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Method and system for preparing glycerol alkyl ether in two steps

A technology of glycerol alkyl ether and glycerol, which is applied in the field of preparing glycerol alkyl ether by two-step method, can solve the problems of long etherification reaction time, which is unfavorable for industrialized production, and achieves improving the miscibility of materials, reducing the amount of production, and improving the yield. Effect

Active Publication Date: 2021-06-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Aiming at the problem that isobutene is easy to polymerize to form isobutene dimer in the one-step process of preparing glycerol alkyl ether from isobutene and glycerin, and the too long etherification reaction time is not conducive to industrial production, the present invention proposes a two-step method for preparing glycerol alkyl ether Methods

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  • Method and system for preparing glycerol alkyl ether in two steps
  • Method and system for preparing glycerol alkyl ether in two steps

Examples

Experimental program
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Effect test

Embodiment 1

[0048] This example illustrates that the present invention can use tert-butanol, isobutene and glycerin to prepare glycerol tert-butyl ether in a two-step process.

[0049] (1) The first step reaction: add glycerol (analytical grade, content 99.0%, Sinopharm Chemical Reagent Co., Ltd.) 10.1 g (0.11 mol), macroporous sulfonic acid catalyst KC111 agent (Hebei Kairui) in a 100 mL reactor Chemical Co., Ltd.) 0.50g and tert-butanol (chemically pure, content 98.0%, Sinopharm Chemical Reagent Co., Ltd.) 24.5g (0.33mol), n tert-butanol: n glycerol is 3:1. The reaction temperature is 70° C., the reaction pressure is 1.2 MPa, and the reaction is performed for 2 hours with electric stirring.

[0050] Gas chromatography analysis shows that the conversion rate of glycerol is 20.2%, the selectivity of monosubstituted tert-butyl glyceryl ether is 60.1%, the selectivity of disubstituted tert-butyl glyceryl ether is 39.0%, and the selectivity of trisubstituted tert-butyl glyceryl ether Sex is...

Embodiment 2

[0074] This example illustrates that the present invention can use tert-butanol, isobutene and glycerin to prepare glycerol tert-butyl ether in a two-step process.

[0075] (1) The first step reaction: add glycerol (analytically pure, content 99.0%, Sinopharm Chemical Reagent Co., Ltd.) 10.1g (0.11mol), macroporous sulfonic acid type catalyst A15 agent (Amberlyst company) in the reactor of 100mL 0.50 g and tert-butanol (chemically pure, content 98.0%, Sinopharm Chemical Reagent Co., Ltd.) 12.2 g (0.165 mol), n tert-butanol: n glycerol is 2:1. The reaction temperature is 70° C., the reaction pressure is 2 MPa, and the reaction is performed for 1 h with electric stirring.

[0076] Gas chromatography analysis shows that the conversion rate of glycerol is 18.5%, the selectivity of monosubstituted tert-butyl glyceryl ether is 69.8%, the selectivity of disubstituted tert-butyl glyceryl ether is 29.8%, and the selectivity of trisubstituted tert-butyl glyceryl ether Sex is 0.4%.

[...

Embodiment 3

[0081] This example illustrates that the present invention can use tert-butanol, isobutene and glycerin to prepare glycerol tert-butyl ether in a two-step process.

[0082] (1) The first step reaction: add glycerol (analytically pure, content 99.0%, Sinopharm Chemical Reagent Co., Ltd.) 10.1g (0.11mol), macroporous sulfonic acid type catalyst A35 agent (Amberlyst company) in the reactor of 100mL 0.50 g and tert-butanol (chemically pure, content 98.0%, Sinopharm Chemical Reagent Co., Ltd.) 24.5 g (0.33 mol), n tert-butanol: n glycerol is 3:1. The reaction temperature is 80° C., the reaction pressure is 1.5 MPa, and the reaction is carried out by electric stirring for 2 hours.

[0083] Gas chromatography analysis shows that the conversion rate of glycerol is 38.2%, the selectivity of monosubstituted tert-butyl glyceryl ether is 49.7%, the selectivity of disubstituted tert-butyl glyceryl ether is 49.2%, and the selectivity of trisubstituted tert-butyl glyceryl ether is 49.2%. se...

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Abstract

The invention provides a two-step method for preparing glycerin alkyl ether, comprising: (1) the first step reaction: under the action of an acidic resin catalyst, tert-butanol and glycerin react to prepare glycerin alkyl ether, and then distill and remove Tert-butanol and water or no treatment; (2) second step reaction: add isobutene to the system, and continue to react with the first step reaction product to prepare glycerol alkyl ether. (3) Product separation. The invention also provides a two-step reaction system for preparing glycerol alkyl ether. The method and system of the present invention have the following advantages: (1) The yield of disubstituted glycerol alkyl ether and trisubstituted glycerol alkyl ether is as high as 95%. In the present invention, a considerable amount of monosubstituted tert-butyl glyceryl ether can be obtained through the first step of reaction, thereby greatly improving the miscibility of materials in the second step of reaction, and greatly increasing the yield of polyether products. (2) The generation amount of isobutene dimer (<5%) can be greatly reduced, and the etherification reaction time can be greatly shortened, and it is easy to carry out in a fixed-bed reactor, and easy to realize industrialization.

Description

technical field [0001] The present invention relates to a method and system for preparing glycerin alkyl ether in two steps. Background technique [0002] The development of the biodiesel industry has resulted in a large global surplus of glycerin and a sharp drop in prices. How to make full and reasonable use of these cheap glycerin has become an important issue. In recent years, research hotspots have focused on the direction of using glycerol to synthesize glycerol ether as a fuel additive. The main reason is that cheap glycerin and alkylating reagents are used as raw materials for etherification reaction, that is, the by-product glycerin of biodiesel is used to reduce production costs, and the product glycerol ether can also be used as a diesel additive to improve diesel performance. In short, it will become a trend to actively carry out research on glycerol alkyl ethers, and it is in line with my country's national conditions. [0003] Glycerin tert-butyl ether is a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/06C07C43/10C07C41/09C07C43/13C07C2/28C07C11/02
CPCC07C2/28C07C41/06C07C41/09C07C2531/10C07C11/02C07C43/10C07C43/13C07C43/135
Inventor 张伟陈艳凤杜泽学刘明斌
Owner CHINA PETROLEUM & CHEM CORP