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Solid acid catalyst for glycerinum esterification and aldolization, and preparation method therefor

A technology of solid acid catalyst and acetal reaction, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., to achieve the effects of simple preparation, simple filtration and recovery, and high catalytic activity

Active Publication Date: 2015-09-02
NANCHANG BAIYUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the above problems, the present invention adopts free radical polymerization method to prepare-SO 3 HPW functionalized quaternary ammonium salt polymer solid acid catalyst to synthesize glyceryl acetate and benzaldehyde glyceryl acetal, this method has not been reported yet

Method used

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  • Solid acid catalyst for glycerinum esterification and aldolization, and preparation method therefor
  • Solid acid catalyst for glycerinum esterification and aldolization, and preparation method therefor

Examples

Experimental program
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Effect test

Embodiment 1

[0015] -SO 3 Functionalized Triallylamine TAM-SO 3 Preparation: In a round-bottomed flask, add 0.1mol of triallylamine and 0.1mol of 1,3-propane sultone into 30mL of toluene solvent, stir at 100°C for 24h, and separate out the lower layer of yellow oil The product was washed three times with ethanol and dried under vacuum at 60 °C for 10 h to obtain TAM-SO 3 .

[0016] Polymeric solid acid catalyst Poly(TAM-SO 3 HPW) preparation: the above 0.05mol TAM-SO 3 Add to 30mL methanol solvent, add 0.1g azobisisobutyronitrile AIBN, then stir at 70°C for 24h, remove the solvent by rotary evaporation, wash the product three times with ethyl acetate, and dry it under vacuum at 60-90°C for 10h to obtain Poly (TAM-SO 3 ), 0.54g Poly(TAM-SO 3 ) and 2g phosphotungstic acid (H 3 PW 12 o 40 ) was added to 50mL of deionized water, stirred at room temperature for 12h, filtered to remove the solvent, and the solid product was vacuum-dried at 60°C for 10h to obtain a polymeric solid acid c...

Embodiment 2

[0018] In a 100mL round bottom flask, add 0.1mol glycerol, 0.6mol acetic acid and 30mL toluene, then add 0.6g of solid acid catalyst Poly(TAM-SO 3 HPW), at a reaction temperature of 120° C., reflux to separate water, and stirred for 2 hours. Through chromatographic analysis, the conversion rate of glycerin was 98%, the selectivity of diacetin was 72, and the selectivity of triacetin was 27%.

Embodiment 3

[0020] In a 100mL round bottom flask, add 0.1mol glycerin and 0.12mol benzaldehyde, then add 0.2g solid acid catalyst Poly(TAM-SO 3 HPW), at a reaction temperature of 30°C, stirred and reacted for 2 hours, through chromatographic analysis, the conversion rate of glycerol was 92%, and the acetal product selectivity of 1,3-dioxolane was 59%, and 1,3-dioxolane The acetal product selectivity of the hexacyclic ring was 38%.

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Abstract

The present invention discloses a solid acid catalyst for the glycerinum esterification and aldolization, and a preparation method therefor. Triallylamine is reacted with 1, 3-propane sultone to obtain -SO3-functionalized quaternary ammonium salt. After that, through the free-radical polymerization process, the quaternary ammonium salt is initiated by azodiisobutyronitrile to be subjected to the polymerization reaction and the obtained polymer is subjected to the protonation reaction with phosphotungstic acid to obtain a polymeric type solid acid catalyst. The preparation method for the solid acid catalyst is simple and easy to operate, high in catalytic efficiency, reusable and lower in production cost, thus providing a very competitive cleaning means.

Description

technical field [0001] The invention relates to a preparation method of a novel solid acid for glycerol esterification and acetal reaction, which uses a free radical polymerization method to prepare Poly(TAM-SO 3 The invention relates to a polymeric solid acid catalyst (HPW), which belongs to the technical field of fine organic chemical industry. Background technique [0002] The increasing scarcity of petroleum resources and the deteriorating global environment have drawn more and more attention to biodiesel. Glycerol is an inevitable non-product in the production process of biodiesel. In recent years, with the continuous rise of oil prices and traditional energy prices, the demand and production of biodiesel have grown rapidly, and the production of crude glycerol, its main by-product, has increased rapidly, showing a situation of oversupply, leading to a decline in the price of glycerol. Therefore, the utilization of glycerin as a by-product of biodiesel has become a dif...

Claims

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Application Information

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IPC IPC(8): B01J31/18C07C69/18C07C67/08C07D317/72
Inventor 冷炎卢丹蒋平平
Owner NANCHANG BAIYUN PHARMA
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