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Preparation method of inorganic solid catalyst for synthesizing dimethyl maleate

A technology of dimethyl maleate and inorganic solids, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, and molecular sieve catalysts. It can solve the problems of resin temperature sensitivity and easy aging, and achieve less side reactions, easy separation, and good heat resistance

Inactive Publication Date: 2010-06-02
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the resin is sensitive to temperature, easy to age, and may produce degradation and pollution products, so there is still a need for improvement

Method used

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  • Preparation method of inorganic solid catalyst for synthesizing dimethyl maleate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 2g of zeolite molecular sieve raw powder in a clean crucible, activate it at 550°C for 4 hours, cool to room temperature, pour it into a round bottom flask, add 60ml of ammonium chloride solution with a concentration of 0.5mol / L, and perform ion exchange at reflux temperature 4h, then filtered, washed and dried. Calcined at 550°C for 4h to obtain the H-type catalyst.

[0015] Take 50g of maleic anhydride and 62ml of methanol, add to the autoclave, then add 0.25g of the above catalyst, seal, stir while heating up, react at 110°C for 12 hours, sample analysis, the calculated DMM yield is 93.4%.

Embodiment 2

[0017] Take 2g of zeolite molecular sieve raw powder in a clean crucible, activate it at 550°C for 4h, cool to room temperature, pour it into a round bottom flask, add 60ml of magnesium chloride solution with a concentration of 0.5mol / L, and carry out ion exchange at reflux temperature for 4h, Then filter, wash and dry. Calcined at 550°C for 4h to obtain Mg-type catalyst.

[0018] Take 50g of maleic anhydride and 62ml of methanol, put them into the autoclave, then add 0.15g of the above catalyst, seal it, stir while heating up, react at 110°C for 12 hours, sample analysis, and calculate the yield of DMM to be 93.7%.

Embodiment 3

[0020] Take 2g of zeolite molecular sieve raw powder in a clean crucible, activate at 550°C for 4h, cool to room temperature, pour it into a round bottom flask, add 60ml of ferric chloride solution with a concentration of 0.5mol / L, and perform ion exchange at reflux temperature 4h, then filtered, washed and dried. Calcined at 350°C for 4h to obtain Fe-type catalyst.

[0021] Take 50g of maleic anhydride and 62ml of methanol, put them into the autoclave, then add 0.25g of the above-mentioned catalyst, seal it, start stirring and heat up at the same time, react at 110°C for 12 hours, sample analysis, and calculate the yield of DMM to be 91.9%.

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Abstract

The invention discloses a preparation method of an inorganic solid catalyst, which is used for synthesizing dimethyl maleate and belongs to a catalyst synthesis technology. The method comprises the following steps of: firstly heating and activating a zeolite molecular sieve, then processing with an ammonium chloride solution, a ferric chloride solution or a magnesium chloride solution, and then calcining and activating to obtain the inorganic solid catalyst with selective catalytic activity. The catalyst can be used for a continuous reaction rectifying production process, is easy to separate, can be recycled, has good heat resisting property, high activity, good selectivity and less side reaction, can be used under the conditions of pressurized high temperature, is not easy to age or deteriorate and can not pollute products, and the single pass yield of the dimethyl maleate reaches more than 90 percent.

Description

technical field [0001] The invention belongs to a method for preparing a catalyst, in particular to a method for preparing an inorganic solid catalyst used for synthesizing dimethyl maleate. Background technique [0002] Dimethyl maleate is commonly known as dimethyl maleate, a colorless oily liquid with a melting point of -19°C and a boiling point of 200.4°C (101.3kPa). Dimethyl maleate is an important organic chemical raw material, which can react with various substances, such as homopolymerization or copolymerization with acrylates, vinyl chloride, vinyl acetate, styrene and other organic substances. Its copolymer can be made into a variety of coatings, adhesives, optical materials, anti-shrinkage finishing agents, etc. with special properties and uses. Dimethyl maleate reacts with dimethyl phosphite and methyl propylene to synthesize 2-phosphonobutane-1,2,4-tricarboxylic acid, a scale and corrosion inhibitor of phosphonic acid. The hydrogenation of dimethyl maleate can...

Claims

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Application Information

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IPC IPC(8): B01J29/06C07C69/60C07C67/08
Inventor 王天贵申艳敏张宏勋孙保帅余锡孟
Owner HENAN UNIVERSITY OF TECHNOLOGY
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