Epoxidation method of gel-free double bond-contained polymer

A polymer and epoxidation technology, which is applied in the field of epoxidation of gel-free polymers containing double bonds, can solve the problem of affecting the economic benefits of the epoxidation process, slowing down the epoxidation reaction speed, and increasing the amount of hydrogen peroxide And other problems, to achieve high yield, high epoxy value, good solubility

Inactive Publication Date: 2009-09-23
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this improvement measure will slow down the epoxidation reaction speed. In order to achieve a high epoxidation conversion rate, it is ne

Method used

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  • Epoxidation method of gel-free double bond-contained polymer
  • Epoxidation method of gel-free double bond-contained polymer
  • Epoxidation method of gel-free double bond-contained polymer

Examples

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Effect test

Embodiment 1

[0021] Dissolve styrene-butadiene rubber (Mn=3.5×10 5 ) to form a 15%wt styrene-butadiene rubber solution. Take 100g of the above-mentioned styrene-butadiene rubber solution, add 0.3g of benzyltrimethylammonium chloride, 7.6mL of formic acid, form a uniform solution, heat up to 40°C, and slowly add 10mL of 30% (v / v) hydrogen peroxide dropwise. Insulate at 40°C for 1 hour, then raise the temperature to 60°C for 5 hours. After the reaction, wash with deionized water four times, separate the organic layer with a separatory funnel, and remove toluene under reduced pressure to obtain epoxidized styrene-butadiene rubber.

[0022] The double bond conversion rate of epoxidized styrene-butadiene rubber was 76.3%, and the extraction residual rate was 1.34%.

Embodiment 2

[0024] Butadiene rubber (Mn=1.1×10 5 ) to form a 10%wt butadiene rubber solution. Take 100g of the above solution, add 1.2g of N-dimethylimidazole chloride and 4.5mL of formic acid to form a homogeneous solution, heat up to 40°C, and slowly add 20mL of 15% (v / v) hydrogen peroxide dropwise. Insulate at 40°C for 2h, then raise the temperature to 65°C for 4h. After the reaction, wash with deionized water for 4 times, separate the organic layer with a separatory funnel, and remove the cyclohexane under reduced pressure to obtain epoxidized butadiene rubber.

[0025] The double bond conversion rate of epoxidized butadiene rubber was 81.3%, and the extraction residual rate was 3.26%.

Embodiment 3

[0027] Dissolve natural rubber with 1,2 dichloroethane (Mn=1.27×10 6 ) to form a 20%wt solution. Then take 100g of the above solution, add 0.4g of N-dimethylbenzimidazole chloride and 3.4mL of formic acid to form a uniform solution, then heat up to 40°C, and slowly add 22mL of 15% (v / v) hydrogen peroxide dropwise. Insulate at 40°C for 1h, then raise the temperature to 65°C for 6h. After the reaction, wash with deionized water for 3 times, separate the organic layer with a separatory funnel, and remove the cyclohexane under reduced pressure to obtain epoxidized natural rubber.

[0028] The double bond conversion rate of epoxidized natural rubber was 85.4%, and the extraction residual rate was 2.83%.

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Abstract

The invention discloses an epoxidation method of a gel-free double bond-contained polymer, which relates to an epoxidation method of polymers, in particular to an epoxidation method of a gel-free double bond-contained polymer, which can avoid gel generation in the epoxidation reaction, improve the solubility property of epoxidation products and solve the difficult problem in commercial process of epoxidation products of double bond-contained polymers. The invention provides an improved epoxidation method of a gel-free double bond-contained polymer, which comprises the steps: the polymer is dissolved in an organic solvent to prepare a polymer solution which is then added with quaternary ammonium salt and formic acid to prepare a solution A by stirring; the solution A is added with hydrogen peroxide, then heat-preserved for reaction for at least one hour, and then heated for reaction to obtain reaction products; and after washing, an organic layer is separated and the solvent is removed by pressure reduction, thus obtaining the epoxidised gel-free double bond-contained polymer. By adding one quaternary ammonium salt or the compound of a plurality of quaternary ammonium salts, the method avoids the gelation phenomenon in the epoxidation reaction, thus leading the epoxidation reaction to be smoothly conducted and leading the epoxidation products to have good solubility property.

Description

technical field [0001] The invention relates to a method for epoxidation of polymers, in particular to a method that can avoid the occurrence of gel in the epoxidation reaction, improve the solubility of epoxidation products, and solve the problem of industrial production of epoxidation products containing double bonds An important problem in the gel-free epoxidation of double bond-containing polymers. Background technique [0002] Polymers containing double bonds are an important class of polymers, and they are usually prepared by homopolymerization or copolymerization of conjugated dienes as monomers. Such polymers usually have good elasticity and can be used as elastomers. However, due to the poor polarity of this type of material, its oil resistance, adhesion and air permeability are poor, which limits the application field of polymers containing double bonds. In order to increase the polarity of such polymers, polar groups can be introduced by copolymerization with sp...

Claims

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Application Information

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IPC IPC(8): C08F36/04C08F8/08
Inventor 林国良吴维芬余谋发
Owner XIAMEN UNIV
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