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Catalyst for preparing 1,4-butanediol or tetrahydrofuran from selective hydrogenation of dimethyl maleate and preparation method thereof

A technology of dimethyl maleate and selective hydrogenation, which is applied in the chemical industry, can solve the problem of a small adjustment range of the composition of the hydrogenation product, and achieves good industrial application prospects and the effect of enhancing elasticity.

Active Publication Date: 2009-08-12
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these catalysts have high selectivity, the adjustment range of the hydrogenation product composition is not large enough to cope with the price fluctuations of 1,4-butanediol or tetrahydrofuran products caused by changes in market demand

Method used

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  • Catalyst for preparing 1,4-butanediol or tetrahydrofuran from selective hydrogenation of dimethyl maleate and preparation method thereof
  • Catalyst for preparing 1,4-butanediol or tetrahydrofuran from selective hydrogenation of dimethyl maleate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 10.0g Cu(NO 3 ) 2 ·3H 2 O, 9.8g Zn(NO 3 ) 2 ·6H 2 O dissolved in 75ml H 2 O is made into a metal ion solution, 8.7gNa 2 CO 3 Dissolved in 82ml H 2 O to obtain a precipitant solution. In a water bath at 60°C, add the metal ion solution and the precipitant solution dropwise under stirring for co-precipitation. After the dropwise addition was completed, the mixture was aged for 1 hour. Wash the precipitate to remove impurity ions, then add 1.68g Al(OH) 3 . The mixture thus obtained was added with 150ml of deionized water, heated to 60°C and stirred for 30min. The filter cake obtained by suction filtration was dried at 120° C. overnight, and the temperature was raised to 450° C. in a muffle furnace at 10 K / min and calcined for 4 hours to obtain catalyst A.

Embodiment 2

[0022] 10.0g Cu(NO 3 ) 2 ·3H 2 O, 9.8g Zn(NO 3 ) 2 ·6H 2 O and 0.15g Mn(NO 3 ) 2 Dissolve in 75ml H 2 O is made into metal ion solution, 8.7g Na 2 CO 3 Dissolved in 82ml H 2 O to obtain a precipitant solution. In a water bath at 60°C, add the metal ion solution and the precipitant solution dropwise under stirring for co-precipitation. After the dropwise addition was completed, the mixture was aged for 1 hour. Wash the precipitate to remove impurity ions, then add 1.68g Al(OH) 3 . The mixture thus obtained was added with 150ml of deionized water, heated to 60°C and stirred for 30min. The filter cake obtained by suction filtration was dried at 120° C. overnight, and the temperature was raised to 450° C. in a muffle furnace at 10 K / min for 4 hours to obtain catalyst B with a Mn content of 1%. Change the added Mn(NO 3 ) 2 Using the same conditions to prepare catalysts C and D with Mn contents of 2% and 5%, respectively.

Embodiment 3

[0024] 10.0g Cu(NO 3 ) 2 ·3H 2 O, 9.8g Zn(NO 3 ) 2 ·6H 2 O and 0.21g Mg(NO 3 ) 2 ·6H 2 O dissolved in 75ml H 2 O is made into metal ion solution, 8.7g Na 2 CO 3 Dissolved in 82ml H 2 O to obtain a precipitant solution. In a water bath at 60°C, the metal ion solution and the precipitant are added dropwise under stirring for co-precipitation. After the dropwise addition was completed, the mixture was aged for 1 hour. Wash the precipitate to remove impurity ions, then add 1.68g Al(OH) 3 . The mixture thus obtained was added with 150ml of deionized water, heated to 60°C and stirred for 30min. The filter cake obtained by suction filtration was dried overnight at 120° C., and the temperature was raised to 450° C. in a muffle furnace at 10 K / min for 4 hours to obtain catalyst E with a Mg content of 1%. Change the added Mg(NO3 ) 2 Using the same conditions to prepare catalysts F and G with Mg contents of 2% and 5%, respectively.

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Abstract

The invention belongs to the field of chemical technology, and in particular relates to a catalyst for preparing 1, 4-butanediol or tetrahydrofuran by selective hydrogenation of dimethyl maleate and a preparation method thereof. The catalyst consists of Cu, Zn, Al, M and O, and the mol content of each metal element is as follows: 30 to 60 percent of Cu, 10 to 50 percent of Zn, 5 to 20 percent of Al and 0 to 10 percent of M, wherein M is any one of Mn, Mg and Cr. The preparation method for the catalyst comprises precipitation, ageing, washing, drying and baking of a catalyst precursor, and reduction activation before use. The catalyst is applied to the hydrogenation reaction of the dimethyl maleate, and the yield of the 1, 4-butanediol at a reaction temperature of 180 DEG C is 73.6 percent; and the yield of the tetrahydrofuran is 96 percent at a reaction temperature of 220 DEG C. Product composition of the catalyst can be well adjusted by changing the reaction condition to adapt to different market demands, and the catalyst has extremely high industrial application value.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a catalyst for selective hydrogenation of dimethyl maleate to prepare 1,4-butanediol or tetrahydrofuran and a preparation method thereof. Background technique [0002] 1,4-Butanediol is an important basic organic synthetic raw material that has developed rapidly in recent years. Due to the longer carbon chain, the polyester or polyurethane synthesized from it has more balanced physical properties than the polymer synthesized from ethylene glycol or propylene glycol. 1,4-Butanediol is widely used, and it mainly has 3 product chains: 1. Production of tetrahydrofuran (referred to as THF), tetrahydrofuran undergoes ring-opening polymerization to produce polytetramethylene ether glycol (abbreviated as PTMEG), pharmaceutical intermediate 2. Production of γ-butyrolactone (abbreviated as GBL), and γ-butyrolactone is further reacted with acetylene to generate 2-pyrr...

Claims

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Application Information

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IPC IPC(8): B01J23/80B01J23/889B01J23/86B01J37/03C07C31/20C07C29/149C07D307/08
Inventor 范康年郭平均乔明华赵正康谢振华杨菊群刘文艳
Owner FUDAN UNIV
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