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Preparation method of butynedioic acid

A butynedic acid and reaction kettle technology, which is applied in the field of butynedic acid carboxylation reaction between calcium carbide and carbon dioxide, can solve environmental problems such as unfriendly

Active Publication Date: 2020-07-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The reaction has undergone repeated alkalization and acidification, using a large amount of alkali and acid, and the process is not environmentally friendly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Anhydrous treatment of solvents: the acetonitrile dehydration process uses anhydrous Na 2 SO 4 dried overnight, then in P 2 o 5 In the presence of reflux at 40°C for 2h, the solvent was distilled off. Transfer the processed solvent to the glove box for later use.

[0037] Anhydrous treatment of additives: Sodium carbonate and sodium phosphate were roasted at 300°C for 8 hours under a nitrogen atmosphere.

Embodiment 2

[0039] Mix 160 mL (3 mol) of acetonitrile with 32 g (0.5 mol) of calcium carbide and 53 g (0.5 mol) of sodium carbonate in the glove box, then add 6.4 g of triphenylphosphine and 4.2 g of silver nitrate (1:1, 34%) Add to the mixture, stir well, and seal the mixture.

[0040] Anhydrous and oxygen-free treatment is performed on the closed reactor, and the reactor is vacuumed and filled with nitrogen three times. Finally, the reactor was evacuated to a negative pressure state with a vacuum pump.

[0041] Using the negative pressure in the kettle, the mixture of calcium carbide, solvent, catalyst and auxiliary agent is moved into the reaction kettle through the feeding pipe, and carbon dioxide is filled in the reaction kettle. Heat and pressurize the reaction. Reaction temperature is 60 ℃, and reaction pressure is 2MPa. The reaction time is 24 hours. After the reaction, the mixture was filtered to separate the liquid, and 16 mL of KOH solution with a concentration of 1 mol / L w...

Embodiment 3

[0043] Mix 160 mL (3 mol) of acetonitrile and 32 g (0.5 mol) of calcium carbide and 53 g (0.5 mol) of sodium carbonate in the glove box, then add 3.9 g of triphenylphosphine and 2.6 g of silver nitrate (1:1, 20%) Add to the mixture, stir well, and seal the mixture.

[0044] Anhydrous and oxygen-free treatment is carried out on the closed reactor, and the reactor is vacuumized three times and filled with nitrogen. Finally, the reactor was evacuated to a negative pressure state with a vacuum pump.

[0045]Use the negative pressure in the kettle to move the mixture of calcium carbide, solvent, catalyst and auxiliary agent into the reaction kettle through the feed pipe, and fill the reaction kettle with carbon dioxide. Heat and pressurize the reaction. Reaction temperature is 60 ℃, and reaction pressure is 2MPa. The reaction time is 24 hours. After the reaction, the mixture was filtered to separate the liquid, and 16 mL of KOH solution with a concentration of 0.6 mol / L was add...

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PUM

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Abstract

The invention discloses a preparation method of butynedioic acid. The method comprises the following steps of: (1) firstly, carrying out water-free and oxygen-free treatment on a closed reaction kettle; (2) putting calcium carbide, a solvent, a catalyst and an auxiliary agent into the reaction kettle, introducing carbon dioxide into the reaction kettle, and heating and pressurizing for reaction; (3) separating the reacted mixture obtained in the step (2) to obtain a liquid mixture, and adding a KOH solution into the liquid mixture; stirring to separate out a white precipitate; and dissolving the white precipitate in hot water, acidifying with concentrated sulfuric acid, cooling, separating out the white precipitate, and filtering to obtain the product. The synthesis method disclosed by theinvention is relatively environment-friendly and low in production cost.

Description

technical field [0001] The invention relates to a synthesis method of butyne dioic acid, in particular to a method for preparing butyne dioic acid through the carboxylation reaction of calcium carbide and carbon dioxide. Background technique [0002] Butynedioic acid generally exists in the form of dihydrate, which is a colorless crystal. It is an important chemical intermediate, which can produce butynediol, butenediic acid and butanediol, butynediic acid. It is also an important pharmaceutical intermediate for the production of the antidote sodium dimercaptosuccinate. With the deepening of its research and the development of new uses, the demand for butynediic acid is increasing day by day. [0003] The industrial synthesis method of butynedioic acid is maleic acid bromination method. Maleic acid is used as raw material to react with bromine water to produce dibromosuccinic acid. Dibromosuccinic acid removes HBr in alkaline solution to obtain butynedioic acid sodium, an...

Claims

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Application Information

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IPC IPC(8): C07C51/15C07C51/02C07C57/18
CPCC07C51/15C07C51/02C07C57/18
Inventor 张志智王陶孙潇磊尹泽群刘全杰方向晨
Owner CHINA PETROLEUM & CHEM CORP
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