阅读说明：本技术 一种水性无机填料分散剂及其制备方法 (Water-based inorganic filler dispersant and preparation method thereof ) 是由 黄異 黄凯 张意 于 2019-10-13 设计创作，主要内容包括：本发明提供了一种水性无机填料分散剂,其原料包括以下组分,各组分以及各组分的质量份分别为：羧酸单体、倍半硅氧烷颗粒、长链单体、纯化水、分子量控制剂、引发剂、手性磷酸、相容剂；所述水性无机填料分散剂为粉体形态,其微观形态为均匀球体颗粒,颗粒平均粒径为12μm～25μm。本发明所制得的水性无机填料分散剂粉体均匀,使用方便简单,且在常温环境下保存24个月不会失效,对于一般的无机材料有良好的分散作用,抗干扰能力强。(The invention provides a water-based inorganic filler dispersing agent, which comprises the following raw materials in parts by mass: carboxylic acid monomer, silsesquioxane particles, long-chain monomer, purified water, molecular weight control agent, initiator, chiral phosphoric acid and compatilizer; the aqueous inorganic filler dispersant is in a powder form, the microscopic form of the aqueous inorganic filler dispersant is uniform spherical particles, and the average particle size of the particles is 12-25 mu m. The water-based inorganic filler dispersing agent prepared by the invention is uniform in powder, convenient and simple to use, free from failure after being stored for 24 months in a normal-temperature environment, good in dispersing effect on common inorganic materials and strong in anti-interference capability.)

1. The water-based inorganic filler dispersing agent is characterized by comprising the following raw materials in parts by mass: 400-500 parts of carboxylic acid monomer, 10-15 parts of silsesquioxane particles, 30-100 parts of long-chain monomer, 80-100 parts of purified water, 20-40 parts of molecular weight control agent, 0.5-1.5 parts of initiator, 0.05-0.2 part of chiral phosphoric acid and 0.05-0.5 part of compatilizer; the aqueous inorganic filler dispersant is in a powder form, the microscopic form of the aqueous inorganic filler dispersant is uniform spherical particles, and the average particle size of the particles is 12-25 mu m.

2. The aqueous inorganic filler dispersant of claim 1, characterized in that: the carboxylic acid monomer is one or a mixture of more than two of methacrylic acid, acrylic acid, maleic anhydride and maleic-rich acid.

3. The aqueous inorganic filler dispersant of claim 1, characterized in that: the silsesquioxane particles are a mixture of cage type silsesquioxane with a vinyl content of 0.15-0.2% and trapezoid type silsesquioxane with a vinyl content of 0.15-0.2% in a mass ratio of 2: 1.

4. The aqueous inorganic filler dispersant of claim 1, characterized in that: the long-chain monomer is a mixture of prenyl polyoxyethylene ether with the molecular weight of 8000-15000 and maleic acid polyethylene glycol monomethyl ether ester with the molecular weight of 6300-15000 according to the proportion of 6: 1.

5. The aqueous inorganic filler dispersant of claim 1, characterized in that: the molecular weight control agent is one or a mixture of more than two of acrylic acid-1, 3-sultone, sodium methallyl sulfonate and 2-acrylamide-2-methylpropanesulfonic acid.

6. The aqueous inorganic filler dispersant of claim 1, characterized in that: the compatilizer is a mixture of polydopamine and ethyl silicate according to any mass ratio.

7. The aqueous inorganic filler dispersant of claim 1, characterized in that: the initiator is a mixture of potassium persulfate and dibenzoyl peroxide, or a mixture of potassium persulfate and azobisisobutyronitrile, and the mixing mass ratio is 2: 1-4: 1.

8. The method for preparing the aqueous inorganic filler dispersant of any one of claims 1 to 7, characterized by comprising the steps of: adding a carboxylic acid monomer, purified water and a long-chain monomer into a reaction kettle, heating to 50 ℃, starting stirring when the temperature reaches, setting the stirring speed at 25-35 rpm, keeping the stirring speed for 15-35 min, adding silsesquioxane, an initiator and a molecular weight control agent, keeping stirring for 15min, heating to 80 ℃, keeping the temperature for 3h, dropwise adding chiral phosphoric acid, keeping the temperature for 1h at 90 ℃, discharging to obtain a semi-finished product, adding 2 mass percent of toluene into the semi-finished product, placing the semi-finished product on a rotary evaporator, drying at 80-105 ℃ in vacuum, stopping drying when the moisture content in the product is determined to be less than 1 percent on an infrared moisture determinator, and discharging to obtain the aqueous inorganic filler dispersing agent.

Technical Field

The invention belongs to the technical field of polymer synthesis, relates to a dispersant, and particularly relates to a water-based inorganic filler dispersant.

Background

The dispersion of inorganic materials in aqueous solutions has been a significant problem in the industries of coatings, construction and the like, and the existing dispersants have many significant disadvantages, such as: the addition amount is too large, the selectivity to a system is high, the problem of failure of part of inorganic materials can occur, the problem of environmental pollution can possibly occur, certain requirements on equipment are met, and the problems are important problems for restricting industrial development. Therefore, the development of a new type of dispersion product with wider applicability is becoming an important social demand.

Chinese patent 201510773263.0 discloses a water-based paint dispersant, which is prepared from acrylic acid, methyl methacrylate, white carbon black, glycol, organic solvent, n-amyl alcohol, malonic acid, initiator, sodium sulfite and neutralizer; the dispersant can reduce the surface tension of the water-based paint, enhance the wetting effect on pigment particles, stably disperse the pigment particles in a liquid phase, and can be quickly and firmly combined with surface groups of the paint, so that the pigment particles are stably suspended in an aqueous solvent, the pigment is well dispersed, and the optimal dispersion effect is achieved. The dispersion effect and the dispersion speed are improved by adding the modified white carbon black; in the preparation process of the dispersant, the molecular weight of a product and the distribution of products are changed by changing the conventional one-time addition of the initiator into the multiple addition of the initiator, so that the prepared dispersant not only has good dispersing performance, but also has good capability of resisting the change of environmental temperature. However, in the patent, because an organic solvent is used, the VOC is high and the environment is not friendly; and the organic solvent is ineffective due to its volatility.

Disclosure of Invention

The invention aims to solve the technical problem of the prior art and provides a water-based inorganic filler dispersing agent and a preparation method thereof, wherein the water-based inorganic filler dispersing agent has uniform powder, is convenient and simple to use, cannot lose efficacy after being stored for 24 months at normal temperature, has good dispersing effect on common inorganic materials, and has strong anti-interference capability.

In order to solve the technical problems, the technical scheme provided by the invention is as follows:

the water-based inorganic filler dispersing agent is characterized by comprising the following raw materials in parts by mass: 400-500 parts of carboxylic acid monomer, 10-15 parts of silsesquioxane particles, 30-100 parts of long-chain monomer, 80-100 parts of purified water, 20-40 parts of molecular weight control agent, 0.5-1.5 parts of initiator, 0.05-0.2 part of chiral phosphoric acid and 0.05-0.5 part of compatilizer; the aqueous inorganic filler dispersant is in a powder form, the microscopic form of the aqueous inorganic filler dispersant is uniform spherical particles, and the average particle size of the particles is 12-25 mu m.

The carboxylic acid monomer is one or a mixture of more than two of methacrylic acid, acrylic acid, maleic anhydride and maleic-rich acid.

The silsesquioxane particles are a mixture of cage type silsesquioxane with a vinyl content of 0.15-0.2% and trapezoid type silsesquioxane with a vinyl content of 0.15-0.2% in a mass ratio of 2: 1.

The long-chain monomer is a mixture of prenyl polyoxyethylene ether with the molecular weight of 8000-15000 and maleic acid polyethylene glycol monomethyl ether ester with the molecular weight of 6300-15000 according to the proportion of 6: 1.

The molecular weight control agent is one or a mixture of more than two of acrylic acid-1, 3-sultone, sodium methallyl sulfonate and 2-acrylamide-2-methylpropanesulfonic acid.

The compatilizer is a mixture of polydopamine and ethyl silicate according to any mass ratio.

The initiator is a mixture of potassium persulfate and dibenzoyl peroxide, or a mixture of potassium persulfate and azobisisobutyronitrile, and the mixing mass ratio is 2: 1-4: 1.

The invention also provides a preparation method of the aqueous inorganic filler dispersing agent, which comprises the following steps: adding a carboxylic acid monomer, purified water and a long-chain monomer into a reaction kettle, heating to 50 ℃, starting stirring when the temperature reaches, setting the stirring speed at 25-35 rpm, keeping the stirring speed for 15-35 min, adding silsesquioxane, an initiator and a molecular weight control agent, keeping stirring for 15min, heating to 80 ℃, keeping the temperature for 3h, dropwise adding chiral phosphoric acid, keeping the temperature for 1h at 90 ℃, discharging to obtain a semi-finished product, adding 2 mass percent of toluene into the semi-finished product, placing the semi-finished product on a rotary evaporator, drying at 80-105 ℃ in vacuum, stopping drying when the moisture content in the product is determined to be less than 1 percent on an infrared moisture determinator, and discharging to obtain the aqueous inorganic filler dispersing agent.

The powder dispersing agent prepared by adopting the special synthesis process and the powder preparation process has the advantages of uniform and spherical powder shape, convenient and simple use, no failure after being stored for 24 months in a normal temperature environment, good dispersing effect on common inorganic materials, strong anti-interference capability and obvious resistance to impurities in inorganic fillers.

Detailed Description

In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention is further described in detail with reference to the following examples.

In the following examples, the silsesquioxane particles were a mixture of cage-type silsesquioxane having a vinyl content of 0.15%, 0.18%, 0.2% and ladder-type silsesquioxane having a vinyl content of 0.15%, 0.18%, 0.2%, respectively, in a mass ratio of 2: 1. The long-chain monomers are respectively a mixture of prenyl polyoxyethylene ether with the molecular weight of 8000-15000 and maleic acid polyethylene glycol monomethyl ether ester with the molecular weight of 6300-15000 according to the proportion of 6: 1. The compatilizer is a mixture of polydopamine and ethyl silicate according to the mass ratio of 1:1, 1:2 and 2:1 respectively.