阅读说明：本技术 一种交联丙烯酸酯乳液的制备方法及其制备的产品 (Preparation method of crosslinked acrylate emulsion and product prepared by preparation method ) 是由 李兴明 于 2020-05-26 设计创作，主要内容包括：本发明公开了一种交联丙烯酸酯乳液的制备方法及其制备的产品,涉及乳液制备的技术领域。一种交联丙烯酸酯乳液的制备方法,包括以下步骤：S1预处理：称取丙烯酸酯粘性单体、三乙二醇单甲醚、丙烯酸酯内聚单体、乳化剂和混合水,搅拌均匀,用微射流均质机均质细化处理,制得细化液；S2交联乳化：称取过硫酸铵、碳酸氢钠和溶解水,加入丙烯酸、己二酸二酰肼和双丙酮丙烯酰胺,制得引发液,将细化液滴加至引发液中,加热,制得乳化液；S3后处理：向乳化液中加入增稠剂和消泡剂,搅拌,制得交联丙烯酸酯乳液产品。交联丙烯酸酯乳液的制备方法具有便于提高产品施工性的优点；交联丙烯酸酯乳液产品具有施工性好的优点。(The invention discloses a preparation method of a cross-linked acrylate emulsion and a product prepared by the same, and relates to the technical field of emulsion preparation. A preparation method of a cross-linked acrylate emulsion comprises the following steps: s1 pretreatment: weighing an acrylate viscous monomer, triethylene glycol monomethyl ether, an acrylate cohesive monomer, an emulsifier and mixed water, uniformly stirring, and homogenizing and refining by using a micro-jet homogenizer to prepare a refined liquid; s2 crosslinking and emulsifying: weighing ammonium persulfate, sodium bicarbonate and dissolved water, adding acrylic acid, adipic dihydrazide and diacetone acrylamide to prepare an initiation liquid, dropwise adding the refined liquid into the initiation liquid, and heating to prepare an emulsion; and S3 post-processing: and adding a thickening agent and a defoaming agent into the emulsion, and stirring to obtain a cross-linked acrylate emulsion product. The preparation method of the crosslinked acrylate emulsion has the advantage of improving the application property of the product; the crosslinked acrylate emulsion product has the advantage of good application property.)

1. The preparation method of the crosslinked acrylate emulsion is characterized by comprising the following steps:

s1 pretreatment: weighing a certain amount of acrylate viscous monomer, triethylene glycol monomethyl ether, acrylate cohesive monomer, emulsifier and mixed water, uniformly stirring, heating to 75-80 ℃, reacting for 10-30 min to prepare a mixed solution, and homogenizing and refining the mixed solution by using a micro-jet homogenizer to prepare a refined solution;

s2 crosslinking and emulsifying: weighing a certain amount of ammonium persulfate, sodium bicarbonate and dissolved water, stirring at the rotating speed of 300-500 r/min, heating to 77-83 ℃, adding acrylic acid, adipic dihydrazide and diacetone acrylamide to prepare a priming solution, dropwise adding the refined solution prepared in the step S1 into the priming solution for 10-15 min, stirring and emulsifying at 77-83 ℃ for 30-40 min to prepare an emulsion;

and S3 post-processing: adding a certain amount of thickening agent and defoaming agent into the emulsion, and stirring at the rotating speed of 400-600 revolutions per minute for 10-20 min to prepare a cross-linked acrylate emulsion product;

the materials are fed according to the following weight portion: 95-115 parts of acrylate viscous monomer, 65-85 parts of acrylate cohesive monomer, 0.8-1.5 parts of ammonium persulfate, 0.6-1.2 parts of sodium bicarbonate, 7-12 parts of emulsifier, 2-2.5 parts of acrylic acid, 8-12 parts of triethylene glycol monomethyl ether, 1-5 parts of adipic acid dihydrazide, 4-8 parts of diacetone acrylamide, 70-80 parts of mixed water, 30-40 parts of dissolved water, 3-5 parts of thickening agent and 2-4 parts of defoaming agent.

2. The preparation method of the crosslinked acrylate emulsion according to claim 1, wherein the materials are added according to the following weight ratio: 100-110 parts of acrylate viscous monomer, 70-80 parts of acrylate cohesive monomer, 1-1.2 parts of ammonium persulfate, 0.8-1 part of sodium bicarbonate, 8.5-10.5 parts of emulsifier, 2-2.5 parts of acrylic acid, 8-12 parts of triethylene glycol monomethyl ether, 2-4 parts of adipic dihydrazide, 5-7 parts of diacetone acrylamide, 70-80 parts of mixed water, 30-40 parts of dissolved water, 3-5 parts of thickening agent and 2-4 parts of defoaming agent.

3. The method of claim 2, wherein the method comprises the steps of: the acrylate viscous monomer is one or more of ethyl acrylate, butyl acrylate and isobutyl acrylate; the acrylate cohesive monomer is methyl methacrylate.

4. The method of claim 3, wherein the method comprises the steps of: the acrylate tackifying monomer is butyl acrylate.

5. The method for preparing a cross-linked acrylate emulsion according to claim 4, wherein the step S1 comprises the following steps:

S1A mucus preparation: weighing butyl acrylate and triethylene glycol monomethyl ether according to a set proportion, stirring at a rotating speed of 100-200 r/min, vacuumizing to reduce the system pressure to-0.095 Mpa to-0.08 Mpa, heating to 75-80 ℃, and reacting for 15-25 min to obtain acrylate mucus;

preparation of S1B polymerization solution: adding methyl methacrylate into the acrylate mucus prepared in the step S1A, stirring at the rotating speed of 300-500 r/min, vacuumizing to reduce the system pressure to-0.06 Mpa to-0.04 Mpa, heating to 75-80 ℃, and reacting for 10-20 min to prepare an acrylate polymerization solution;

S1C pre-emulsification: and (2) adding an emulsifier and mixed water into the acrylate polymerization liquid prepared in the step S1B, stirring for 10min-30min at the rotating speed of 2000-4000 rpm to prepare a mixed liquid, and homogenizing and refining the mixed liquid by using a micro-jet homogenizer to prepare a refined liquid.

6. The method of claim 2, wherein the method comprises the steps of: the emulsifier is sodium dodecyl sulfate.

7. The method of claim 5, wherein the method comprises the steps of: the median particle size of the refining liquid is 90nm-120 nm.

8. A crosslinked acrylate emulsion characterized by: the method for preparing the cross-linked acrylate emulsion according to any one of claims 1 to 7.

Technical Field

The invention relates to the technical field of preparation of acrylate emulsion, in particular to a preparation method of cross-linked acrylate emulsion and a product prepared by the same.

Background

The acrylic ester emulsion has excellent adhesion property and is widely used in the fields of building coatings, decorative paints and the like. The main components of the acrylic emulsion are organic acrylate compounds and water, and the compatibility of the acrylate and the water is poor, so that the stability of the acrylic emulsion is influenced. In the preparation of acrylic emulsion, in order to improve the stability and adhesion of acrylic emulsion, a certain amount of acrylic acid with better water solubility is usually added.

The application publication No. CN106977647A discloses an acrylic emulsion, the formula of the acrylic emulsion is composed of a kettle bottom material containing an A-103 emulsifier, emulsion, an ammonium persulfate initiator, an ammonia water PH value regulator, a defoaming agent and a functional auxiliary agent, and the emulsion is composed of the following components by mass: 195-205kg of water, 6.5-8.5kg of A-103 emulsifier, 6.5-8.5kg of K12 emulsifier, 355 kg of butyl acrylate, 13-17kg of acrylic acid, 58-62kg of methyl methacrylate, 48-52kg of acrylonitrile and 1-3kg of functional monomer. According to the technical scheme, the acrylic acid with good water solubility is added into the acrylic acid emulsion, so that the compatibility of each component in the acrylic acid emulsion is improved, and the stability of the acrylic acid emulsion is improved.

However, the use amount of acrylic acid in the technical scheme is large, so that ammonia water is needed to neutralize carboxyl groups on acrylic acid molecules subsequently, the ammonia water has strong pungent smell, construction of workers is not facilitated, and the constructability of products is reduced.

Disclosure of Invention

In view of the defects of the prior art, the first object of the present invention is to provide a method for preparing a crosslinked acrylate emulsion which facilitates to improve the workability of products, and has the advantage of facilitating to improve the workability of products.

The second object of the present invention is to provide a crosslinked acrylate emulsion which can reduce the amount of acrylic acid used to some extent, and which has an advantage that the workability of the product can be improved to some extent.

In order to achieve the first object, the invention provides the following technical scheme: a preparation method of a cross-linked acrylate emulsion comprises the following steps:

s1 pretreatment: weighing a certain amount of acrylate viscous monomer, triethylene glycol monomethyl ether, acrylate cohesive monomer, emulsifier and mixed water, uniformly stirring, heating to 75-80 ℃, reacting for 10-30 min to prepare a mixed solution, and homogenizing and refining the mixed solution by using a micro-jet homogenizer to prepare a refined solution;

s2 crosslinking and emulsifying: weighing a certain amount of ammonium persulfate, sodium bicarbonate and dissolved water, stirring at the rotating speed of 300-500 r/min, heating to 77-83 ℃, adding acrylic acid, adipic dihydrazide and diacetone acrylamide to prepare a priming solution, dropwise adding the refined solution prepared in the step S1 into the priming solution for 10-15 min, stirring and emulsifying at 77-83 ℃ for 30-40 min to prepare an emulsion;

and S3 post-processing: adding a certain amount of thickening agent and defoaming agent into the emulsion, and stirring at the rotating speed of 400-600 revolutions per minute for 10-20 min to prepare a cross-linked acrylate emulsion product;

the materials are fed according to the following weight portion: 95-115 parts of acrylate viscous monomer, 65-85 parts of acrylate cohesive monomer, 0.8-1.5 parts of ammonium persulfate, 0.6-1.2 parts of sodium bicarbonate, 7-12 parts of emulsifier, 2-2.5 parts of acrylic acid, 8-12 parts of triethylene glycol monomethyl ether, 1-5 parts of adipic acid dihydrazide, 4-8 parts of diacetone acrylamide, 70-80 parts of mixed water, 30-40 parts of dissolved water, 3-5 parts of thickening agent and 2-4 parts of defoaming agent.

By adopting the technical scheme, a certain amount of hydrophilic triethylene glycol monomethyl ether is added in the preparation process of the cross-linked acrylate emulsion, the triethylene glycol monomethyl ether and ester functional groups on partial acrylate viscous monomers and acrylate cohesive monomer molecules perform ester exchange reaction to generate an esterified substance with certain hydrophilicity and lipophilicity in the preparation process of the cross-linked acrylate emulsion, and then the esterified substance is homogenized and refined by a microfluid homogenizer to prepare the stable refined liquid, so that the compatibility of each component in the emulsion is improved, the stability of the emulsion is improved, the use amount of acrylic acid is reduced to a certain extent, the use of ammonia water with strong irritation is avoided, and the constructability of the emulsion is improved.

Preferably, the materials are fed according to the following weight portion: 100-110 parts of acrylate viscous monomer, 70-80 parts of acrylate cohesive monomer, 1-1.2 parts of ammonium persulfate, 0.8-1 part of sodium bicarbonate, 8.5-10.5 parts of emulsifier, 2-2.5 parts of acrylic acid, 8-12 parts of triethylene glycol monomethyl ether, 2-4 parts of adipic dihydrazide, 5-7 parts of diacetone acrylamide, 70-80 parts of mixed water, 30-40 parts of dissolved water, 3-5 parts of thickening agent and 2-4 parts of defoaming agent.

By adopting the technical scheme, the cross-linked acrylic emulsion with better stability is prepared by using better raw material proportion, so that the market competitiveness and the market value of products are improved.

Preferably, the acrylate viscous monomer is one or more of ethyl acrylate, butyl acrylate and isobutyl acrylate; the acrylate cohesive monomer is methyl methacrylate.

By adopting the technical scheme, the proper acrylate adhesive monomer and acrylate cohesive monomer are selected, so that the adhesive force and stability of the crosslinked acrylic emulsion are improved, the adhesive force of the emulsion on the coated article is improved, the durability of the product is prolonged, the market competitiveness of the product is improved, and the market value of the product is improved.

Preferably, the acrylate tackifying monomer is butyl acrylate.

By adopting the technical scheme, butyl acrylate is selected as the acrylate viscous monomer, which is beneficial to improving the adhesive force of the cross-linked acrylic emulsion, improving the adhesive force of the emulsion on the coated article, prolonging the durability of the product, improving the market competitiveness of the product and improving the market value of the product.

Preferably, the emulsifier is sodium lauryl sulfate.

By adopting the technical scheme, the sodium dodecyl sulfate is selected, and is easy to be compounded with other components of the crosslinked acrylate emulsion in the preparation process of the crosslinked acrylate emulsion, so that the stability of the emulsion is improved, the quality guarantee period of the product is prolonged, the market competitiveness of the product is improved, and the market value of the product is improved.

Preferably, the step S1 includes the following steps:

S1A mucus preparation: weighing butyl acrylate and triethylene glycol monomethyl ether according to a set proportion, stirring at a rotating speed of 100-200 r/min, vacuumizing to reduce the system pressure to-0.095 Mpa to-0.08 Mpa, heating to 75-80 ℃, and reacting for 15-25 min to obtain acrylate mucus;

preparation of S1B polymerization solution: adding methyl methacrylate into the acrylate mucus prepared in the step S1A, stirring at the rotating speed of 300-500 r/min, vacuumizing to reduce the system pressure to-0.06 Mpa to-0.04 Mpa, heating to 75-80 ℃, and reacting for 10-20 min to prepare an acrylate polymerization solution;

S1C pre-emulsification: and (2) adding an emulsifier and mixed water into the acrylate polymerization liquid prepared in the step S1B, stirring for 10min-30min at the rotating speed of 2000-4000 rpm to prepare a mixed liquid, and homogenizing and refining the mixed liquid by using a micro-jet homogenizer to prepare a refined liquid.

By adopting the technical scheme, butyl acrylate is firstly used for reacting with a part of triethylene glycol monomethyl ether, and then methyl methacrylate is added for reacting with the rest of triethylene glycol monomethyl ether, so that the modification ratio of the triethylene glycol monomethyl ether to different components in the emulsion can be controlled, the components of the crosslinked acrylic emulsion are optimized, the stability of the product is improved, the quality guarantee period of the product is prolonged, the market competitiveness of the product is improved, and the market value of the product is improved.

Preferably, the median particle size of the refining solution is 90nm-120 nm.

By adopting the technical scheme, if the particle size of the latex particles is too large, the latex particles are easy to settle and are not beneficial to suspending the latex particles in water, and the viscosity of the latex is reduced due to the overlarge latex particles, so that the uniform and stable dispersion of the latex particles in water is not beneficial, and the stability of a latex product is adversely affected; if the particle size of the latex particles is too small, the polymerization effect of each component in the emulsion is influenced, and the stability of the emulsion product is adversely affected; the invention prepares the refining liquid with proper grain size through the homogenizing and refining treatment of the micro-jet homogenizer, thereby better controlling the grain size of latex particles in the emulsion, being beneficial to improving the stability of the cross-linked acrylic emulsion, prolonging the shelf life of the product, improving the market competitiveness of the product and improving the market value of the product.

In order to achieve the second object, the invention provides the following technical scheme: a cross-linked acrylate emulsion is prepared by the preparation method of the cross-linked acrylate emulsion.

By adopting the technical scheme, the cross-linked acrylate emulsion prepared by the invention is beneficial to improving the stability of products, reduces the consumption of acrylic acid to a certain extent, avoids the use of ammonia water with strong pungent smell, improves the constructability and stability of the products, improves the market competitiveness of the products and improves the market value of the products.

In summary, the invention includes at least one of the following beneficial technical effects:

1. according to the invention, triethylene glycol monomethyl ether is added into the acrylic emulsion to modify the acrylate monomer component in the cross-linked acrylate emulsion, so that the hydrophilicity of the emulsion component is improved, and then the micro-jet homogenizer is used for homogenizing and refining to prepare the refined liquid with a proper particle size, so that the stability of the emulsion is improved, the dosage of acrylic acid is reduced, the use of ammonia water with strong irritation is avoided, and the constructability of the emulsion is improved;

2. the invention uses proper acrylate adhesive monomer, acrylate cohesive monomer and emulsifier, which is helpful to improve the stability and adhesive force of the product, prolong the shelf life and durability of the product, improve the market competitiveness of the product and improve the market value of the product;

3. according to the invention, butyl acrylate is firstly used for reacting with a part of triethylene glycol monomethyl ether, and then methyl methacrylate is added for reacting with the rest of triethylene glycol monomethyl ether, so that the modification ratio of the triethylene glycol monomethyl ether to different components in the emulsion can be controlled, the components of the crosslinked acrylic emulsion are optimized, the stability of the product is improved, the market competitiveness of the product is improved, and the market value of the product is improved.

Detailed Description