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Preparation of polystyrolsulfon acid and application

A technology for waste polystyrene and ethyl acetate, which is applied in the preparation of carboxylate, the preparation of organic compounds, organic compounds/hydrides/coordination complex catalysts, etc. Unfriendly and other problems, to achieve the effect of high sulfonation rate, high esterification rate and high product viscosity index

Inactive Publication Date: 2014-12-17
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, the use of sulfonic acid to catalyze the esterification reaction, especially the esterification of aromatic acids, tert-butanol, and polyols that are difficult to catalyze with general solid acids, has a very good effect [4-7] , but p-toluenesulfonic acid and alkylsulfonic acid are a kind of homogeneous catalysts, which cannot be recycled, and need to consume a large amount of water to wash after the esterification reaction, which belongs to environmentally unfriendly catalysts. Therefore, it is necessary to develop a A polystyrene sulfonation catalyst that can not only utilize recycled polystyrene, but also be environmentally friendly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 15 g of waste polystyrene, break it into granules, add 20 mL of ethyl acetate to dissolve, filter to remove insoluble matter, distill the obtained liquid to remove ethyl acetate under stirring, and obtain solid polystyrene. Add 40g of 98% fuming sulfuric acid and 100mL of dichloroethane to the flask, raise the temperature to 70°C and stir for 0.5 hours, continue to heat up to 85°C, react for 4 hours, cool to room temperature, add acetone, there is precipitation, filter , washed the filter cake with acetone (to remove unreacted sulfuric acid), and dried overnight at 100°C in vacuum to obtain light yellow solid polystyrene sulfonic acid, weighing 23.3g, with a yield of 90%. Dissolve a certain amount of polystyrene sulfonated product in acetone, use phenolphthalein as indicator, and titrate with 0.1mol / L NaOH standard solution, do 3 parallel experiments, take the average value, and obtain a sulfonated degree of 85% .

[0023] Esterification Catalyzed by Polystyrene ...

Embodiment 2

[0025] Esterification of pentaerythritol and oleic acid catalyzed by polystyrene sulfonic acid

[0026] Under argon protection, add 0.1 mol of pentaerythritol and 0.44 mol of oleic acid to a 250 mL flask equipped with a mechanical stirrer, add 3.5 g of the solid sulfonic acid prepared in Example 1, stir and react at 180°C for 6 hours, and cool After filtering to remove insoluble matter, after weighing the product, accurately weigh 1g of the product, dissolve it in methanol, use phenolphthalein as indicator, titrate with standard 0.05M KOH methanol solution, parallel 3 times, and calculate the esterification rate to be 92%. After washing the remaining product with water to remove pentaerythritol, excess oleic acid was removed under reduced pressure, and the measured viscosity index was 150.

Embodiment 3

[0028] Esterification of trimethylolpropane and oleic acid catalyzed by polystyrene sulfonic acid

[0029] Under argon protection, add 0.1 mol of trimethylolpropane and 0.33 mol of oleic acid to a 250 mL flask equipped with a mechanical stirrer, add 3.0 g of the solid sulfonic acid prepared in Example 1, and stir the reaction at 160°C After cooling for 6 hours, filter to remove insoluble matter, weigh the product and accurately weigh 1g of the product, dissolve it in methanol, use phenolphthalein as indicator, titrate with standard 0.05M KOH methanol solution, parallel 3 times, and calculate the esterification rate 94%. After washing the remaining product with water to remove trimethylolpropane, excess oleic acid was removed under reduced pressure, and the measured viscosity index was 135.

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Abstract

The invention relates to synthesis of polystyrolsulfon acid and its application. Recovered polystyrene is used as a raw material and is purified by ethyl acetate dissolution; and fuming sulphuric acid is used for sulfonation so as to prepare polystyrolsulfon acid which is used as a catalyst to be applied in catalyzing an esterification reaction between polyol and carboxylic acid. Research results show that, in comparison with benzenesulfonic acid, the catalyst has advantages of low production cost, high esterification rate, convenient recovery, simple product aftertreatment technology, high viscosity index of an esterification product and the like.

Description

technical field [0001] The invention relates to the preparation of polystyrene sulfonic acid and its catalytic polyol esterification application. Background technique [0002] Polystyrene is a widely used polymer material, mainly used in disposable tableware, packaging materials and other fields. It is difficult to biodegrade, so it has become a white garbage that seriously pollutes the environment. In recent years, some researchers have carried out research on the recycling and application of PS. Li Yuguang et al. [1] Using the template method, use a mixed sol of tetraethylorthosilicate and 3-mercaptopropyltrimethoxysilane to transform in situ in the interstitial space of polystyrene colloidal crystals. After removing the template, use hydrogen peroxide to oxidize the mercapto group into a sulfonic acid group. For the first time, 3DOMSiO with regularly arranged macropores was successfully prepared 2 -SO 3 Material H catalyzes the synthesis of butyl acetate with a maximu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C08F112/08C08F8/36C07C69/14C07C69/33C07C67/08C07C69/58
CPCY02P20/584
Inventor 曹丝雨马泊静李助钰黄怡然武青青王瑜曹澜缤许胜米普科俞旻彦潘辰晖
Owner EAST CHINA UNIV OF SCI & TECH
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