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Esterification catalyst for synthesizing ethylene/propylene glycol ether carboxylate, and preparation method thereof

A propylene glycol ether carboxylate and esterification technology, which is applied in the preparation of carboxylate, the preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problems of complex reaction process, increased production cost, environmental pollution, etc. The effect of shortening the process flow and saving equipment investment

Inactive Publication Date: 2010-06-09
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because sulfuric acid has a catalytic effect on esterification, oxidation, dehydration, etc. at the same time, a series of side reactions occur. The post-treatment of the reaction product must be neutralized by alkali and washed with water to remove sulfuric acid as a catalyst, resulting in the following disadvantages in the reaction: Reaction process Complexity, poor reaction selectivity, coloring of products, catalysts that cannot be recycled and reused, severe equipment corrosion, waste water and residues, and considerable loss of products, causing environmental pollution and increasing production costs

Method used

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  • Esterification catalyst for synthesizing ethylene/propylene glycol ether carboxylate, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Reaction material composition (mass ratio):

[0050] 60 parts of acetic acid 76 parts of ethylene glycol methyl ether

[0051] 28 parts of benzene Catalyst 4.1 parts

[0052] Wherein the preparation of catalyst is as follows:

[0053] First 4 parts of Ti(SO 4 ) 2 Dissolve in 50 parts of distilled water, add 8 parts of carrier hydrogen type ZSM-5 (SiO 2 / Al 2 o 3 =38) Crystallization, keep pH=1~5, stir the above mixture at 80°C, age for 24h, filter, wash the filter cake with deionized water, dry in vacuum at 100°C for 2 hours, and bake at 200°C for 2 hours, cooling at room temperature to obtain a metal-crosslinked solid acid catalyst, and the formed solid acid catalyst is pulverized and sieved to 100-200 mesh to form a titanium-based solid acid catalyst.

[0054] Add acetic acid, ethylene glycol methyl ether, benzene, and the catalyst into a conventional esterification reaction vessel according to the above ratio, and heat to a reaction temperature of 86-90° C. to...

Embodiment 2

[0057] Reaction material composition (mass ratio):

[0058] 36 parts of acetic acid 45 parts of ethylene glycol ether

[0059] 18 parts of benzene Catalyst 2.7 parts

[0060] Wherein the preparation of catalyst is as follows:

[0061] First, 4 parts of cerium sulfate (Ce(SO 4 ) 2 4H 2 O) was dissolved in 50 parts of distilled water, and 10 parts of carrier silica gel (mSiO 2 ·nH 2 O), keep the pH=1~5, stir the above mixture at 80°C, age for 24h, then filter, wash the filter cake with deionized water, dry in vacuum at 100°C for 1 hour, roast at 250°C for 2 hours, cool at room temperature, A metal-crosslinked solid acid catalyst is prepared, and the formed solid acid catalyst is pulverized and sieved to 200 meshes to form a cerium-based solid acid catalyst.

[0062] Add acetic acid, ethylene glycol ether, benzene, and the catalyst into a conventional esterification reaction vessel according to the above proportions, heat to a reaction temperature of 90-96° C., and distill...

Embodiment 3

[0065] Reaction material composition (mass ratio):

[0066] 36 parts of acetic acid 59 parts of ethylene glycol ether

[0067] 38 parts of benzene, 3 parts of catalyst

[0068] Wherein the preparation of catalyst is as follows:

[0069] 4 parts of cerium phosphate (CePO 4 2H 2 O) was dissolved in 50 parts of distilled water, and 10 parts of carrier silica gel (mSiO 2 ·nH 2 O), keep pH=1~5, stir the above mixture at 80°C, age for 24h, filter, wash the filter cake with deionized water, dry in vacuum at 100°C for 0.5 hour, roast at 150°C for 2 hours, cool at room temperature, A metal-crosslinked solid acid catalyst is prepared, and the formed solid acid catalyst is pulverized and sieved to 200 meshes to form a cerium-based solid acid catalyst.

[0070] Add acetic acid, ethylene glycol ethyl ether, benzene, and the catalyst into a conventional esterification reaction vessel according to the above ratio, heat to a reaction temperature of 90-95° C., and distill water to carry ...

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Abstract

The invention provides an esterification method for synthesizing ethylene / propylene glycol ether carboxylate. A catalyst used in the method consists of an active substance and a carrier, wherein the active substance is tin salt (such as tin tetrachloride), titanium salt (such as titanium sulfate, titanium tetrachloride or titanium nitrate), zirconium salt (such as zirconium sulfate, zirconium tetrachloride or zirconium nitrate) or cerium salt (such as cerous sulfate, cerium tetrachloride or cerous nitrate); the carrier is silica gel, hydrogen-type ZSM-5, activated clay or diatomite; the content of the active substance in percentage by mass is 10 to 30 percent; and the content of the carrier in percentage by mass is 70 to 90 percent. The method has the advantages of inhibiting the occurrence of side reaction during production, improving the selectivity of target products, shortening production cycle, reducing investment in production equipment and avoiding the problems of production equipment corrosion, environmental pollution, high energy consumption and the like.

Description

technical field [0001] The invention relates to a method for the esterification reaction of ethylene and propylene glycol ether carboxylates, and in particular provides a cationic solid acid catalyst for the esterification reaction of polyol ethers and a preparation method thereof. Background technique [0002] Organic carboxylic acid esters are a class of important fine organic chemical products widely used, mainly used in industries such as solvents, plasticizers, resins, coatings, fragrances, cosmetics, medicines, surfactants and organic synthesis. At present, the method for industrially producing organic carboxylic acid esters is mainly the direct esterification of carboxylic acids and alcohols. For example, the direct esterification of acetic acid and ethylene glycol methyl ether, ethylene glycol ethyl ether and ethylene glycol butyl ether at home and abroad to synthesize ethylene glycol monoalkyl alcohol ether acetate has significant economic benefits and important the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40B01J27/053B01J27/10B01J29/06C07C67/08C07C69/14C07C69/80C07C69/78
Inventor 王永杰张木张丹阳徐恒启王凤洁
Owner SHENYANG POLYTECHNIC UNIV
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