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Preparation method of ethylene glycol mono-tert-butyl ether

A technology of mono-tert-butyl ether and methyl-tert-butyl ether, which is applied in the field of preparation of ethylene glycol mono-tert-butyl ether, can solve problems such as high pressure requirements, harsh equipment material requirements, and high energy consumption for separation, achieving The effect of low reaction pressure, low production cost and simple process flow

Active Publication Date: 2020-02-07
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, the prior art has the following deficiencies: (1) isobutylene is used as a reactant, which easily produces dimerization, etc., (2) due to the presence of inorganic acid as a catalyst, the reaction product generates water, which increases the problem of treating waste acid water , 3) The reaction has high pressure requirements, and the corresponding requirements for the material of the equipment are harsh, the reactants are not completely reacted, and the separation energy consumption is relatively large

Method used

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  • Preparation method of ethylene glycol mono-tert-butyl ether

Examples

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Comparison scheme
Effect test

Embodiment 1

[0040] Mix 200.0g of boehmite, 80g of magnesium stearate, 80g of ammonium borate, and 5g of zirconium hydroxide evenly, add 50g of silicon carbide, 160g of silicon oxide, and 9g of fruit shell activated carbon powder, mix evenly, put them into a ball mill for 1 hour, and then Add 10g Tianqing powder and 8g sucrose and mix evenly to form mixture A, dissolve 60.0g ammonium phosphotungstate in 20ml deionized water, add to the above mixture A, knead for 40 minutes, extrude into strips, dry naturally, at 650℃ Calcined for 4h to obtain the finished catalyst a.

[0041] see figure 1 The process flow shown, fixed bed reactor pressure 0.15MPa, reaction temperature 55°C, ethylene glycol to MTBE (molar ratio) 1.05, space velocity 1.50h -1, under the action of catalyst a, the exchange reaction of alcohol ether occurs, and the reaction product enters the separation and rectification tower equipped with catalyst a (tower pressure 0.12MPa, reflux ratio is 1, tower kettle 188~192°C, tower to...

Embodiment 2

[0043] Mix 260.0g of aluminum glue, 60g of light magnesia, 70g of boric acid, and 4g of zirconium hydroxide, add 70g of silicon carbide, 200g of silicon oxide, and 12g of coconut shell activated carbon powder, mix evenly, put them into a ball mill for 1.5 hours, and then add 15g each Mix citric acid and 8g starch evenly to form mixture A, dissolve 90.0g ammonium phosphotungstate in 30ml deionized water, add to the above mixture A, knead for 70 minutes, extrude into strips, dry naturally, and bake at 700°C for 3h, That is, the finished catalyst product b is obtained.

[0044] see figure 1 The process flow shown, fixed bed reactor pressure 0.10MPa, reaction temperature 55°C, ethylene glycol to MTBE (molar ratio) 1.05, space velocity 2.50h -1 , under the action of catalyst b, the exchange reaction of alcohol ether occurs, and the reaction product enters the separation and rectification tower equipped with catalyst b (tower pressure 0.08MPa, reflux ratio is 1, tower still 187~191...

Embodiment 3

[0046] see figure 1 The process flow shown, fixed bed reactor pressure 0.45MPa, reaction temperature 65°C, ethylene glycol to MTBE (molar ratio) 1.1, space velocity 2.00h -1 , under the action of No. b catalyst, the alcohol-ether exchange reaction occurs, and the reaction product enters the separation and rectification tower equipped with No. ~65°C), the upper part of the reaction section, the lower part of the reaction section supplemented with MTBE, the reaction product and MTBE were further reacted and separated in the separation and rectification tower, methanol was obtained from the top of the tower, and ethylene glycol mono-tert-butyl ether and ethylene glycol were obtained from the bottom of the tower The mixture of alcohol di-tert-butyl ether, the product in the distillation column is separated into the azeotropic distillation column (tower pressure 0.08MPa, reflux ratio is 4, column reactor 185-190°C, tower top temperature 98.5-99°C), In the azeotropic tower, ethylen...

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Abstract

The invention relates to a preparation method of ethylene glycol mono-tert-butyl ether, and belongs to the technical field of organic chemical engineering. The preparation method of the ethylene glycol mono-tert-butyl ether provided by the invention uses ethylene glycol and methyl tert-butyl ether as raw materials, uses a solid acid catalyst, and uses a fixed bed reaction and a reactive distillation process to prepare the ethylene glycol mono-tert-butyl ether. The method has low reaction pressure, a simple process flow and low production costs, and belongs to environment-friendly processes.

Description

technical field [0001] The invention relates to a preparation method of ethylene glycol mono-tert-butyl ether, which belongs to the technical field of organic chemical industry. Background technique [0002] Ethylene glycol mono-tert-butyl ether has many advantages such as high flash point, non-flammability, and low toxicity. , is widely used in water-based surface coatings, jet fuel anti-icing agents, brake fluids, inks, dyes, medicines, spices and cleaning agents and other industries, and can also be used as the base fluid for synthetic brake fluids in the automotive industry. Due to its good environmental performance, it can also be used as a substitute for ethylene glycol n-butyl ether in some application fields. [0003] Ethylene glycol mono-tert-butyl ether has a variety of preparation methods, the most common is the preparation route of isobutylene and ethylene glycol reaction. This technical route is prone to dimerization reaction of isobutylene, with many by-produ...

Claims

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Application Information

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IPC IPC(8): C07C43/13C07C41/14C07C41/42B01J27/228
CPCC07C41/14C07C41/42B01J27/228B01J2523/00C07C43/13B01J2523/22B01J2523/305B01J2523/31B01J2523/41B01J2523/48Y02P20/10
Inventor 朱相春菅秀君贾庆龙马瑞杰解红梅
Owner CHINA PETROLEUM & CHEM CORP
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