Preparation method of spherical crosslinked polyacrylic resin

A technology for cross-linking polyacrylic acid and acrylic monomers, which is applied in the field of preparation of spherical cross-linked polyacrylic resin, can solve the problems of irregular shape of resin products, wide product particle size distribution, poor environmental protection, etc. Consistent quality, easy-to-remove effect

Inactive Publication Date: 2015-04-08
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Xylene is a highly toxic organic solvent, which makes the production process less environmentally friendly
Although this method can obtain granular products, the method is cumbersome to operate through the later gelation process, further drying, crushing, and grading and sieving processes; in addition, the resin product obtained by crushing has irregular shapes and wide particle size distribution.
Patent CN102504079A discloses a preparation method of spherical polyacrylic resin, which can prepare a spherical acrylic resin thickener with a diameter of 100-400 μm, but the core of the method is still reverse suspension polymerization

Method used

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  • Preparation method of spherical crosslinked polyacrylic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Add 500 g of ethyl acetate to a 2000 ml four-neck flask equipped with a thermometer, reflux condensing device, and mechanical stirring device; under nitrogen protection, add 150 g of acrylic acid monomer, and stir evenly; in an ice-water bath, at a stirring rate of 300 rpm, add hydrogen Sodium oxide 0.42g, stir until completely dissolved; at a stirring rate of 300rpm, add 2.8g of cross-linking agent N,N-methylenebisacrylamide and 4.7g of triethylene glycol dimethacrylate, stir evenly; At a speed of 300rpm, add 15g of surfactant XP70 and stir for 10min; at a stirring speed of 500rpm, add 7.5g of initiator LPO and stir evenly; increase the stirring speed to 800rpm, raise the temperature of the reaction system to 78°C, and Polymerization was carried out for 3 hours. After cooling down to room temperature, filter under reduced pressure, wash twice with 100g of hot ethyl acetate at 50-60°C; dry under reduced pressure at 40°C to constant weight to obtain spherical crosslinked...

Embodiment 2

[0055] Add 450g of ethyl acetate and 50g of absolute ethanol to a 2000ml four-neck flask equipped with a thermometer, reflux condensing device, and mechanical stirring device, and stir evenly; under nitrogen protection, add 148.8g of acrylic acid monomer, and stir evenly; At a stirring rate of 200rpm, add 0.074g of sodium carbonate and stir until completely dissolved; at a stirring rate of 200rpm, add 18.2g of polymerizable monomer polyethylene glycol acrylate (n=8) and 8.1 g of isooctyl methacrylate g; at a stirring rate of 200rpm, add 1.75g ​​of cross-linking agent allyl sucrose ether, and stir evenly; add 14g of surfactant C8EO7, stir for 10min, and mix well; at a stirring rate of 600rpm, add 4.4g of initiator AVBN, and stir uniform. The stirring rate was increased to 700 rpm, the temperature of the reaction system was raised to 71° C., and the polymerization reaction was carried out at this temperature for 4 hours. After cooling down to room temperature, filter under redu...

Embodiment 3

[0057] Add 497.5 g of ethyl acetate and 2.5 g of deionized water into a 2000 ml four-neck flask with a thermometer, reflux condensing device, and mechanical stirring device, and stir evenly; under nitrogen protection, add 39.2 g of acrylic acid monomers, and stir evenly; In an ice-water bath, at a stirring rate of 200 rpm, add 6.1 g of potassium hydroxide and stir until completely dissolved; at a stirring rate of 200 rpm, add 0.8 g of copolymerized monomer methyl methacrylate; at a stirring rate of 300 rpm, add crosslinking Agent ethylene glycol dimethacrylate 0.8g, stir well; at a stirring rate of 300rpm, add 1.2g of surfactant C13E7, stir for 10min, mix well; at a stirring rate of 550rpm, add initiator AIBN 0.48g, stir well ; Increase the stirring rate to 600rpm, raise the temperature of the reaction system to 65°C, and conduct a polymerization reaction at this temperature for 8 hours. After cooling down to room temperature, filter under reduced pressure, rinse twice with 10...

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Abstract

The invention discloses a preparation method of spherical crosslinked polyacrylic resin. The preparation method comprises the following steps: adding ethyl acetate or the mixed solvent composed of ethyl acetate and other solvents in a reactor as a reaction medium, adding an acrylic monomer in the reaction medium under the protection of nitrogen, adding alkaline substances in a reaction system, then sequentially adding a crosslinker, a surfactant and an initiator, and then heating to a reaction temperature and reacting; after the polymerization reaction is ended, cooling the reaction system to a room temperature, filtering, washing the filter cake by hot ethyl acetate, and drying to obtain the spherical polyacrylic resin. The preparation method disclosed by the invention has the advantages of being simple and convenient to operate, and high in product purity.

Description

technical field [0001] The invention relates to a preparation method of spherical crosslinked polyacrylic acid resin. Background technique [0002] Polymers composed of acrylic acid and its salts or esters have a wide variety of uses. Such polymers include homopolymers of acrylic acid or copolymers of acrylic acid with a maximum content of about 15% by mass of comonomer. Typical monomers involved might be acrylic acid, methacrylic acid, alkyl acrylates, alkyl methacrylates, acrylamide, etc., or other polymerizable monomers with similar structures. The cross-linked polyacrylic resin is a moderate polyol composed of a compound having two or more ethylenically unsaturated groups or a disubstituted or more allyl ether cross-linking agent of such a polyol and an acrylic monomer. Cross-linked acrylic / ester copolymer. [0003] As a water-swellable thickener or rheology modifier, cross-linked polyacrylic resin is usually used to adjust the viscosity of liquid or emulsion, improve...

Claims

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Application Information

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IPC IPC(8): C08F220/06C08F222/36C08F222/20C08F220/28C08F220/18C08F222/14C08F220/14C08F220/56C08F216/12C08F2/14
Inventor 张威王万绪杜志平马晓原李萍
Owner CHINA RES INST OF DAILY CHEM IND
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