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Solid superacid catalyst formalic acid esterification

A technology of solid super acid and malate, applied in physical/chemical process catalyst, carboxylate preparation, organic compound preparation, etc., can solve the difficulty of separation between catalyst and reaction system, the difficulty of catalyst recycling, and the pollution of reaction tail liquid. environment and other problems, to achieve the effect of easy recycling, good recycling and good stability

Inactive Publication Date: 2019-07-12
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, concentrated sulfuric acid is used as a catalyst in the production of malic acid diester by malic esterification in industry. There are many disadvantages in using concentrated sulfuric acid as a catalyst, such as severe corrosion of equipment, difficulty in separating the catalyst from the reaction system, difficulty in recycling the catalyst, and reaction tail liquid. It is strongly acidic and seriously pollutes the environment, etc.

Method used

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  • Solid superacid catalyst formalic acid esterification
  • Solid superacid catalyst formalic acid esterification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Solid super acid catalyst SO 4 2- / ZrO 2 Preparation: Put 1g ZrO on the watch glass 2 Soaked in 0.6mL of 5mol / L sulfuric acid solution for 2h, dried in 110℃ oven for 12h, calcined in air at 400℃ for 4h to obtain SO 4 2- / ZrO 2 , Where SO 4 2- The load is 22%.

[0025] Dissolve 1g reactant malic acid in 2g methanol and add SO 4 2- / ZrO 2 100mg. Heat to reflux at 60℃ for 2h, filter out the catalyst SO 4 2- / ZrO 2 , The reaction solution was rotated at 60° C. to remove methanol, and 1.14 g of dimethyl malate product was collected, with a yield of 95%.

[0026] The recovered catalyst was dried at 110° C. and used again in the above-mentioned esterification reaction of malic acid and methanol. The above-mentioned reaction conditions remained unchanged, and 1.14 g of dimethyl malate product was obtained with a yield of 95%.

Embodiment 2

[0028] Solid super acid catalyst SO 4 2- / ZrO 2 Preparation: Put 1g ZrO on the watch glass 2 Soaked in 0.6mL 10mol / L sulfuric acid solution for 4h, dried in 110℃ oven for 12h, calcined in air at 650℃ for 4h to obtain SO 4 2- / ZrO 2 , Where SO 4 2- The load is 58%.

[0029] Dissolve 1g reactant malic acid in 6g methanol and add SO 4 2- / ZrO 2 500mg. Heat to reflux at 60℃ for 4h, filter out the catalyst SO 4 2- / ZrO 2 , The reaction solution was rotated at 60° C. to remove methanol, and 1.18 g of dimethyl malate product was collected, with a yield of 98%.

[0030] The recovered catalyst was dried at 110°C and used in the above-mentioned malic acid and methanol esterification reaction, the above-mentioned reaction conditions remained unchanged, and the number of cycles was 2, 3, 4, and 5 times to obtain dimethyl malate product They are 1.18g, 1.18g, 1.16g, and 1.16g respectively. The yields were 98%, 98%, 97%, and 97%, respectively.

Embodiment 3

[0032] Solid super acid catalyst SO 4 2- / MoO 3 Preparation: Put 1g MoO on the watch glass 3 Soaked in 0.5mL of 5mol / L sulfuric acid solution for 2h, dried in 110℃ oven for 12h, calcined in air at 400℃ for 4h to obtain SO 4 2- / MoO 3 , Where SO 4 2- The load is 23%.

[0033] Dissolve 1g of reactant malic acid in 2g of ethanol and add SO 4 2- / MoO 3 100mg. Heat to reflux at 70℃ for 2h, filter out the catalyst SO 4 2- / MoO 3 , The reaction solution was rotated at 60°C to distill out ethanol, and 1.35 g of diethyl malate product was collected, with a yield of 96%.

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Abstract

The invention relates to a solid superacid catalyst for malic acid esterification. The catalyst contains a main body SO4<2-> and an oxide carrier containing Lewis acid sites. The conversion rate of malic acid catalyzed by the catalyst reaches 100%, and yield of malic acid diester reaches 95% and above. In comparison with a traditional concentrated sulfuric acid catalyst, the solid superacid catalyst has higher catalytic activity, and is easy to separate from the reaction system to facilitate recycling of the catalyst. In addition, the catalyst has good cycling stability, will not corrode reaction equipment, is green and environmentally-friendly, and has a good reaction prospect.

Description

Technical field [0001] The invention relates to catalyst technology, in particular to a catalyst for catalyzing the esterification of malic acid. Background technique [0002] 1,2,4-Butanetriol is a chemical that has important uses in both civilian and military industries. It can be used to prepare biologically active agents, pharmaceutical slow-release agents, cigarette additives, and aircraft, rockets, missiles and other military weapons. Propellant etc. At present, the methods for producing 1,2,4-butanetriol include the direct hydrolysis of butenol, the epoxidation-hydrogenation of butenediol, and the malic acid esterification hydrogenation method (that is, the first esterification of malic acid to obtain apples). Acid diester, malic acid diester and then hydrogenated to obtain 1,2,4-butanetriol). Because malic acid can be obtained by fermenting biomass such as corn stalks, compared with other preparation methods, using malic acid as a raw material to prepare 1,2,4-butanetri...

Claims

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Application Information

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IPC IPC(8): B01J27/053C07C67/08C07C69/675
CPCC07C67/08B01J27/053C07C69/675Y02P20/584
Inventor 李学兵于培李广慈
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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