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Free radical-controllable RAFT soap-free emulsion polymerization method for hydroxy acrylic resin

A free radical hydroxyacrylic acid, soap-free emulsion polymerization technology, applied in the direction of coating, etc., can solve the problems of paint film adhesion, water resistance and gloss reduction, poor bonding force between resin and substrate, etc., and achieve a wide range of polymerization monomer adaptation Sexuality, easy synthesis, and the effect of preventing polymerization inhibition

Pending Publication Date: 2021-04-09
HUNAN AEROSPACE SANFENG SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the hydroxyacrylic emulsion prepared by traditional emulsion polymerization contains more small molecule emulsifiers, the emulsifiers will migrate to the surface of the film during the drying process of the paint film, resulting in poor bonding between the resin and the substrate, and poor film adhesion, water resistance and Gloss reduction

Method used

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  • Free radical-controllable RAFT soap-free emulsion polymerization method for hydroxy acrylic resin
  • Free radical-controllable RAFT soap-free emulsion polymerization method for hydroxy acrylic resin
  • Free radical-controllable RAFT soap-free emulsion polymerization method for hydroxy acrylic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. "One-pot method" RFAT solution polymerization to prepare regular amphiphilic block copolymer macromolecular RAFT reagents:

[0038] The hydrophilic monomer is acrylic acid and hydroxyethyl methacrylate, the hydrophobic monomer is styrene, and the RAFT reagent is S-n-dodecyl-S'-(α,α'-dimethyl-α'' -Acetoxy)trithiocarbonate (DDMAT), the initiator is 4,4'-azobis(cyanovaleric acid) (V501), the solvent is 1,4-dioxane, and its composition formula is as follows :

[0039]

[0040] Concrete preparation process is as follows:

[0041] (1) Add 5.46 g of RAFT reagent DDMAT into a four-necked round bottom flask, stir and dissolve it in 184.26 g of 1,4-dioxane solvent, and inject N 2 Divide O 2 After 30 min, the temperature was raised to 80 °C; then 0.42 g of oil-soluble initiator V501 was fully dissolved in an appropriate amount of solvent, and then mixed with 21.6 g of acrylic acid and 65.07 g of hydroxyethyl methacrylate two hydrophilic unsaturated monomers in parallel A...

Embodiment 2

[0053] 1. "One-pot method" RFAT solution polymerization to prepare regular amphiphilic block copolymer macromolecular RAFT reagents:

[0054] The hydrophilic monomer is acrylic acid and hydroxyethyl methacrylate, the hydrophobic monomer is isooctyl methacrylate, and the RAFT reagent is S-n-dodecyl-S'-(α,α'-dimethyl -α''-acetoxy)trithiocarbonate (DDMAT), the initiator is 4,4'-azobis(cyanovaleric acid) (V501), the solvent is 1,4-dioxane, and The component formula is as follows:

[0055]

[0056] Concrete preparation process is as follows:

[0057] (1) Add 5.46 g of RAFT reagent DDMAT into a four-necked round bottom flask, stir and dissolve it in 184.26 g of 1,4-dioxane solvent, and inject N 2 Divide O 2 After 30 min, the temperature was raised to 80 °C; then 0.42 g of oil-soluble initiator V501 was fully dissolved in an appropriate amount of solvent, and then mixed with 21.6 g of acrylic acid and 65.07 g of hydroxyethyl methacrylate two hydrophilic unsaturated monomers in ...

Embodiment 3

[0069] 1. "One-pot method" RFAT solution polymerization to prepare regular amphiphilic block copolymer macromolecular RAFT reagents:

[0070] The hydrophilic monomers are acrylic acid and hydroxyethyl methacrylate, and the RAFT reagent is S-n-dodecyl-S'-(α,α'-dimethyl-α''-acetoxy) trithiocarbonic acid Ester (DDMAT), the initiator is 4,4′-azobis(cyanovaleric acid) (V501), the solvent is 1,4-dioxane, and its composition formula is as follows:

[0071]

[0072] Concrete preparation process is as follows:

[0073] (1) Add 5.46 g of RAFT reagent DDMAT into a four-necked round bottom flask, stir and dissolve it in 184.26 g of 1,4-dioxane solvent, and inject N 2 Divide O 2 After 30 min, the temperature was raised to 80 °C; then 0.42 g of oil-soluble initiator V501 was fully dissolved in an appropriate amount of solvent, and then mixed with 21.6 g of acrylic acid and 40 g of hydroxyethyl methacrylate two hydrophilic unsaturated monomers in parallel Add it dropwise into a round b...

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PUM

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Abstract

The invention discloses a free radical-controllable RAFT soap-free emulsion polymerization method for hydroxy acrylic resin, belonging to the technical field of RAFT emulsion polymerization. The method comprises the following steps: firstly, preparing an amphiphilic block copolymer macromolecular RAFT reagent with a regular structure from two monomers with different hydrophilicity and hydrophobicity through a one-pot-process RAFT solution polymerization technology, self-assembling the amphiphilic macromolecular RAFT reagent in water under the action of a neutralizer to obtain a micelle, then adding a required acrylate monomer and a water-soluble initiator, and carrying out emulsion polymerization to prepare a hydroxy acrylic resin emulsion. The amphiphilic block copolymer macromolecular RAFT reagent prepared by the invention not only can be used as an RAFT reagent to regulate and control polymerization, but also functions as an emulsifier, so adverse effects of emulsifier micromolecules on a paint film are avoided, and the water resistance of the paint film is improved. Hydroxyl groups are introduced in the preparation process of the amphiphilic block copolymer macromolecular RAFT reagent, so the macromolecular RFAT reagent which does not participate in the reaction can react with a curing agent in the curing process of the paint film, thereby enhancing the properties of the paint film. Moreover, the method is controllable in polymerization process, simple to operate, low in VOC and high in polymerization rate, and belongs to an environment-friendly preparation process.

Description

technical field [0001] The invention relates to the field of emulsion polymerization, in particular to an amphiphilic macromolecular RAFT agent, a preparation method thereof and an application in a soap-free emulsion polymerization method of hydroxyacrylic resin. Background technique [0002] In recent years, with the enhancement of public awareness of environmental protection and the implementation of relevant national policies, the use of traditional solvent-based coatings has been increasingly restricted. Water-based coatings with the advantages of non-toxic, non-flammable, environmentally friendly, green and energy-saving are the current development trend of the coatings industry. Water-based acrylic resin has the characteristics of excellent film-forming properties, good weather resistance, excellent color and gloss retention, and is widely used in the coating of exterior walls, wood, metal, plastic and glass. [0003] Waterborne hydroxyacrylate dispersions are divided...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/18C08F220/14C08F2/38C09D153/00
CPCC08F2/38C08F220/14C08F293/005C08F2438/03C09D153/00C08F220/1804
Inventor 徐常利李著初杨艺聪
Owner HUNAN AEROSPACE SANFENG SCI & TECH CO LTD
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