adhesive strength
According to the GB/T29906-2013 molded polyphenyl board thin plastered exterior wall external thermal insulation system material standard, the water resistance strength of the redispersible emulsion powder obtained in the comparative example is tested, and the result is as follows: the adhesive strength between the polystyrene board and the molded polystyrene board is 0.07MPa, and the adhesive strength between the polystyrene board and the concrete board is 0.73MPa.
4. Early strength
The three-day strength of the redispersible emulsion powder obtained in the comparative example is tested according to the GBT17671-1999 cement mortar strength test method, and the result shows that the redispersible emulsion powder added with the organic silicon cross-linking agent has the compressive strength of 9.6MPa.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (8)

1. A water-resistant redispersible latex powder characterized in that: the raw materials of the water-resistant redispersible latex powder comprise polymer emulsion, polyvinyl alcohol aqueous solution, anti-caking agent and organic siloxane grafted polyvinyl formal.
2. The water-resistant redispersible latex powder of claim 1 wherein: the polymer emulsion is a mixture of vinyl acetate-versatic acid ethylene copolymer emulsion and at least one of vinyl acetate-ethylene copolymer emulsion and polyacrylate emulsion, and the mass percentage of the vinyl acetate-versatic acid ethylene copolymer emulsion accounts for 30-40% of the total mass of the polymer emulsion.
3. The water-resistant redispersible latex powder as claimed in claim 1 or 2, wherein: the solid content of the polymer emulsion is 45-60%, and the viscosity is 2300-5400mPa.s.
4. The water-resistant redispersible latex powder of claim 1 wherein: the polymerization degree of the polyvinyl alcohol is 500-2400, and the alcoholysis degree is 78-90%.
5. The water-resistant redispersible latex powder of claim 1 wherein: the solid content of the polyvinyl alcohol aqueous solution is 15% -30%, and the mass ratio of the polyvinyl alcohol aqueous solution to the polymer emulsion is 1.
6. The water-resistant redispersible latex powder of claim 1 wherein: the addition amount of the anti-caking agent accounts for 1-4% of the mass of the solids in the polymer emulsion, the polyvinyl alcohol aqueous solution and the organosiloxane grafted polyvinyl formal; the addition amount of the organic siloxane grafted polyvinyl formal accounts for 0.5 to 1.5 percent of the mass of the solid in the polymer emulsion and the polyvinyl alcohol aqueous solution.
7. The water-resistant redispersible latex powder of claim 1 wherein: the anti-caking agent is at least one of heavy calcium powder, talcum powder, kaolin, bentonite and gas-phase silicon dioxide.
8. A method for preparing the water-resistant redispersible latex powder of any one of claims 1 to 7, comprising the steps of:
step 1, adding water into polyvinyl alcohol, heating and stirring to prepare a polyvinyl alcohol aqueous solution;
step 2, mixing the polyvinyl alcohol aqueous solution, the polymer emulsion and the organic siloxane grafted polyvinyl formal according to a ratio, and uniformly stirring to obtain a spray solution;
and 3, conveying the prepared spray liquid into drying equipment for spray drying, carrying out high-speed centrifugal atomization to form micro droplets, adding an anti-caking agent from a feeding port above the drying equipment through compressed air to prevent bonding, and then cooling and separating the obtained rubber powder particles to obtain the water-resistant redispersible latex powder.
CN202310032084.6A 2023-01-10 2023-01-10 Water-resistant redispersible latex powder and preparation method thereof Pending CN115819808A (en)

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CN112322230A (en) * 2020-11-04 2021-02-05 巢湖皖维金泉实业有限公司 Polyvinyl acetate emulsion adhesive with excellent water resistance and preparation method thereof
CN113024885A (en) * 2021-03-16 2021-06-25 中国科学院长春应用化学研究所 Emulsion separation material and preparation method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09254531A (en) * 1996-03-25 1997-09-30 Mitsubishi Paper Mills Ltd Ink jet recording sheet
US20030044611A1 (en) * 2001-08-16 2003-03-06 Kurt Stark Silane-modified polyvinyl acetals
US20060052530A1 (en) * 2002-07-25 2006-03-09 Andreas Bacher Polyvinyl alcohols and polyvinyl acetals containing silane
CN1903898A (en) * 2006-07-21 2007-01-31 华南理工大学 Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method
CN101173021A (en) * 2007-10-26 2008-05-07 上海大学 Acrylic acid series nucleocapsid polymer emulsion and re-dispersible emulsion powder, and method for producing thereof
CN101649096A (en) * 2009-06-29 2010-02-17 上海东升新材料有限公司 Ampholytic re-dispersible emulsion powder
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CN112322230A (en) * 2020-11-04 2021-02-05 巢湖皖维金泉实业有限公司 Polyvinyl acetate emulsion adhesive with excellent water resistance and preparation method thereof
CN113024885A (en) * 2021-03-16 2021-06-25 中国科学院长春应用化学研究所 Emulsion separation material and preparation method thereof
CN114316850A (en) * 2022-01-12 2022-04-12 浙江志强涂料有限公司 Water-retaining building adhesive and preparation process thereof

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