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Method for preparing diol mono-tert-butyl ether

A mono-tert-butyl ether and diol technology, which is applied in the field of diol mono-tert-butyl ether preparation, can solve the problems of reduced reactor efficiency, complicated operation, and high equipment investment, and achieve equipment investment and energy consumption reduction, The effect of the simplification of the separation process

Active Publication Date: 2017-02-15
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The above method requires that the content of water must be greater than 90mol% in the reflux of the azeotropic distillation tower, and then all the water is evaporated, and the condensed water is refluxed again. This evaporation and cooling process consumes a large amount of steam and consumes a lot of energy. high
In addition, in order to suppress the generation of ethylene glycol di-tert-butyl ether, 51% of the reactor outlet product needs to be returned to the reactor inlet, so that the efficiency of the reactor is greatly reduced
According to the introduction of the patent JP1981-103127, the above separation system includes 5 towers and 1 oil-water separator, the investment is high and the operation is complicated
[0007] In a word, the generation of excessive ethylene glycol di-tert-butyl ether by-products is the key factor leading to high separation difficulty, high energy consumption and high equipment investment. Reducing the generation of ethylene glycol di-tert-butyl ether by-products in the reaction stage is the solution The key to this problem, the existing technology has not yet provided an effective solution

Method used

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  • Method for preparing diol mono-tert-butyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of ethylene glycol mono-tert-butyl ether.

[0028] The reactor is a reactive distillation tower, including a rectification section and a reaction section, the material is 316L, the inner diameter is 65mm, the height of the catalyst bed in the reaction section is 1m, and the height of the rectification section is 1m. The reaction section is filled with acidic resin (Amberlyst-70, Dow Chemical) soaked and replaced with ethylene glycol in advance. The lower part of the bed is supported by a sieve plate and the glass fiber cloth laid on it, and the upper part of the bed is supported by glass fiber cloth and its The upper sieve plate is fixed, and the stainless steel corrugated wire mesh structured packing is used in the middle of the bed, and the resin is dispersed and filled in the gaps of the corrugated wire mesh structured packing. The porosity of the structured packing is 95%, and the specific surface area is 700m 2 / m 3 , the interlayer spacing is 5mm, th...

Embodiment 2

[0032] Preparation of propylene glycol mono-tert-butyl ether.

[0033] The reactor was the same as in Example 1.

[0034] The reactor is operated under normal pressure, 1,2-propanediol is preheated to 170°C through the preheater from the fresh glycol pipeline 1 and fed to the top of the reaction section, and isobutene is fed into the reaction in gaseous form from the fresh isobutene pipeline 2 At the bottom of the section, liquid 1,2-propanediol and gaseous isobutene flow countercurrently in the catalyst bed, and the bed temperature is maintained at 170°C. The unreacted 1,2-propanediol (boiling point 188°C) enters the tower tank, and circulates back to the front end of the preheater through the circulation pump and the glycol circulation line 6 . The 1,2-propanediol mono-tert-butyl ether (boiling point 143° C.) and unreacted isobutylene generated by the reaction escape from the reaction section, and after being purified by the rectification section, the top extraction pipelin...

Embodiment 3

[0037] Preparation of ethylene glycol mono-tert-butyl ether.

[0038] The reactor is a reactive distillation tower, including a rectification section and a reaction section, the material is 316L, the inner diameter is 65mm, the height of the catalyst bed in the reaction section is 1m, and the height of the rectification section is 1.5m. The reaction section is filled with acidic resin (Amberlyst-70, Dow) soaked and replaced with ethylene glycol in advance. The lower part of the bed is supported by a sieve plate and the glass fiber cloth laid on it, and the upper part of the bed is supported by glass fiber cloth and its upper part. The sieve plate is fixed, and the stainless steel corrugated wire mesh structured packing is used in the middle of the bed, and the resin is dispersed and filled in the gaps of the corrugated wire mesh structured packing. The porosity of the structured packing is 80%, and the specific surface area is 400m 2 / m 3 , the interlayer spacing is 8mm, the...

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Abstract

The present invention relates to a method for preparing diol mono-tert-butyl ether. According to the method, isobutene gas and liquid-phase diol are introduced into the catalyst bed layer in the middle portion of a reactor, the generated diol mono-tert-butyl ether is instantly distilled from the bed layer under the gas stripping effect of the isobutene gas so as to avoid the generation of ethylene glycol di-tert-butyl ether due to the continuous reaction between the diol mono-tert-butyl ether and the isobutene, the diol mono-tert-butyl ether is separated on the upper portion of the reactor, the separated diol mono-tert-butyl ether is condensed on the tower top, the condensed diol mono-tert-butyl ether is extracted from the tower top or the side line, and the unreacted isobutylene and the unreacted diol are respectively extracted from the tower top and the tower bottom and then are recycled to the inlet. With the process of the present invention, the generation of the diol di-tert-butyl ether can be inhibited, such that the problems that the azeotropy of the diol di-tert-butyl ether and the diol mono-tert-butyl ether causes high separation energy consumption, high investment, and the like can be avoided.

Description

technical field [0001] The invention relates to a method for preparing diol mono-tert-butyl ether. Background technique [0002] Glycol tert-butyl ether is an isomer of glycol n-butyl ether. Because of its tert-butyl structure, it has lower photochemical properties, lower toxicity and More excellent hydrophilicity, it is an important chemical product in glycol ethers, it can be used as an excellent solvent for coatings, inks, etc., and it can also be used in detergents. The common ethylene glycol n-butyl ether is usually synthesized by the ring-opening reaction of butanol and ethylene oxide, but ethylene glycol tert-butyl ether cannot be prepared by the reaction of tert-butanol and ethylene oxide, because tert-butanol It is difficult to react with ethylene oxide, and the selectivity of ethylene glycol monoether is particularly low, mainly producing higher molecular weight ethylene oxide oligomers. Therefore, ethylene glycol tert-butyl ether uses a technique similar to the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/06C07C41/42C07C43/13C07C43/11
CPCC07C41/06C07C41/42C07C43/13C07C43/11
Inventor 袁帅何岩黎源王中华黄少峰吕艳红吴华杰宋伟锋董龙跃姜庆梅
Owner WANHUA CHEM GRP CO LTD
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