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Catalyst for preparing aromatic polycarboxylic acid through liquid-phase oxidation

A polycarboxylic acid, liquid-phase oxidation technology, applied 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: 2017-12-08
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 through liquid-phase oxidation

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Experimental program
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Effect test

Embodiment 1

[0033] 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:

[0034] 1) Weigh 80g p-xylene, 400g acetic acid, 20g metal acetate (based on the whole solution, which contains 500ppmwCo 2+ 、250ppmw Mn 2+ 、25ppmw Ce 4+ ) and 0.55g 1,1,2,2-tetrabromoethane (based on the entire solution, bromine is 1000ppmw) and 5ppmw (based on the entire solution) anthraquinone-1-sodium sulfonate, mixed uniformly and added to the autoclave, Airtight.

[0035] 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.

[0036] 3) Add nitrogen, the space velocity is 4h -1 , and start the stirrer, the stirring rate is 400rpm, the temperature is raised to 186° C., and the pressure is ma...

Embodiment 2

[0041] 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:

[0042] 1) Weigh 80g p-xylene, 400g acetic acid, 20g metal acetate (based on the whole solution, which contains 500ppmwCo 2+ 、250ppmw Mn 2+ 、25ppmw Ce 4+ ) and 0.55g of 1,1,2,2-tetrabromoethane (based on the entire solution, bromine is 1000ppmw) and 5ppmw (based on the entire solution) anthraquinone-2-sodium sulfonate, mixed evenly and added to the autoclave, Airtight.

[0043] 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.

[0044] 3) Add nitrogen, the space velocity is 4h -1, and start the stirrer, the stirring rate is 400rpm, the temperature is raised to 186° C., and the pressure is mai...

Embodiment 3

[0049] 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:

[0050] 1) Weigh 80g p-xylene, 400g acetic acid, 20g metal acetate (based on the whole solution, which contains 500ppmwCo 2+ 、250ppmw Mn 2+ 、25ppmw Ce 4+ ) and 0.55g 1,1,2,2-tetrabromoethane (based on the entire solution, bromine is 1000ppmw) and 5ppmw (based on the entire solution) anthraquinone-1-potassium sulfonate, mixed uniformly and added to the autoclave, Airtight.

[0051] 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.

[0052] 3) Add nitrogen, the space velocity is 4h -1 , and start the stirrer, the stirring rate is 400rpm, the temperature is raised to 186° C., and the pressure is...

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Abstract

The invention relates to a catalyst for preparing aromatic polycarboxylic acid through liquid-phase oxidation. The invention mainly aims to overcome the problem of high usage amount of bromine in conventional catalysts used for preparation of aromatic polycarboxylic acid through liquid-phase oxidation of polyalkyl substituted aromatic hydrocarbons. The catalyst comprises a Co salt, a Mn salt, a Ce salt, a bromine-containing compound and anthraquinone monosulfonate, wherein a weight ratio of Co to Mn to Ce to Br to anthraquinone monosulfonate is 500: (200-300): (20-100): (1000-2000): (5-20). With such a technical scheme, the above technical problem is overcome, and the catalyst can be used for production of aromatic polycarboxylic acid through liquid-phase oxidation of polyalkyl substituted aromatic hydrocarbons.

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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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/04C07C51/265C07C63/26
CPCC07C51/265B01J31/0225B01J31/0231B01J31/04B01J2231/70B01J35/19C07C63/26
Inventor 肖忠斌朱小丽孙广斌
Owner CHINA PETROLEUM & CHEM CORP
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