Siloxane group containing polyacrylic acid material and synthesizing technique thereof

The technology of siloxane acrylate and siloxane group is applied in the field of polyelectrolyte preparation, which can solve the problems of solvent toxic operation, product pollution, environmental pollution and the like, and achieve the effects of easy polymerization reaction, easy separation and purification, and low price.

Inactive Publication Date: 2009-12-09
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the suspension, dispersion, and precipitation polymerization in organic solvents require the separation of the product and the solvent after the reaction, which is an energy-consuming and time-consuming process.
Moreover, the toxicity and flammability of solvents bring inconvenience to the operation, and the volatilization and discharge of various organic solvents have caused serious pollution to the environment, and the products will also be polluted.

Method used

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  • Siloxane group containing polyacrylic acid material and synthesizing technique thereof
  • Siloxane group containing polyacrylic acid material and synthesizing technique thereof
  • Siloxane group containing polyacrylic acid material and synthesizing technique thereof

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Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0033] The synthetic technology that the present invention proposes in supercritical carbon dioxide contains siloxane group acrylic acid material, raw material acrylic acid (AA) is analytically pure, decompression distillation removes polymerization inhibitor; Initiator is azobisisobutyronitrile (AIBN) , recrystallized with methanol; siloxane monomer vinyltriethoxysilane (Wuda Organic Silicon Company), not processed.

[0034] Synthetic technical steps and processing conditions are as follows:

[0035] step one:

[0036] Weigh 2.1g of acrylic acid, 0.05g of vinyltriethoxysilane, 0.25g of butyl acrylate, and 0.021g of azobisisobutyronitrile into a 20mL stainless steel autoclave to seal;

[0037] Step two:

[0038] First inject carbon dioxide to about 5MPa, pause for 30 seconds, slowly deflate and discharge the air in the kettle, repeat 2 to 3 times; then inject carbon dioxide with a high-pressure metering pump to a pressure of 16MPa, close the intake valve; start the magnetic ...

Embodiment approach 2

[0043] The raw material acrylic acid (AA) is analytically pure, and the polymerization inhibitor is removed by distillation under reduced pressure; the initiator is azobisisobutyronitrile (AIBN), which is recrystallized with methanol; octadecyl acrylate is purchased from Aldrich Company without treatment; Alkane monomer vinyl triethoxysilane (Wuhan Silicone Co., Ltd.), not processed;

[0044] Synthetic technical steps and processing conditions are as follows:

[0045] step one:

[0046] Weigh 2.1g of acrylic acid, 0.021g of azoisobisbutyronitrile, 0.2333g of octadecyl acrylate, and 0.04g of vinyltriethoxysilane into a 20mL stainless steel autoclave to seal;

[0047] Step two:

[0048] First inject carbon dioxide to about 6MPa, pause for 10 seconds, slowly deflate and discharge the air in the kettle, repeat 2 to 3 times; then inject carbon dioxide with a high-pressure metering pump to a pressure of 14MPa, close the intake valve; start the magnetic stirrer, and at the same tim...

Embodiment approach 3

[0053] The raw material acrylic acid (AA) is analytically pure, and the polymerization inhibitor is removed by distillation under reduced pressure; the initiator is azobisisoheptanonitrile, which is recrystallized with methanol; Purchased from Aldrich Company without processing;

[0054] Synthetic technical steps and processing conditions are as follows:

[0055] step one:

[0056] Weigh 2.0g of acrylic acid, 0.021g of azobisisoheptanonitrile, 0.2333g of hexadecyl acrylate, and 0.05g of vinylhexyltrimethoxysilane into a 20mL stainless steel autoclave to seal;

[0057] Step two:

[0058] First inject carbon dioxide to about 6MPa, pause for 20S, slowly deflate and discharge the air in the kettle, repeat 2 to 3 times; then inject carbon dioxide with a high-pressure metering pump to a pressure of 15MPa, close the intake valve; start the magnetic stirrer, and at the same time Gradually raise the temperature to 60°C and react for 6 hours. After the reaction is over, cool the reac...

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Abstract

The invention provides a polyacrylic acid material with oxosilane and the synthesis technology. The material is the polymer of acrylic acid and vinylsiloxane or acrylic ester with oxosilane and acrylic ester. The synthesis technique comprises the following steps: adding acrylic acid and vinylsiloxane or acrylic ester with oxosilane and acrylic ester according to 0.5-99.5:0.1-99.5:0-99.5 in the autoclave; adding 0.01-5.0wt% initiating agent; controlling the pressure of carbon dioxide at 8-25MPa; heating to 40-100Deg. C; reacting for 2-8 hours; extracting the product to the constant weight with carbon dioxide in the original position. The invention solves the difficult problem that the organic oxosilane monomer can't be grafted to the backbone chain, which has the food quality product and no pollution, can be used for tertiary oil extraction, the conversion of solar energy, the water treatment, emulsion paint, soil improvement, food and medical purpose.

Description

technical field [0001] The invention relates to a preparation technology of polyelectrolyte, in particular to a polyacrylic acid material containing siloxane groups in supercritical carbon dioxide and its synthesis technology. Background technique [0002] Water-soluble polymer products are widely used in tertiary oil recovery, solar energy conversion, water treatment, latex paint, food, soil improvement, film and frictional drag reduction, and water-based paint, ink, cosmetics, papermaking, pharmaceutical preparations or textile printing and dyeing. In order to impart some special properties to water-soluble polymers, it is often achieved by means of copolymerization, cross-linking, and association. [0003] Since the polarities of water-soluble monomers and oil-soluble monomers are very different, the incompatibility of the two makes the polymerization process very complicated. The micellar copolymerization method, inverse microemulsion polymerization method, and soap-fre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/06C08F4/04C08F4/34C08F4/40
CPCY02P20/54
Inventor 陈鸣才张怀平许凯刘鹏祝纶宇陈德宏
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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