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Catalyst for preparing aromatic polycarboxylic acid by liquid phase oxidization

A polycarboxylic acid, liquid-phase oxidation technology, used in physical/chemical process catalysts, preparation of organic compounds, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of low bromine consumption, high bromine content, impurities low content

Active Publication Date: 2017-02-22
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 by liquid phase oxidization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 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:

[0033] 1) Mix 80g p-xylene, 400g acetic acid and 20g catalyst acetic acid solution (containing cobalt acetate, manganese acetate, zirconium acetate, 1,1,2,2-tetrabromoethane, 1,4-benzenedisulfonic acid) evenly Then add to the autoclave and seal it; wherein, based on the weight of the mixture, it contains 500ppmw Co 2+ 、250ppmw Mn 2+ , 25ppmw Zr 4+ , 1000ppmw bromine and 5ppmw 1,4-benzenedisulfonic acid.

[0034] 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.

[0035] 3) Add nitrogen, the mass space velocity is 4h -1 , and start the stirrer, the stirring rate is 400rpm, the temperature is ...

Embodiment 2

[0040] 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:

[0041] 1) Mix 80g p-xylene, 400g acetic acid and 20g catalyst acetic acid solution (containing cobalt acetate, manganese acetate, zirconium acetate, 1,1,2,2-tetrabromoethane, 1,5-naphthalene disulfonic acid) evenly Then add to the autoclave and close it; by weight of the mixture, it contains 500ppmw Co 2+ 、250ppmw Mn 2+ , 25ppmw Zr 4+ , 1000ppmw bromine and 5ppmw 1,5-naphthalene disulfonic acid.

[0042] 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.

[0043] 3) Add nitrogen, the mass space velocity is 4h -1 , and start the stirrer, the stirring rate is 400rpm, the temperature is raised t...

Embodiment 3

[0048] 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:

[0049] 1) Mix 80g p-xylene, 400g acetic acid and 20g catalyst acetic acid solution (containing cobalt acetate, manganese acetate, zirconium acetate, 1,1,2,2-tetrabromoethane, 2,6-naphthalene disulfonic acid) evenly Then add to the autoclave and close it; by weight of the mixture, it contains 500ppmw Co 2+ 、250ppmw Mn 2+ , 25ppmw Zr 4+ , 1000ppmw bromine and 5ppmw 2,6-naphthalene disulfonic acid. .

[0050] 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.

[0051] 3) Add nitrogen, the mass space velocity is 4h -1 , and start the stirrer, the stirring rate is 400rpm, the temperature is raise...

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Abstract

The invention relates to a catalyst for preparing an aromatic polycarboxylic acid by liquid phase oxidization, and mainly solves the problem of excessive use level of bromine in the catalyst for preparing the aromatic polycarboxylic acid through multi-alkyl-substituted aromatic hydrocarbon liquid phase oxidization existing in the prior art. The catalyst comprises a Co salt, a Mn salt, a Zr salt, a bromine compound and aromatic disulfonic acid, wherein the weight ratio of Co to Mn to Zr to Br to aromatic disulfonic acid is 500:(200-300):(20-100):(1000-2000):(5-20); the technical scheme solves the technical problem well and can be used for the production of preparing the aromatic polycarboxylic acid through multi-alkyl-substituted aromatic hydrocarbon liquid phase oxidization.

Description

technical field [0001] The present invention relates to a catalyst used for preparing aromatic polycarboxylic acid 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 th...

Claims

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Application Information

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IPC IPC(8): B01J31/38C07C51/265C07C63/26
Inventor 肖忠斌畅延青杨运信
Owner CHINA PETROLEUM & CHEM CORP
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