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Method for preparing cyclopropanecarboxylic acid by using heteropolyacid catalyst

A technology for cyclopropanecarboxylic acid and isopropyl cyclopropanecarboxylate, which is applied in the field of preparation of cyclopropanecarboxylic acid, can solve the problems that equipment is easy to cause corrosion, is difficult to separate, and has low catalyst reuse rate, and achieves easy separation, low corrosiveness, high yield effect

Inactive Publication Date: 2019-01-29
DAFENG YUELONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Both of the above two processes generate saline waste water, which brings great pressure to the treatment of the three wastes. The cyclopropaneformic acid product produced by it will contain residual sulfuric acid, which is difficult to separate. It is easy to cause corrosion to the equipment during the reaction, and the catalyst will Reuse rate is relatively low

Method used

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  • Method for preparing cyclopropanecarboxylic acid by using heteropolyacid catalyst
  • Method for preparing cyclopropanecarboxylic acid by using heteropolyacid catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0017] 192g cyclopropanic acid isopropionic acid was put into the flask, added 54g water, and stirred evenly. Add 5g of silicotungstic acid, stir well and react at room temperature for 2h. After the reaction was completed, filter, collect the silicotungstic acid catalyst for mechanical use, and carry out atmospheric distillation of the mother liquor, and collect 118.3 g of fractions at 80-82°C in total, with a conversion rate of 91.71%. As detected by GC, the content of cyclopropanecarboxylic acid was 99.63%.

Embodiment 2

[0019] 192g of isopropyl cyclopropanate was dropped into the flask, 54g of water was added, and stirred evenly. Add 4.3g of silicotungstic acid, stir well and react at room temperature for 2h. After the reaction was completed, filter, collect the phosphotungstic acid catalyst for mechanical use, and carry out atmospheric distillation of the mother liquor, and collect 116.8 g of 80-82 ° C fractions in total, with a conversion rate of 90.54%. As detected by GC, the content of cyclopropanecarboxylic acid is 99.59%.

Embodiment 3

[0021] 192g of isopropyl cyclopropanate was dropped into the flask, 54g of water was added, and stirred evenly. Add 5g of silicotungstic acid collected in Example 1, stir well and react at room temperature for 2h. After the reaction was completed, filter, collect the silicotungstic acid catalyst and continue to use it mechanically. The mother liquor was distilled at atmospheric pressure, and a total of 117.6g of 80-82°C fractions were collected, with a conversion rate of 91.16%. As detected by GC, the content of cyclopropanecarboxylic acid was 99.61%. After applying mechanically 10 times of reaction, the conversion rate is still 90%, and the content of cyclopropanecarboxylic acid collected is more than or equal to 99%.

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Abstract

The invention provides a method for preparing cyclopropanecarboxylic acid by using a heteropolyacid catalyst. The method comprises the following steps: adding 192g of isopropyl cyclopropanecarboxylateinto a flask, adding 54g of water, uniformly carrying out stirring, adding 1-10% of the heteropolyacid catalyst, uniformly carrying out stirring, then carrying out a reaction at room temperature for2 hours, carrying out filtering after the reaction is ended, collecting the heteropolyacid catalyst for reuse, carrying out normal-pressure distillation on the obtained mother liquor, and collecting fractions at a temperature of 80-82 DEG C to obtain the cyclopropanecarboxylic acid. According to the invention, the catalyst with relatively good selectivity is selected, so that generation of a largeamount of salt-containing wastewater can be avoided, the catalyst can be reused and can be easily separated from the system, the yield is relatively high, and the novel catalyst adopted in the process has low corrosion to equipment.

Description

technical field [0001] The invention belongs to the preparation method of cyclopropanic acid, and more specifically relates to a method for preparing cyclopropanic acid by hydrolyzing isopropyl cyclopropanic acid. Background technique [0002] The prior art technique mainly contains two kinds, and a kind of isopropyl cyclopropanate is raw material, and sodium hydroxide is a catalyst, and hydrolysis generates sodium cyclopropanate and isopropanol, and then acidification obtains cyclopropanic acid; Cyclopropanecarboxylic acid isopropyl ester is used as raw material, sulfuric acid is used as catalyst, directly generates cyclopropanecarboxylic acid and isopropanol. [0003] Both of the above two processes generate saline waste water, which brings great pressure to the treatment of the three wastes. The cyclopropaneformic acid product produced by it will contain residual sulfuric acid, which is difficult to separate. It is easy to cause corrosion to the equipment during the react...

Claims

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Application Information

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IPC IPC(8): C07C51/09C07C61/04
CPCC07C51/09C07C2601/02C07C61/04
Inventor 杨采风江以桦
Owner DAFENG YUELONG CHEM
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