Method for preparing solid acrylic acid copolymer

A technology of solid acrylic acid and copolymer, which is applied in the field of preparation of solid acrylic acid copolymer, which can solve the problems of environmental pollution, energy consumption and time-consuming, and achieve the effects of broad application prospects, shortened reaction time and simple method

Inactive Publication Date: 2011-02-16
TAIYUAN UNIV OF TECH
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  • Claims
  • Application Information

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Problems solved by technology

It is an energy-consuming and time-consuming process, and it is easy to cause environmental pollution; the publication number is CN101096394, which discloses the invention patent of "a polyacrylic acid material containing siloxane group and its synthesis technology", using supercritical carbon dioxide as the medium, Preparation of a polyacrylic acid material containing siloxane groups

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  • Method for preparing solid acrylic acid copolymer

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preparation example Construction

[0020] A preparation method of a solid acrylic acid copolymer, wherein the method is to rapidly prepare a hydrophobically associative solid acrylic acid copolymer in supercritical carbon dioxide, and the reaction medium is supercritical carbon dioxide. The polymer monomers used are explosively polymerizable in supercritical carbon dioxide, or can be explosively polymerized with another monomer or monomers. It is one or more of acrylic acid, long-chain acrylic acid ester, and vinylpyrrolidone, styrene, and acrylamide. The polymers prepared in the present invention may be di- or terpolymers. The specific steps and process conditions are as follows:

[0021] Add acrylic acid, long-chain acrylic acid ester, and one of styrene, vinylpyrrolidone, and acrylamide into the autoclave. The acrylic acid, long-chain acrylic acid ester, and comonomer are in a molar ratio of 0.5-99.5:0.5-20:0.5-99.5, and then an initiator of 0.1-4.0 wt% of the total monomer weight is added. Put in a magne...

specific Embodiment approach 1

[0027] The invention proposes a method for rapidly preparing hydrophobically associative solid acrylic copolymer in supercritical carbon dioxide.

[0028] Weigh 2.0 g of acrylic acid, 0.021 g of initiator azobisisobutyronitrile, 0.12 g of octadecyl acrylate, and 0.1 g of vinylpyrrolidone into a 20 mL stainless steel autoclave, put in a magnetic stirrer, and seal; slowly fill in The carbon dioxide was reduced to 4Mpa, the air inlet was closed, and the air in the kettle was exhausted. Pour carbon dioxide into the autoclave with a high-pressure metering pump, increase the pressure of carbon dioxide to 9Mpa, then close the inlet and outlet valves, and heat in a water bath. Start the magnetic stirring, heat the water bath to 60°C, and when the temperature rises to the predetermined value of 60°C, if the pressure does not reach the predetermined value of 16Mpa, add or release carbon dioxide to make the pressure reach the required pressure. After 30 minutes of reaction, the system e...

specific Embodiment approach 2

[0030] Weigh 1.5 g of acrylic acid, 0.021 g of initiator azobisisobutyronitrile, 0.1 g of octadecyl acrylate; 0.5 g of vinylpyrrolidone was added to a 20 mL stainless steel autoclave, placed in a magnetic stirring bar, and sealed; slowly filled Carbon dioxide to 2Mpa, close the air inlet, and exhaust the air in the kettle. Pour carbon dioxide into the autoclave with a high-pressure metering pump, increase the pressure of carbon dioxide to 10Mpa, then close the inlet and outlet valves, and heat in a water bath. Start the magnetic stirring, heat the water bath to 60°C, and when the temperature rises to the predetermined value of 60°C, if the pressure does not reach the predetermined value of 18Mpa, add or release carbon dioxide to make the pressure reach the required pressure. After 15 minutes of reaction, the system exploded. In order to avoid the excessive increase of the pressure of the reactor by the explosion reaction, the reactor was cooled by water, and after the pressur...

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Abstract

The invention discloses a method for preparing a solid acrylic acid copolymer, which comprises the following steps of: adding acrylic acid, acrylic acid long-chain ester and copolymerization monomer into a reaction kettle in a molar ratio of 0.5-99.5: 0.5-20: 0.5-99.5, adding an initiator in an amount which is 0.1 to 4.0 weight percent of the total weight of the reactants into the reaction kettle, introducing carbon dioxide of 9 to 16MPa into the reaction kettle, stirring the mixture, heating the mixture to between 45 and 90 DEG C, reacting the mixture under the pressure of 14 to 19MPa for 10 to 120 minutes, releasing the carbon dioxide to obtain a white powdery product after the pressure in the reaction kettle is constant, and finally performing in-situ extraction at the temperature of between 30 and 60 DEG C under the pressure of 8 to 16MPa by using the carbon dioxide till the product has constant weight so as to obtain the solid acrylic acid copolymer. The conversion rate of the polymer is over 95 percent, and the solid acrylic acid copolymer is applied in the fields of daily necessities, food, cosmetics, medicaments and the like with high material purity requirements.

Description

technical field [0001] The invention relates to a preparation method of a solid acrylic acid copolymer, in particular to a method for rapidly preparing a hydrophobically associated solid acrylic acid copolymer in supercritical carbon dioxide. Background technique [0002] The existing hydrophobically associative acrylic copolymers are mainly liquid products of solution polymerization and emulsion polymerization, and the preparation of solid acrylic copolymers is an important development direction of acrylic copolymers. Compared with liquid acrylic copolymers, solid acrylic copolymers have the advantages of convenient storage and transportation, low transportation cost, good storage and transportation process safety, and high active ingredients. Therefore, the research on the synthesis methods and properties of water-soluble solid acrylic copolymers has important practical significance. [0003] Hydrophobically associative water-soluble polymers refer to polymers prepared by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/56C08F220/06C08F226/10C08F212/08C08F220/18C08F2/00
Inventor 张怀平陈鸣才王宝成曹青高峰卫英慧
Owner TAIYUAN UNIV OF TECH
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