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Method for preparing tert-butyl glyceryl ether by using solid acid catalyst

A solid acid catalyst, a technology of tert-butyl glycerol, which is applied in the dehydration of hydroxyl-containing compounds to prepare ether, chemical instruments and methods, physical/chemical process catalysts, etc. The problems of low recovery rate and low glycerol conversion rate can achieve good catalytic effect, stable structure and improved economy.

Pending Publication Date: 2021-12-07
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Purpose of the invention: the present invention aims at the problems of low conversion rate of glycerol, low selectivity of multi-substituted tert-butyl glycerol ether and low recovery rate of reaction catalyst under high temperature and high pressure when glycerol is converted into tert-butyl glycerol ether in the prior art, and provides a A kind of method utilizing solid acid catalyst to prepare tert-butyl glycerol ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] The preparation method of the supported phosphotungstic acid solid acid catalyst is as follows: adding the carrier and phosphotungstic acid into water and stirring at room temperature; the stirred materials are left standing, dried and calcined in order to obtain the required catalyst.

[0027] The mass ratio of carrier to phosphotungstic acid is 1:0.1-0.3; for every 1g of carrier, the corresponding volume of deionized water is calculated from its water absorption.

[0028] The calcination temperature of the catalyst is 250-400° C., and the calcination time is 2-4 hours.

Embodiment 1

[0030] The preparation method of supported phosphotungstic acid solid acid catalyst of the present invention specifically comprises the following steps:

[0031] (1) Carrier pretreatment: ZrO 2 Place in a muffle furnace and bake at 400°C for 2 hours to remove impurities in the powder and improve the purity of the carrier;

[0032] (2) Get 5g of roasted ZrO 2 Add 0.500g phosphotungstic acid into 1.5mL deionized water, stir at room temperature for 1h; load phosphotungstic acid onto ZrO by stirring 2 surface;

[0033] (3) The material in step (2) was left to stand at room temperature for 8 hours to fully impregnate the active components, and then placed in an oven at 110° C. for 12 hours to completely remove the moisture;

[0034] (4) Calcining the dried solid matter in air at 250°C for 4h to obtain a catalyst with a theoretical loading of phosphotungstic acid of 10wt%, denoted as (10)HPW / ZrO 2 .

[0035] (10)HPW / ZrO that embodiment 1 makes 2 Catalyst application in glyceri...

Embodiment 2

[0039] The preparation method of supported phosphotungstic acid solid acid catalyst of the present invention specifically comprises the following steps:

[0040] (1) Carrier pretreatment: ZrO 2 Place in a muffle furnace and bake at 400°C for 2 hours to remove impurities in the powder and improve the purity of the carrier;

[0041] (2) Get 5g of roasted ZrO 2 Add 0.750g phosphotungstic acid into 1.5mL deionized water, stir at room temperature for 1h; load phosphotungstic acid onto ZrO by stirring 2 surface;

[0042](3) The material in step (2) was left to stand at room temperature for 8 hours to fully impregnate the active components, and then placed in an oven at 100°C for 12 hours to completely remove the moisture;

[0043] (4) Calcinate the dried solid matter in air at 300°C for 3 hours to obtain a catalyst with a theoretical loading of phosphotungstic acid of 15 wt%, which is denoted as (15)HPW / ZrO 2 .

[0044] (15) HPW / ZrO that embodiment 2 makes 2 Catalyst applicati...

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Abstract

The invention discloses a method for preparing tert-butyl glyceryl ether by using a solid acid catalyst, and belongs to the technical field of organic synthesis. Glycerol and tert-butyl alcohol are used as raw materials, supported phosphotungstic acid solid acid is used as a catalyst, after a reaction is performed for a period of time in a closed pressure-resistant reactor at a certain temperature, the product is subjected to conventional separation, and the tert-butyl glyceryl ether is obtained; and the conversion rate of glycerol is 76.3-93.2%, the selectivity of tri-tert-butyl glyceryl ether (TTBG) is 5.5-11.3%, and the selectivity of di-tert-butyl glyceryl ether (DTBG) is 30.1-45.7%. The supported phosphotungstic acid solid acid catalyst is prepared by taking phosphotungstic acid as an active component, impregnating a carrier and the phosphotungstic acid according to a certain mass ratio by adopting an equivalent-volume impregnation method for 9-12 hours, then drying, and roasting at the temperature of 250-400 DEG C for 2-4 hours. By screening the optimal reaction conditions and utilizing the phosphotungstic acid to modify the catalyst, the conversion rate of glycerol and the selectivity of polysubstituted tert-butyl glyceryl ether can be effectively improved when glycerol is converted to generate tert-butyl glyceryl ether, and the catalyst can be recycled for multiple times.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing tert-butyl glyceryl ether with a solid acid catalyst. Background technique [0002] With the increasing energy crisis and environmental pollution, biodiesel, as a renewable resource, has been researched and put into production by more and more countries. However, for every ton of biodiesel produced, 0.1 ton of by-product glycerol is produced, so it is necessary to convert it into value-added chemicals through proper technology. Increasing the development and utilization of glycerol, a by-product of biodiesel, will improve the comprehensive utilization and economy of the entire process. [0003] Glyceryl ethers are currently known as valuable alternative fuel additives. Disubstituted tert-butyl glyceryl ether and trisubstituted tert-butyl glyceryl ether are suitable additives mixed into diesel and biodiesel because they are non-polar ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/09C07C43/13C07C43/10B01J27/188
CPCC07C41/09B01J27/188C07C43/135C07C43/10Y02P20/584
Inventor 肖国民刘雪萍高李璟韩菲杨素张进魏瑞平
Owner SOUTHEAST UNIV
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