Method and system for preparation of glycerin alkyl ether

A technology of glycerin alkyl ether and glycerin, which is applied in the field of preparation of glycerin alkyl ether, can solve the problems of long reaction time, reduced catalyst life, catalyst deactivation, etc., and achieves the effects of lowering reaction temperature, controlling selectivity, and reducing residence time

Pending Publication Date: 2018-07-06
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0010] In the process of preparing glycerol tert-butyl ether from isobutene and glycerol, isobutene is prone to dimerization reaction to obtain isobutene dimer, thereby reducing the conversion rate of isobutene into glycerol alkyl ether, and leading to carbon deposition deactivation of the catalyst, reducing Catalyst life
However, the glycerol-tert-butanol system for preparing glycerol alkyl ethers has the problem that the selectivity o...

Method used

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  • Method and system for preparation of glycerin alkyl ether
  • Method and system for preparation of glycerin alkyl ether
  • Method and system for preparation of glycerin alkyl ether

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[0040] The reaction system for preparing glycerol alkyl ether provided by the present invention, the preferred embodiment includes: glycerin storage tank (1), tert-butanol storage tank (2), mixing tank (3), isobutylene storage tank (4), fixed bed reaction device (5), reaction product storage tank (6), evaporator (7), gas compression liquefaction system (8), evaporator (9), condenser (10), evaporator (11), isobutylene dimer storage Tank (12), water tank (13), water washing tower (14), phase separation tank (15), evaporator (16), evaporator (17), polyether product storage tank (18), condenser (19) , the line (20) used to transport raw glycerin from the glycerol storage tank (1) to the mixing tank (3), the line used to transport tert-butanol from the tert-butanol storage tank (2) to the mixing tank (3) (21), for the pipeline (22) that glycerol and tert-butanol mixture is transported from the mixing tank (3) to the fixed bed reactor (5), for transporting isobutylene from the isobu...

Embodiment 1

[0057] 10.0 g of macroporous sulfonic acid catalyst KC111 agent (Hebei Kairui Chemical Co., Ltd.) was filled in the fixed-bed reactor on the high-pressure micro-reactor test device. Preparation of glycerin feed: tert-butanol added to glycerol at a ratio of n-tert-butanol: n-glycerol = 1:2 to obtain a glycerol / tert-butanol solution with greatly improved fluidity.

[0058] (1) Response:

[0059]Fixed bed KC111 agent 10.0g (layer height 22cm), glycerol / tert-butanol solution feed rate 0.28ml / min (n tert-butanol: n glycerin = 1:2); liquid isobutene feed rate 0.64ml / min (n Isobutene: n glycerol = 4:1), the residence time is 1.0 h, the reactor temperature is 80° C., and the nitrogen back pressure is 2.0 MPa.

[0060] Test results: the conversion rate of glycerol is 100.00%; the selectivity of monosubstituted glycerol alkyl ether is 4.92%, the selectivity of polysubstituted glycerol alkyl ether is 95.08% (the selectivity of disubstituted glycerol alkyl ether is 77.99%, The selectivi...

Embodiment 2

[0067] 10.0 g of macroporous sulfonic acid catalyst KC111 agent (Hebei Kairui Chemical Co., Ltd.) was filled in the fixed-bed reactor on the high-pressure micro-reactor test device. Preparation of glycerin feed: Add tert-butanol to glycerin at a ratio of n-tert-butanol:n-glycerin=1:2 to obtain a glycerin / tert-butanol solution with greatly improved fluidity.

[0068] (1) Reaction: In fixed bed KC111 agent 10.0g (layer height 22cm), glycerol / tert-butanol solution feed rate 0.11ml / min (n tert-butanol: n glycerol=1:2); liquid isobutene feed rate 0.27ml / min (n isobutene: n glycerol = 4:1), the residence time is 2.5h, the reactor temperature is 70°C, and the nitrogen back pressure is 2.0MPa.

[0069] Test results: the conversion rate of glycerol is 100.00%, the selectivity of monosubstituted glycerol alkyl ether is 3.01%, the selectivity of polysubstituted glycerol alkyl ether is 96.99% (the selectivity of disubstituted glycerol alkyl ether is 72.92%, the selectivity of trisubstitut...

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Abstract

The invention provides a method for preparation of glycerin alkyl ether. The method includes: (1) adding a mixed solution of tert-butyl alcohol and glycerin and liquid isobutylene simultaneously intoa fixed bed reactor filled with an acidic resin catalyst to carry out glycerin etherification reaction on the system; (2) letting the material flowing out of the fixed bed reactor into a gas separation system to be separated into a gas phase and a liquid phase; (3) letting the liquid phase material enter a tert-butyl alcohol separation system to separate tert-butyl alcohol and (4) collecting the polyether product. The invention also provides a reaction system for preparation of glycerin alkyl ether. Under the reaction conditions of a temperature of 45-80DEG C and a glycerin residence time of 0.80-2.50h, the glycerin conversion rate can reach 100%, the polyether selectivity is up to 98.6% or more, and the selectivity of an isobutylene dimer is 1.7% or below. The method lowers the reaction temperature, greatly reduces the residence time of glycerin in the fixed bed, and well controls the selectivity of isobutylene dimer.

Description

technical field [0001] The present invention relates to a method and system for preparing glycerol alkyl ether. 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 very promisin...

Claims

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Application Information

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IPC IPC(8): C07C43/13C07C43/10C07C41/09C07C41/06C10L1/04C10L1/185
CPCC07C41/06C07C41/09C10L1/04C10L1/1852C10L2270/026C07C43/135C07C43/10
Inventor 张伟刘明斌陈艳凤杜泽学
Owner CHINA PETROLEUM & CHEM CORP
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