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Method for preparation of diester phthalate by o-xylene liquid-phase oxidation and esterification coupling

A technology of phthalic acid diester and xylene liquid, which is applied in the field of preparing phthalic acid diester by coupling liquid-phase oxidation and esterification of o-xylene, which can solve the problems of raw material consumption, energy consumption, complicated operation, and poor safety. , achieve the effect of reducing energy consumption and simple and convenient operation

Active Publication Date: 2015-03-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the main problems such as raw material consumption and high energy consumption, poor safety and complicated operation that exist in the preparation process of phthalic acid diesters at present, the purpose of the invention is to: develop a kind of o-xylene liquid-phase oxidation and esterification coupling preparation The method of phthalic acid diester, o-xylene is directly oxidized and esterified, the intermediate product is directly reacted without separation, and the product phthalic acid diester is obtained, which has the following outstanding advantages:

Method used

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  • Method for preparation of diester phthalate by o-xylene liquid-phase oxidation and esterification coupling
  • Method for preparation of diester phthalate by o-xylene liquid-phase oxidation and esterification coupling

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In the continuous reaction device, the mixture of o-xylene, dimethyl phthalate, manganese acetate, cobalt acetate, and potassium acetate is pumped into the oxidation reaction tube (the concentration of cobalt, manganese, and potassium ions in the reaction mixture are each 300ppm, The concentration of o-xylene is 30%), filled with 3MPa oxygen, oxidation occurs at 200°C, and the reaction residence time is 2h. The mixture of the oxidized mixture and methanol is pumped into the esterification reaction tube equipped with silicoaluminophosphate molecular sieve (the molar ratio of methanol to the starting o-xylene is 10:1, the mass ratio of the silicoaluminophosphate molecular sieve to the starting o-xylene 1:100), esterification occurs at 150°C, and the reaction residence time is 3h. After the esterification reaction, the mixture is pumped into the oxidation reaction tube to oxidize the second methyl group on the benzene ring, and then pumped into the esterification reaction ...

Embodiment 2～18

[0023] The specific method of Examples 2-18 is similar to that of Example 1, and the specific reaction conditions and results are listed in Table 1.

[0024] As can be seen from the above examples, using o-xylene and alcohol as raw materials, under the reaction conditions shown in Table 1, the coupling of liquid-phase oxidation and esterification is carried out, that is, the o-xylene is mainly oxidized to o-methyl Benzoic acid, after the esterification reaction, the second methyl group on the benzene ring is oxidized to a carboxyl group, and then the esterification reaction occurs, which can realize the process of converting o-xylene into dimethyl phthalate. The reaction temperature is 150-230°C. Compared with the gas-phase oxidation method, the reaction conditions are milder and the CO is greatly reduced. 2 Generation and discharge, low raw material consumption and energy consumption, good safety; intermediate products do not need to be separated and purified, the operation i...

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Abstract

The invention relates to a method for preparation of diester phthalate by o-xylene liquid-phase oxidation and esterification coupling. In the presence of a catalyst, air or oxygen is used as an oxygen source for preparation of the diester phthalate by o-xylene liquid-phase oxidation and esterification coupling. The method has the advantages of mild reaction conditions, safe operation, low raw material and energy consumption, high conversion rate and high selectivity and the like.

Description

technical field [0001] The invention relates to a method for preparing phthalic acid diester by coupling liquid-phase oxidation and esterification of o-xylene. Background technique [0002] Phthalic acid diester is an important bulk chemical, mainly used as rubber and plastic additives. Its use is the only way to improve the quality of plastics, rubber and polyester products. Its function is to weaken the intermolecular force of polymers and increase The mobility of molecular chains reduces the crystallinity of molecular chains, thereby improving the plasticity, flexibility, stretchability and processing properties of polymers. According to statistics, the global annual consumption of phthalate diesters is more than 6 million tons. [0003] At present, the preparation method of phthalic acid diester is to convert o-xylene into phthalic anhydride (phthalic anhydride) through gas-phase oxidation reaction, and then esterify the phthalic anhydride obtained by separation and pur...

Claims

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Application Information

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IPC IPC(8): C07C69/80C07C69/83C07C67/08
CPCC07C51/215C07C67/08C07C67/313C07C69/80C07C69/76C07C63/16C07C63/04
Inventor 徐杰高进黄义争苗虹马红
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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