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Method for preparing copolymer nano composite material in supercritical CO2

A supercritical, reaction product technology, applied in the production of bulk chemicals, can solve problems such as environmental hazards and large energy consumption, and achieve the effects of improved heat resistance and thermal stability, controllable structure, and large-scale industrial application prospects.

Inactive Publication Date: 2009-05-27
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the polymer melt intercalation method reported in the literature, such as the control factors for the preparation of polymer / layered silicate nanocomposites by the melt intercalation method, has high requirements for the organic surfactant and treatment process of the modified montmorillonite. And the high-temperature melting in the processing process can easily induce the degradation of matrix macromolecules; the polymer solution intercalation method reported in literature such as the research on the preparation of CR / organic vermiculite nanocomposites by solution intercalation method must find a suitable solvent that can dissolve the polymer. However, such methods often involve the use of a large amount of organic solvents, which not only brings great harm to the environment, but also consumes a large amount of energy to remove and treat these solvents

Method used

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  • Method for preparing copolymer nano composite material in supercritical CO2
  • Method for preparing copolymer nano composite material in supercritical CO2
  • Method for preparing copolymer nano composite material in supercritical CO2

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 0.054g of initiator, 0.23g of fluoromontmorillonite, 0.1g of stabilizer, 1.37g of reaction monomer acrylonitrile and 2.863g of styrene into the reaction kettle equipped with a stirring device, then fill with carbon dioxide, discharge, and circulate Three times, to remove the oxygen in the reactor, fill in carbon dioxide, heat the reaction system to 65°C, add carbon dioxide again until the pressure of the system is 25Mpa, start stirring, react for 10 hours, then cool the reactor to 15°C, release carbon dioxide, the reactor was opened to obtain 3.9580 g of the target product.

[0028] The initiator is azobisisobutyronitrile.

[0029] The structural formula of described stabilizer is as follows:

[0030]

[0031] Where: p is 40, q is 40, and n is 40.

[0032] The test results are as follows:

[0033] (1) The monomer conversion rate is 84.42%.

[0034] (2) The molecular weight is 2.18×10 5 g / mol.

[0035] (3) For the measurement results of FT-IR, see figure 1 ...

Embodiment 2

[0041] 0.54g initiator, 0.135g montmorillonite, 0.1g stabilizer, 1.37g reaction monomer acrylonitrile and 2.863g styrene are added in the reaction kettle provided with stirring device, then filled with carbon dioxide, then discharged, and circulated three times, To remove the oxygen in the reactor, fill in carbon dioxide, heat the reaction system to 80°C, add carbon dioxide again until the pressure of the system is 25Mpa, start stirring, react for 10 hours, then cool the reactor to 15°C, release carbon dioxide, The reactor was opened to obtain 3.643 g of the target product.

[0042] Described initiator is dibenzoyl peroxide;

[0043] The structural formula example 1 of the stabilizer, wherein: p is 40, q is 40, and n is 40.

[0044] The test results are as follows:

[0045] (1) The monomer conversion rate is 80.76%.

[0046] (2) The molecular weight is 1.96×10 5 g / mol.

[0047] (3) The measurement result of FT-IR is the same as that of Example 1.

[0048] (4) Small angle...

Embodiment 3

[0051] Adopt the same method as embodiment 1, wherein:

[0052] 0.54g initiator, 0.45g montmorillonite, 0.1g stabilizer, 1.37g reactive monomer acrylonitrile and 2.863g styrene

[0053] The test results are as follows:

[0054] (1) The monomer conversion rate is 78.72%.

[0055] (2) The molecular weight is 2.41×10 5 g / mol.

[0056] (3) The measurement result of FT-IR is the same as that of Example 1.

[0057] (4) Small angle X-ray diffraction analysis results are shown in figure 2 Curve e in.

[0058] (5) The results of thermogravimetric analysis are shown in image 3 Curve i in .

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Abstract

The invention provides a method for preparing copolymer nano-composite materials in supercritical CO2. The method comprises the following steps: an initiator, fluorine-containing montmorillonite, a stabilizer, acrylonitrile as a reactive monomer and styrene are placed in carbon dioxide in a supercritical state, react for 10 to 12 hours, and then are cooled to between 15 and 35 DEG C; pressure is released so as to discharge carbon dioxide; and a target product is collected from reaction products. The method has the advantages that the monomer conversion rate of the nano-composite materials prepared by the method can reach more than 80 percent; both the heat resistance and thermal stability of the nano-composite materials are greatly improved; the molecular weight of the target product can be up to 10<5>g / mol; and the product is controllable in structure, narrow in molecular weight distribution and larger in industrial application prospects. The structural formula of the stabilizer is shown in a figure.

Description

technical field [0001] The present invention relates to the method for preparing poly(styrene-acrylonitrile) / fluorine-containing montmorillonite nanocomposite material, especially relate to supercritical CO 2 Method for preparing poly(styrene-acrylonitrile) / montmorillonite nanocomposites. Background technique [0002] Poly(styrene-acrylonitrile) / montmorillonite nanocomposite material, referred to as (PSAN / MMT) nanocomposite material, is a material obtained by intercalating poly(styrene-acrylonitrile) to montmorillonite. At present, there have been many literature reports on the preparation method of montmorillonite intercalation materials related to high molecular polymer materials), but there are some defects in the current methods. For example, the polymer melt intercalation method reported in the literature, such as the control factors for the preparation of polymer / layered silicate nanocomposites by the melt intercalation method, has high requirements for the organic su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/10C08F2/00C08F2/44C08K3/34
CPCY02P20/54
Inventor 董擎之王晶孙扶
Owner EAST CHINA UNIV OF SCI & TECH