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Method and catalyst for preparing adipic acid

A technology of adipic acid and catalyst, applied in the field of preparation of adipic acid, can solve the problems of toxic gas, low catalyst activity, slow reaction rate, etc., and achieve the effects of reducing pollution, high catalyst activity, and high yield

Active Publication Date: 2013-04-17
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above patents provide new ideas for the utilization of 6-hydroxycaproic acid and the preparation of adipic acid, but there are still problems such as low yield of adipic acid, release of nitrogen oxide poisonous gas during the preparation process, low catalyst activity and slow reaction rate, etc. question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]In a 250ml three-neck flask equipped with magnetic stirring and condensing reflux tube, put 10g of 6-hydroxyhexanoic acid, 30%H 2 o 2 20ml, and add catalyst phosphomolybdic acid 0.2g, stir and mix thoroughly, heat up to 70°C, and stir for 4 hours. After the reaction was completed, it was filtered and condensed to 0° C., and kept for 12 hours, at which time a large amount of crystals were precipitated. After filtration, the product was vacuum-dried at 90° C. for 2 hours to obtain 1.22 g of a white adipic acid product with a purity of 98% and a yield of adipic acid of 11.1%.

Embodiment 2

[0032] In a 250ml three-neck flask equipped with magnetic stirring and condensing reflux tube, put 10g of 6-hydroxyhexanoic acid, 30%H 2 o 2 20ml, and add 0.2g of catalyst phosphotungstic acid, stir and mix thoroughly, heat up to 70°C, and stir for 4 hours. After the reaction was completed, it was filtered and condensed to 0° C., and kept for 12 hours, at which time a large amount of crystals were precipitated. After filtration, the product was vacuum-dried at 90° C. for 2 hours to obtain 3.4 g of a white adipic acid product with a purity of 98% and a yield of adipic acid of 30.9%.

Embodiment 3

[0034] In a 250ml three-neck flask equipped with magnetic stirring and condensing reflux tube, put 10gε-caprolactone, 30%H 2 o 2 20ml, and add 0.2g of catalyst phosphotungstic acid, stir and mix thoroughly, heat up to 70°C, and stir for 4 hours. After the reaction was completed, it was filtered and condensed to 0° C., and kept for 12 hours, at which time a large amount of crystals were precipitated. After filtration, the product was vacuum-dried at 90°C for 2 hours to obtain a white adipic acid product 3.7 with a purity of 98% and a yield of adipic acid of 28.9%.

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PUM

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Abstract

The invention discloses a method and catalyst for preparing adipic acid. With metal oxyacid of tungsten or molybdenum or salt thereof as a catalyst and aqueous hydrogen peroxide solution with the mass fraction of 30-50% as an oxidizer, catalytic oxidation is carried out on 6-hydroxyl adipic acid or epsilon-caprolactone or mixture of the 6-hydroxyl adipic acid and the epsilon-caprolactone to synthesize the adipic acid under the conditions that a reaction temperature is 50-150 DEG C, reaction time is 1-15 times, molar ratio of raw material to hydrogen peroxide is 1: (1-10) and mass ratio of the raw material to the catalyst is (20-200): 1. The adipic acid is prepared from the 6-hydroxyl adipic acid or the epsilon-caprolactone as the raw material, no organic solvent is used in a preparation process, and no nitric acid is used, so that environmental pollution is reduced; and the oxidant is hydrogen peroxide, the catalyst is polyoxometallate, and no toxic gas is discharged in a reaction process, yield of the apidic acid is high and activity of the catalyst is high.

Description

technical field [0001] The invention belongs to the technical field of adipic acid preparation, and in particular relates to a method for preparing adipic acid and a catalyst thereof. Background technique [0002] Adipic acid is an important chemical intermediate for the preparation of nylon 66 and polyurethane. At present, the total production capacity of adipic acid in my country is close to 1 million tons per year. The industrial preparation method of adipic acid includes two steps. First, the mixture of cyclohexanol and cyclohexanone is prepared by catalytic oxidation of cyclohexane with air or oxygen, that is, KA oil; Preparation of adipic acid by oxidation of KA oil under catalytic action. In the nitric acid oxidizing KA oil stage, a large amount of nitrogen oxides will inevitably be produced, which will cause serious pollution to the ecological environment, and concentrated nitric acid will also cause serious corrosion to equipment, so there are many methods for prep...

Claims

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Application Information

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IPC IPC(8): C07C55/14C07C51/285B01J31/18B01J23/30B01J27/24
Inventor 杨克俭马国栋史文涛钱震张蒙左宜赞张媛张舜光袁海朋王志文王元平王绍伟王海国孙承宇宋辉石华刘文刘俊生梁莹
Owner CHINA TIANCHEN ENG
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