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Production method of dicarboxylic acid

A technology of dicarboxylic acid and production method, applied in the directions of carboxylate preparation, oxidative preparation of carboxylic acid, chemical instruments and methods, etc., can solve the problems of easy deactivation, difficult recovery, small specific surface, etc., and achieve high lactone The effect of conversion rate, good activity stability

Active Publication Date: 2014-08-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, heteropolyacid catalysts have disadvantages such as unstable properties, small specific surface area, easy deactivation, difficult recovery and short service life, so they have not been widely promoted at present.

Method used

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  • Production method of dicarboxylic acid
  • Production method of dicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take by weighing 4.6 grams of titanium-silicon molecular sieves (produced by Hunan Jianchang Petrochemical Company, trade name HTS, analyzed by X-ray diffraction to be the titanium-silicon molecular sieve of MFI structure, there is an adsorption isotherm and a desorption isotherm between the adsorption isotherm and the desorption isotherm of the low-temperature nitrogen adsorption of this molecular sieve) Hysteresis ring, the grains are hollow grains and the radial length of the cavity part is 15-180 nanometers; the molecular sieve sample is at 25°C, P / P 0 =0.10, the benzene adsorption capacity that records under the condition of adsorption time 1 hour is 78 mg / gram) is packed in the 100ml three-necked flask, then adds magnetic stirring bar, 22.81 gram ε-caprolactone, 3.6 gram water, 6.4 gram of methanol and 23ml of 30% hydrogen peroxide, the molar ratio of ε-caprolactone to hydrogen peroxide is 1:1. The three-necked flask is placed on a temperature-controlled magnetic ...

Embodiment 2

[0029] Take by weighing 4.88 grams of titanium-silicon molecular sieves (produced by Hunan Jianchang Petrochemical Co., Ltd., brand HTS, analyzed by X-ray diffraction to be the titanium-silicon molecular sieve of MFI structure, there exists between the adsorption isotherm and the desorption isotherm of the low-temperature nitrogen adsorption of this molecular sieve) Hysteresis ring, the grains are hollow grains and the radial length of the cavity part is 15-180 nanometers; the molecular sieve sample is at 25°C, P / P 0=0.10, the benzene adsorption capacity measured under the condition of adsorption time 1 hour is 78 mg / g) is installed in the 100ml three-necked flask, then adds magnetic stirring bar, 22.81 gram ε-caprolactone, 6.4 gram water and 23ml The concentration is 30% hydrogen peroxide, and the molar ratio of ε-caprolactone to hydrogen peroxide is 1:1. The three-necked flask is placed on a temperature-controlled magnetic stirrer, and the upper part of the three-necked flas...

Embodiment 3

[0031] Take by weighing 2.65 grams of titanium-silicon molecular sieves (produced by Hunan Jianchang Petrochemical Company, brand HTS, analyzed by X-ray diffraction to be the titanium-silicon molecular sieve of MFI structure, there is an adsorption isotherm and a desorption isotherm between the adsorption isotherm and the desorption isotherm of the low-temperature nitrogen adsorption of this molecular sieve) Hysteresis ring, the grains are hollow grains and the radial length of the cavity part is 15-180 nanometers; the molecular sieve sample is at 25°C, P / P 0 =0.10, the benzene adsorption capacity that records under the condition of adsorption time 1 hour is 78 mg / gram) is packed in the 100ml three-necked flask, then adds magnetic stirring bar, 11.41 gram epsilon-caprolactone, 9.2 gram acetone, 20 Gram acetic acid and 46ml concentration are 30% hydrogen peroxide, and the molar ratio of ε-caprolactone and hydrogen peroxide is 1: 4 this moment. The three-necked flask is placed o...

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Abstract

The invention relates to a production method of dicarboxylic acid. The production method is characterized in that reaction is carried out in the presence of a catalyst under the reaction conditions that molar ratio of lactone to solvent to hydrogen peroxide is 1: (0-80): (0.2-20), temperature is 90-200 DEG C and pressure is 0.1-3.0MPa and corresponding dicarboxylic acid is obtained by recycling, wherein the catalyst is a titanium-silicon molecular sieve and the mass ratio of the catalyst to the lactone is 1: (5-300). Compared with the prior art, the production method provided by the invention overcomes the defects of the traditional nitric acid oxidation process that the production technology is complex, equipment is corroded, a potential safety hazard exists, environmental pollution is serious and the like.

Description

technical field [0001] The invention relates to a method for preparing corresponding dicarboxylic acids by oxidizing lactones, and more specifically relates to a method for obtaining corresponding dicarboxylic acids by oxidizing lactones by using hydrogen peroxide as an oxidizing agent. Background technique [0002] Dicarboxylic acid is an important organic chemical raw material. Taking adipic acid as an example, it is a dicarboxylic acid with important industrial significance. It is mainly used to make adiponitrile, and then produce hexamethylenediamine Together to produce nylon 66 (polyamide) and engineering plastics. In addition, it is also used in the production of various ester products, as plasticizers and advanced lubricants, as raw materials for polyurethane elastomers, in the production of unsaturated polyesters, hexanediol and adipate, and in various foods And beverage acidulant, medicine, yeast purifying agent, insecticide, adhesive, raw material for synthetic le...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/31C07C51/285C07C55/14C07C55/12
CPCY02P20/584
Inventor 夏长久林民朱斌史春风龙立华舒兴田邹飞艳汝迎春
Owner CHINA PETROLEUM & CHEM CORP