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Method for making 1,1-difluoroethylene polymer

A technology of vinylidene fluoride and a manufacturing method, applied in 1 field, can solve the problems of complicated polymerization operation, increased equipment cost burden, temperature rise above critical temperature, etc., and achieves the effects of high bulk density and easy scale coverage

Inactive Publication Date: 2012-10-10
KUREHA KAGAKU KOGYO KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production method of this 1,1-vinylidene fluoride polymer requires strict temperature control
In addition, a method of obtaining a polymer with a high apparent specific gravity by adding additional monomers is disclosed, but in addition to using a high-pressure pump to feed the monomers, it is necessary to raise the temperature above the critical temperature, which increases the burden of equipment costs and complicates the polymerization operation. question

Method used

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  • Method for making 1,1-difluoroethylene polymer
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  • Method for making 1,1-difluoroethylene polymer

Examples

Experimental program
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Embodiment

[0061] Hereinafter, examples are given to further describe the present invention in detail, but the present invention is not limited to the examples.

[0062] The physical properties of the vinylidene fluoride polymer powders obtained in Examples and Comparative Examples were measured by the following methods.

[0063] 〔Inherent viscosity〕

[0064] 4 g of 1,1-vinylidene fluoride polymer powder was added to 1 liter of N,N-dimethylformamide, and a solution was prepared for dissolving at 80° C. for 8 hours. This solution was kept at 30° C., the logarithmic viscosity was measured with an Ubbelohde viscometer, and the inherent viscosity was obtained from the following formula. Logarithmic viscosity [η] = ln (η rel ) / C

[0065] Among them, η rel Indicates the number of falling seconds of the sample solution / the number of falling seconds of the solvent, and C represents the concentration of the sample solution (0.4g / dl).

[0066] 〔SEM observation〕

[0067] The 1,1-vinylidene fl...

Embodiment 1

[0083] 1024g of ion-exchanged water, 0.4g of methylcellulose, 0.2g of sorbitan trioleate (span85, referring to the following formula (1)), 400g of 1,1- Ethylene difluoride, 0.6 g of diisopropyl peroxydicarbonate (IPP), and 1.8 g of ethyl acetate were subjected to suspension polymerization at 26° C. for 31 hours. The polymerization yield of the suspension polymerization was 89%.

[0084] After the polymerization, the polymer slurry was heat-treated at 95°C for 30 minutes, dehydrated, washed with water, and dried at 80°C for 20 hours to obtain vinylidene fluoride polymer powder (1).

[0085] The obtained 1,1-difluoroethylene polymer powder (1) had an inherent viscosity of 3.1 dl / g, an average particle diameter of 150 μm, and a bulk density of 0.46 g / cm 3 . In addition, the SEM photograph of the cross section of the vinylidene fluoride polymer powder (1) is shown in figure 2 .

[0086]

Embodiment 2

[0088] 1024g of ion-exchanged water, 0.2g of methyl cellulose, 0.4g of sorbitan trioleate (span85), 400g of 1,1-difluoroethylene, 0.6g of peroxide were put into an autoclave with an inner volume of 2 liters. Diisopropyl dicarbonate (IPP), 1.8 g of ethyl acetate, and suspension polymerization at 26° C. for 79 hours. The polymerization yield of the suspension polymerization was 89%.

[0089] After the polymerization, the polymer slurry was heat-treated at 95°C for 30 minutes, dehydrated, washed with water, and dried at 80°C for 20 hours to obtain vinylidene fluoride polymer powder (2).

[0090] The obtained 1,1-difluoroethylene polymer powder (2) had an inherent viscosity of 3.1 dl / g, an average particle diameter of 220 μm, and a bulk density of 0.53 g / cm 3 . In addition, the SEM photograph of the cross section of 1,1-vinylidene fluoride polymer powder (2) is shown in image 3 .

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Abstract

The invention provides a method for making a 1,1-difluoroethylene polymer to obtain the 1,1-difluoroethylene polymer being high in bulk density without increasing auxiliary devices and the scale covering in a polymerization system. The method for making the 1,1-difluoroethylene polymer comprises that a monomer taking the 1,1-difluoroethylene polymer as the main content is dispersed in an aqueous medium containing suspension to be subjected to suspension polymerization. Therefore, the method is characterized in that the suspension polymerization is carried out under the existing of polyoxyethylene sorbitan fatty acid ester having a hydrophilic-lipophilic balance value (HLB) in the range of 1-8.

Description

technical field [0001] The present invention relates to a method for producing vinylidene fluoride polymers, and more specifically, to a method for producing vinylidene fluoride polymers with a high bulk density. Background technique [0002] 1,1-Difluoroethylene-based polymers are excellent in chemical resistance, weather resistance, stain resistance, etc., and can be used as materials for producing various films and molded articles after melt molding. In addition, 1,1-vinylidene fluoride polymers can also be used as resins for coatings or adhesives. [0003] 1,1-Difluoroethylene-based polymers can be synthesized by various polymerization methods, but in industrial production, they are synthesized by emulsion polymerization or suspension polymerization. In the emulsion polymerization method, since latex with a small particle size of about 0.2 to 0.5 μm is produced, granulation treatment using a coagulant is performed after polymerization, but complicated post-treatment is ...

Claims

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Application Information

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IPC IPC(8): C08F214/22C08F2/20
Inventor 五十岚民人武藤慎太郎堀江胜雄菅原绘美
Owner KUREHA KAGAKU KOGYO KK
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