Preparation method of powdery polyacrylic acid thickener

A technology of polyacrylic acid and thickener, which is applied in the field of preparation of powdered polyacrylic acid thickener, which can solve the problems of inconvenient production and easy volatilization, and achieve the effects of fast dissolution, low solvent toxicity and improved thickening ability

Inactive Publication Date: 2013-07-03
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the alcohol solvent has the effect of dissolving and swelling the acrylic thickener, it cannot be selected; the organic solvent with a lower boiling point is easy to volatilize during the reaction process, and the reaction needs to be carried out in an autoclave, which brings inconvenience to production, and the boiling point is higher. The organic solvent needs to be dried and removed at a higher temperature, and cannot be used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 200 mL of ethyl acetate, 35 g of acrylic acid, 5 g of ethyl methacrylate, and 0.07 g of pentaerythritol triallyl ether into a 500 mL four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, and pass nitrogen gas for 30 min. Start stirring, raise the temperature to 70°C, dissolve 0.14g of lauryl peroxide in 6ml of ethyl acetate, use a normal pressure funnel to add dropwise within 15 to 17 minutes, then add 2g of sodium bicarbonate to ease the polymerization reaction and control the reaction The temperature is 71-73°C, and the reaction is kept for 4 hours after the initiator is completely dropped. Cool to room temperature, filter, wash twice with ethyl acetate, remove unreacted raw materials in the polymer by suction filtration, place the filter cake in a porcelain dish, and dry in vacuum at 45°C for 24 hours to obtain a white powder with a yield of 96.8 %; its average particle size distribution is about 0.5μm, the dissolution time of its 0.5% a...

Embodiment 2

[0033] Add 150 mL of ethyl acetate and 100 mL of cyclohexane, 30 g of methacrylic acid, 14 g of butyl acrylate, and 0.28 g of trimethylolpropane into a 500 mL four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser. Acrylic acid ester, blow nitrogen for 30min, start stirring, raise the temperature to 70°C, dissolve 0.35g of dibenzoyl peroxide in 14ml of ethyl acetate, drop it in 20-23min with a normal pressure funnel, then add 3g of triethanolamine , to ease the polymerization reaction, control the reaction temperature at 73-75°C, wait until the initiator is completely dripped and keep warm for 5 hours. Cool to room temperature, filter, wash 3 times with cyclohexane to remove unreacted raw materials in the polymer, filter with suction, place the filter cake in a porcelain plate, and dry in vacuum at 40°C for 30h to obtain a white fine powder. Its average particle size distribution is about 0.4μm, the dissolution time of its 0.5% aqueous solution is 397s,...

Embodiment 3

[0035]Add 150 mL of ethyl acetate, 80 mL of n-hexane, 40 g of butenedioic acid, 2 g of lauryl acrylate, and 0.28 g of pentaerythritol triallyl ether in a 500 mL four-necked flask equipped with a stirrer, a thermometer, and a reflux condenser. , blow nitrogen for 30min, start stirring, raise the temperature to 50°C, dissolve 0.56g of azobisisobutyronitrile in 23ml of ethyl acetate, add dropwise in 25-27min with a normal pressure funnel, then add 3.5g of sodium bicarbonate and 1g of sodium hydroxide moderates the polymerization reaction, controls the reaction temperature at 56-58°C, waits until the initiator is completely dripped and keeps warm for 5 hours. Cool to room temperature, filter, wash twice with ethyl acetate, remove unreacted raw materials in the polymer, filter with suction, place the filter cake in a porcelain plate, and dry in vacuum at 50°C for 36 hours to obtain a white fine powder. The yield Its average particle size distribution is about 0.6μm. The dissolution...

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Abstract

A preparation method of a powdery polyacrylic acid thickener comprises the following steps: at room temperature, adding organic solvent, polymeric monomers, comonomers, neutralizers and cross linking agents in a reaction kettle in sequence, introducing nitrogen to remove all oxygen, starting stirring to cause the reactants to be uniformly mixed, rising the temperature to the reaction temperature, dissolving initiators in the organic solvent having the same reaction system as the initiators, dripping off for 15-30 min, preserving the reaction temperature for 3-6 hours, cooling, filtering, washing with the organic solvent, removing unreacted raw materials in the product, and vacuum-drying a filter cake for 24-48 hours at the temperature of 40-50 DEG C to obtain white powder. The preparation method has the advantages of simple preparation process, environmental friendliness, low energy consumption and low cost.

Description

technical field [0001] The invention belongs to a preparation method of a powdery polyacrylic acid thickener. Background technique [0002] Since the polyacrylic acid thickener Carbomer 934 was introduced into the market in 1953, it has been widely used in coatings, textiles, pharmaceuticals, building materials, detergents and cosmetics. In recent years, with the needs of modern industry, acrylic thickeners have developed rapidly, and the development and application of new synthesis methods have attracted the attention of scientific and technological workers. [0003] At present, the preparation methods of polyacrylic acid thickener mainly adopt three kinds of emulsion polymerization method, inverse emulsion polymerization method and precipitation method. The reaction speed of the emulsion polymerization method is faster, the molecular weight of the polymer is higher, the viscosity of the material is low, it is easy to transfer heat and mix, and the production is easy to co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/06C08F222/02C08F220/18C08F2/06
Inventor 王万绪马晓原杜志平张威台秀梅
Owner CHINA RES INST OF DAILY CHEM IND
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