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Preparation method of ethylene glycol monoether

A technology of ethylene glycol monoether and aliphatic alcohol, applied in ether preparation, alkylene oxide preparation of ether, organic chemistry, etc., can solve problems such as affecting the economics of the device, the inability of the device to operate stably for a long time, and potential safety hazards.

Pending Publication Date: 2021-10-12
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] There are many advantages in the synthesis of ethylene glycol monoether by reactive distillation, but the selection of catalysts is relatively difficult and complicated
When selecting the most widely used alkali metal catalysts in industry, such as KOH, NaOH and sodium alkoxide, there are three technical bottlenecks: (1) if the raw material contains moisture, the active component of the catalyst, the alcohol oxyanion, is very easy to react with water. reaction, which will lead to a serious reduction in catalyst activity, and moisture will accumulate in the tower at the same time, requiring additional water removal facilities; (2) Since the inorganic base is not volatile, the catalyst is difficult to recover and reuse, which not only affects the economics of the device, but also It will cause environmental problems such as solid waste treatment; (3) the alkaline catalyst in the product needs to be neutralized, and the salt in the product will affect the quality of the product
[0012] When selecting the solid catalyst, that is, when adopting the heterogeneous reaction rectification process, although the limitation of the homogeneous reaction process may be overcome, there are still many problems: (1) the molding of the solid base catalyst and the placement in the tower are not necessary. Mature and effective method; (2) The deactivation problem of the catalyst will lead to the long-term stable operation of the device; (3) The vapor-liquid-solid three-phase mass transfer in the reactive distillation column is complicated, especially the surface heterogeneity of the solid catalyst The mass transfer mechanism and reaction mechanism will be difficult to determine due to internal diffusion problems
When a tubular reactor is used, the existence of non-condensable gas in the tube will lead to a severe decrease in the heat transfer rate, which will be a huge safety hazard
In addition, if too much ethylene is generated during the reaction process, the flow pattern of the fluid in the tube will be a gas-liquid two-phase flow, which will cause flow pattern disorder and cause serious back-mixing of the material in the tube
Therefore, although the use of triethylamine catalyst has its advantages, if the reactor is not properly selected, it is difficult to achieve the purpose of large-scale industrialized safe production

Method used

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  • Preparation method of ethylene glycol monoether
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  • Preparation method of ethylene glycol monoether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] With n-butanol as the low carbon aliphatic alcohol participating in the reaction, adopt figure 1The shown rectification tower is used as a reactor, and the structural parameters of the rectification tower are as follows: the catalytic rectification tower is provided with 17 theoretical plates, the feed ports of n-butanol and triethylamine are all arranged on the second plate, and the ethylene oxide The feeding port 5 is arranged on the twelfth plate.

[0076] The operating conditions of the catalytic rectification tower: the operating pressure is 0.2MPa, the feed flow rate of ethylene oxide is 2.27kmol / h, the feed molar flow ratio of n-butanol and ethylene oxide is 1.3:1, triethylamine and oxide The feed molar flow ratio of ethane is 0.04:1, the liquid holdup is 70L, and the reboil ratio is 9.

[0077] During the reaction process, the non-condensable gas is discharged through the second condenser 23, and there is no extraction at the top of the tower, and the liquid ph...

Embodiment 2

[0081] Take ethanol as the low-carbon aliphatic alcohol participating in the reaction, and adopt the rectifying tower identical with embodiment 1 to carry out reaction.

[0082] Among them, the operating conditions of the catalytic rectification tower: the operating pressure is 0.3MPa, the ethylene oxide feed flow rate is 2.27kmol / h, the feed molar flow ratio of ethanol and ethylene oxide is 1.1:1, triethylamine and cyclic The feed molar flow ratio of oxyethane is 0.04:1, the liquid holdup is 70L, and the reboil ratio is 8.

[0083] During the reaction process, the non-condensable gas is discharged through the second condenser 23, and there is no extraction at the top of the tower, and the liquid phase product extracted from the tower reactor is cooled and then analyzed by chromatography.

[0084] The molar composition of the tower still product is: ethanol 18.71%, ethylene glycol monoethyl ether 72.80%, diethylene glycol monoethyl ether 5.41%, triethylene glycol monoethyl eth...

Embodiment 3

[0087] Take methanol as the low-carbon aliphatic alcohol participating in the reaction, and adopt the same rectifying tower as in Example 1 to carry out the reaction.

[0088] Among them, the operating conditions of the catalytic rectification tower: the operating pressure is 0.4MPa, the ethylene oxide feed flow rate is 2.27kmol / h, the feed molar flow ratio of n-butanol and ethylene oxide is 1.1:1, triethylamine and The feed molar flow ratio of ethylene oxide is 0.03:1, the liquid holdup is 50L, and the reboil ratio is 10.

[0089] During the reaction process, the non-condensable gas is discharged through the second condenser 23, and there is no extraction at the top of the tower, and the liquid phase product extracted from the tower reactor is cooled and then analyzed by chromatography.

[0090] The molar composition of the bottom product is: methanol 18.78%, ethylene glycol monomethyl ether 72.51%, diethylene glycol monomethyl ether 6.20%, triethylene glycol monomethyl ether...

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Abstract

The invention provides a preparation method of ethylene glycol monoether, which comprises the following step: by taking ethylene oxide and low-carbon fatty alcohol as raw materials and triethylamine as a catalyst, reacting in a rectifying tower to prepare the ethylene glycol monoether. The preparation method of ethylene glycol monobutyl ether disclosed by one embodiment of the invention has the advantages of being simple, easy to implement, green, environmentally friendly and capable of realizing large-scale production.

Description

technical field [0001] The invention relates to ethylene glycol monoether, in particular to a preparation method of ethylene glycol monoether. Background technique [0002] Ethylene glycol monoether is an important derivative of ethylene oxide. It is an environmentally friendly solvent with excellent performance and is widely used in industrial fields such as ink, paint, leather and brake fluid. Industrially, glycol ether products are mainly synthesized by ethoxylation reaction using ethylene oxide and low-carbon alcohol as raw materials under the action of a catalyst. Taking the reaction of alcohol (expressed in ROH) and ethylene oxide (EO) as an example, the ethoxylation reaction can be expressed as: [0003] ROH+EO→RO(EO) 1 h [0004] RO(EO) 1 H+EO→RO(EO) 2 h [0005] RO(EO) 2 H+EO→RO(EO) 3 h [0006] ······ [0007] ROH+nEO→RO(EO) n h [0008] The above ethoxylation reaction will generate a series of ethoxylated homologues with different addition numbers of e...

Claims

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Application Information

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IPC IPC(8): C07C41/03C07C43/13B01D3/14
CPCC07C41/03B01D3/14C07C43/13
Inventor 林子昕安维中侯瞬别海燕
Owner OCEAN UNIV OF CHINA