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Catalyst for preparing aromatic polycarboxylic acid

A technology of catalyst and polycarboxylic acid, which is applied in the direction of physical/chemical process catalyst, carboxylate preparation, metal/metal oxide/metal hydroxide catalyst, etc. It can solve the problems of low bromine consumption, high bromine content and low impurity content And other issues

Active Publication Date: 2017-10-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is the problem of high bromine content in catalysts existing in the prior art, and a catalyst for preparing aromatic polycarboxylic acids by liquid-phase oxidation of polyalkylated aromatic hydrocarbons is provided, and the amount of bromine used in the catalyst is low , high yield of target product and low impurity content

Method used

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  • Catalyst for preparing aromatic polycarboxylic acid
  • Catalyst for preparing aromatic polycarboxylic acid
  • Catalyst for preparing aromatic polycarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The reaction was carried out in a 1000ml titanium autoclave equipped with a magnetic stirrer, a gas delivery pipe, a reflux condenser, a thermocouple, and a bursting disc, with a stirring speed of 400rpm and heated by circulating hot oil. The reaction steps are as follows:

[0038] 1) Mix 80g p-xylene, 400g acetic acid and 20g catalyst acetic acid solution (containing cobalt acetate, manganese acetate, zirconium acetate, zinc acetate, 1,1,2,2-tetrabromoethane, 1,4-benzenedisulfonic acid Sodium) is added into autoclave after mixing evenly, and airtight; Wherein by weight of the mixture, containing 500ppmw Co 2+ 、250ppmw Mn 2+ , 25ppmw Zr 4+ , 30ppmw Zn 2+ , 1000ppmw bromine and 5ppmw 1,4-benzenedisulfonate sodium.

[0039] 2) Add 2.0MPa nitrogen to carry out the airtight test for 30 minutes, and the pressure drop within 30 minutes is not more than 0.1MPa, which is qualified.

[0040] 3) Add nitrogen, the mass space velocity is 4h -1 , and start the stirrer, the sti...

Embodiment 2

[0045] The reaction was carried out in a 1000ml titanium autoclave equipped with a magnetic stirrer, a gas delivery pipe, a reflux condenser, a thermocouple, and a bursting disc, with a stirring speed of 400rpm and heated by circulating hot oil. The reaction steps are as follows:

[0046]1) Mix 80g p-xylene, 400g acetic acid and 20g catalyst acetic acid solution (containing cobalt acetate, manganese acetate, hafnium acetate, zinc acetate, 1,1,2,2-tetrabromoethane, 1,4-benzenedisulfonic acid Sodium) is added into autoclave after mixing evenly, and airtight; Wherein by weight of the mixture, containing 500ppmw Co 2+ 、250ppmw Mn 2+ 、25ppmw Hf 4+ , 30ppmw Zn 2+ , 1000ppmw bromine and 5ppmw 1,4-benzenedisulfonate sodium.

[0047] 2) Add 2.0MPa nitrogen to carry out the airtight test for 30 minutes, and the pressure drop within 30 minutes is not more than 0.1MPa, which is qualified.

[0048] 3) Add nitrogen, the mass space velocity is 4h -1 , and start the stirrer, the stirrin...

Embodiment 3

[0053] The reaction was carried out in a 1000ml titanium autoclave equipped with a magnetic stirrer, a gas delivery pipe, a reflux condenser, a thermocouple, and a bursting disc, with a stirring speed of 400rpm and heated by circulating hot oil. The reaction steps are as follows:

[0054] 1) Mix 80g p-xylene, 400g acetic acid and 20g catalyst acetic acid solution (containing cobalt acetate, manganese acetate, zirconium acetate, cadmium acetate, 1,1,2,2-tetrabromoethane, 1,4-benzenedisulfonic acid Sodium) is added into autoclave after mixing evenly, and airtight; Wherein by weight of the mixture, containing 500ppmw Co 2+ 、250ppmw Mn 2+ , 25ppmw Zr 4+ 、30ppmw Cd 2+ , 1000ppmw bromine and 5ppmw 1,4-benzenedisulfonate sodium.

[0055] 2) Add 2.0MPa nitrogen to carry out the airtight test for 30 minutes, and the pressure drop within 30 minutes is not more than 0.1MPa, which is qualified.

[0056] 3) Add nitrogen, the mass space velocity is 4h -1 , and start the stirrer, the s...

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Abstract

The invention relates to a catalyst for preparing aromatic polycarboxiylic acid and mainly solves the problem that the using amount of bromine of a catalyst for preparing the aromatic polycarboxylic acid by substituting aromatic hydrocarbons by multiple alkyl groups through liquid-phase oxidation in the prior art is too high. By adopting the technical scheme, the catalyst for preparing the aromatic polycarboxylic acid is prepared from Co salt, Mn salt, IVB group metal salt, IIB group metal salt, a bromine-containing compound and an aromatic sulfonic acid compound, wherein the aromatic sulfonic acid compound is selected from at least one of aromatic disulfonic acid or aromatic disulfonate, the technical problem is well solved, and the catalyst can be used for production of preparing the aromatic polycarboxylic acid by substituting the aromatic hydrocarbons by the multiple alkyl groups through the liquid-phase oxidation.

Description

technical field [0001] This invention relates to catalysts for the preparation of aromatic polycarboxylic acids by liquid phase oxidation. Background technique [0002] Purified terephthalic acid, commonly known as PTA, is the basic raw material for the synthesis of polyethylene terephthalate (PET), and its demand continues to grow. It is estimated that in 2015, the global demand for PTA will reach 50 million tons. At present, the production technology of PTA is mainly a two-step process of p-xylene (PX) oxidation and hydrogenation refining developed by Amoco-MC Company. The oxidation step uses a Co-Mn-Br catalyst system with acetic acid as a solvent; hydrogenation mainly uses P-formylbenzoic acid (4-CBA) is added to p-toluic acid (p-TA), then centrifuged and washed with water. [0003] During the development of PTA production process, four main patent technologies of Amoco, Mitsui, ICI and Eastman have been formed. What these four technologies have in common is that they ...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C51/265C07C63/26
CPCC07C51/265B01J31/0225B01J23/75B01J27/138B01J27/08B01J21/066B01J23/34B01J35/19C07C63/26
Inventor 肖忠斌朱小丽孙广斌王艳红畅延青
Owner CHINA PETROLEUM & CHEM CORP
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