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Method for promoting grafting efficiency of acrylate core/shell structure latex particle

An acrylate, core-shell structure technology, applied in the field of polymer chemistry, can solve the problem of low grafting efficiency

Inactive Publication Date: 2006-12-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the generation of graft copolymers in the graft polymerization process is formed by the chain transfer reaction of free radicals, and the main chain of the acrylate polymer is a saturated chain, the grafting efficiency is generally low, usually between 20-30%. between

Method used

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  • Method for promoting grafting efficiency of acrylate core/shell structure latex particle
  • Method for promoting grafting efficiency of acrylate core/shell structure latex particle
  • Method for promoting grafting efficiency of acrylate core/shell structure latex particle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First, add 2.94 g of azo-bis(4-cyano)pentanol and 2.70 g of catalyst triethylamine into a three-necked flask containing a magnetic stirring rotor, then add 25 mL of acetone to completely dissolve it, and place the reaction bottle on ice In a water bath (0° C.), 15 mL of an acetone solution containing 2.50 g of methacryloyl chloride was added dropwise. The reaction was stopped after 20 hours of reaction. The solution turns from colorless and transparent to white, which is washed with water, dried, and solvent removed to obtain a light yellow initiator type monomer, i.e. azo-bis(4-cyano)pentyl dimethacrylate. The yield of the product is rate of 74%, the product's 1 H NMR spectrum as figure 1 As shown, no impurities were found.

[0019] Add 120 parts (weight fraction based on acrylate, the same below) of deionized water and 5 parts of sodium dodecylbenzenesulfonate into the three-necked bottle. Add mixed monomers (acrylic acid ester, ethylene glycol methacrylate and az...

Embodiment 2

[0022] First, add 2.94 g of azo-bis(4-cyano)pentanol and 2.70 g of catalyst triethylamine into a three-necked flask containing a magnetic stirring rotor, then add 30 mL of acetone to completely dissolve it, and place the reaction flask on ice In a water bath (0° C.), 4.00 g of methacryloyl chloride was added dropwise. The reaction was stopped after 10 hours of reaction. The solution changed from colorless and transparent to white, which was washed with water and dried to obtain azo-bis(4-cyano)pentyl dimethacrylate with a yield of 83%.

[0023] Add 140 parts of deionized water and 5 parts of sodium dodecylbenzenesulfonate into the three-necked bottle. Add mixed monomers (acrylic acid ester, methylolpropane triacrylate and azo-bis(4-cyano)pentyl bismethacrylate in a weight ratio of 100 / 1.5 / 0.5) under stirring, and emulsify under nitrogen protection for 10 Minutes later, add 0.6 parts of potassium persulfate (dissolved in 30 parts of deionized water), add 0.10 parts of ferrous...

Embodiment 3

[0026] First, 5.90 g of azo-bis(4-cyano)pentanol and 5.50 g of catalyst pyridine were added to a three-necked flask containing a magnetic stirring rotor, 60 mL of tetrahydrofuran was added, and the reaction flask was placed in an ice-water bath (0°C). 8.00 g of methacryloyl chloride was added dropwise. The reaction was stopped after 18 hours of reaction. It was washed with water and dried to obtain azo-bis(4-cyano)pentyl bismethacrylate with a yield of 83%.

[0027] Add 140 parts of deionized water and 4 parts of sodium dodecylbenzenesulfonate into the three-necked bottle. Add mixed monomers (acrylic acid ester, ethylene glycol methacrylate and azo-bis(4-cyano)pentyl dimethacrylate in a weight ratio of 100 / 1.5 / 2.0) under stirring, and emulsify under nitrogen protection for 10 Minutes later, add 0.7 parts of potassium persulfate (dissolved in 30 parts of deionized water), add 0.15 parts of ferrous sulfate, and 0.08 parts of carved white block. The reaction temperature is 7°C...

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Abstract

The invention relates to a method for increasing grafting efficiency for emulsion particle with acrylate being core-shell, belonging to high molecular chemical field, and especially relating to composite of high molecular compound. The polymer of acrylate core-shell employs cross-linked acrylate rubber polymer as core, the grafting rate of which is low, between 20-30%. The invention comprises following steps: preparing initiator monomer containing azo group for initiating function and polymerisable ethenyl double bond; then, preparing acroleic acid butyl seed latex at low temperature with redox initiating system, employing methacrylic acid gylcol ester or methylol propane triacrylate as crosslinking agent; finally, adding shell monomer, heating, and the azo group breaking into free radical and initiating shell monomer polymerization. The free radical is connected on main chain of polyacrylacid ester with chemical bond, which increases initiating rate; and the two ends of azo monomer is provided with polymerization double bond, which increases grafting efficiency to above 70%.

Description

technical field [0001] The invention belongs to the field of macromolecular chemistry, in particular to the composition of macromolecular compounds. Background technique [0002] The acrylate core / shell structure polymer is a core / shell structure polymer with a cross-linked acrylate rubber-like polymer as the "core" and a plastic-like polymer as the "shell". The basic preparation method is to adopt step-by-step emulsion polymerization method: first prepare seed latex particles by seed emulsion polymerization method, and moderately cross-link in the presence of cross-linking agent, then add other monomers dropwise, and then add water-soluble initiator, so that It is grafted on the surface layer of seed latex particles to prepare a core / shell structure polymer. Since the generation of graft copolymers in the graft polymerization process is formed by the chain transfer reaction of free radicals, and the main chain of the acrylate polymer is a saturated chain, the grafting effi...

Claims

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Application Information

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IPC IPC(8): C08F265/06C08F2/44C08F4/04C08L33/08
Inventor 张秀娟付志峰石艳
Owner BEIJING UNIV OF CHEM TECH
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