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Crude terephthalic acid hydrofining catalyst

A crude terephthalic acid, hydrorefining technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, carboxylate preparations, etc., can solve problems such as catalyst poisoning, and improve the Anti-toxic effect

Active Publication Date: 2016-04-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] One of the problems to be solved by the present invention is that in the prior art, after the acetic acid in the crude terephthalic acid is removed by washing with PX, the remaining PX will poison the Pd / C catalyst used for refining the crude terephthalic acid. Provide A catalyst for crude terephthalic acid hydrorefining, the catalyst has the characteristics that it is not affected by PX for CTA hydrorefining

Method used

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Experimental program
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Effect test

Embodiment 1

[0019] The preparation of catalyst: first according to the Pd content in Pd-Ce-Hf / C catalyst is 0.5wt%, Ce content is 0.2wt% and Hf content is 0.4wt% and weighs the corresponding mass of H 2 PdCl 4 , CeCl 3 and HfCl 4 And dissolve it in 15wt% hydrochloric acid to form 250ml impregnation solution, mix the resulting impregnation solution with 50 grams of activated carbon, impregnate for 12h, then vacuum dry at 110°C for 3h to obtain a catalyst precursor, and finally use 5 times the volume of nitrogen diluted hydrogen Reduction at 160°C for 3 hours at 150ml / min and filtration to obtain the finished Pd-Ce-Hf / C catalyst. According to ICP-AES analysis, the Pd content in the catalyst is 0.5wt%, the Ce content is 0.2wt%, and the Hf content is 0.4wt%. , for the convenience of comparison, the resulting catalyst composition is listed in Table 1.

[0020] Catalyst evaluation: 18g of crude terephthalic acid containing 3300ppm p-carboxybenzaldehyde (4-CBA), 5wt% PX, 42g of water and 2g o...

Embodiment 2

[0022] The preparation of catalyst: first according to the Pd content in Pd-Ce-Hf / C catalyst is 0.1wt%, Ce content is 0.2wt% and Hf content is 0.4wt% and weighs the corresponding mass of H 2 PdCl 4 , CeCl 3 and HfCl 4 And dissolve it in 15wt% hydrochloric acid to form 250ml impregnation solution, mix the resulting impregnation solution with 50 grams of activated carbon, impregnate for 12h, then vacuum dry at 110°C for 3h to obtain a catalyst precursor, and finally use 5 times the volume of nitrogen diluted hydrogen Reduction at 150ml / min at 160°C for 3h and filtration to obtain the finished Pd-Ce-Hf / C catalyst. According to ICP-AES analysis, the Pd content in the catalyst is 0.1wt%, the Ce content is 0.2wt% and the Hf content is 0.4wt%. , for the convenience of comparison, the resulting catalyst composition is listed in Table 1.

[0023] Catalyst evaluation: 18g of crude terephthalic acid containing 3300ppm p-carboxybenzaldehyde (4-CBA), 5wt% PX, 42g of water and 2g of the ...

Embodiment 3

[0025] The preparation of catalyst: first according to Pd-Ce-Hf / C catalyst, Pd content is 0.45wt%, Ce content is 0.2wt% and Hf content is 0.4wt% and weighs the H of corresponding mass 2 PdCl 4 , CeCl 3 and HfCl 4 And dissolve it in 15wt% hydrochloric acid to form 250ml impregnation solution, mix the resulting impregnation solution with 50 grams of activated carbon, impregnate for 12h, then vacuum dry at 110°C for 3h to obtain a catalyst precursor, and finally use 5 times the volume of nitrogen diluted hydrogen Reduction at 160°C for 3 hours at 150ml / min and filtration to obtain the finished Pd-Ce-Hf / C catalyst. According to ICP-AES analysis, the Pd content in the catalyst is 0.45wt%, the Ce content is 0.2wt% and the Hf content is 0.4wt%. , for the convenience of comparison, the resulting catalyst composition is listed in Table 1.

[0026] Catalyst evaluation: 18g of crude terephthalic acid containing 3300ppm p-carboxybenzaldehyde (4-CBA), 5wt% PX, 42g of water and 2g of the...

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Abstract

The invention relates to a crude terephthalic acid hydrofining catalyst, and solves the problem that in the prior art, when PX is employed to wash for removal of acetic acid from crude terephthalic acid, the residual PX can cause poisoning of a Pd / C catalyst used for crude terephthalic acid refining. According to a technical scheme, the catalyst for crude terephthalic acid refining adopts activated carbon as the carrier, includes Pd, Ce and Hf as the active components, and can be applied to the industrial production of purified terephthalic acid.

Description

technical field [0001] The invention relates to a catalyst for hydrogenation refining of crude terephthalic acid, a preparation method thereof, and a method for hydrogenation refining of crude terephthalic acid containing PX. Background technique [0002] The production process of purified terephthalic acid (PTA) is to prepare crude terephthalic acid (CTA) by oxidizing p-xylene (PX) as raw material, and then send CTA to subsequent hydrogenation after crystallization, filtration and drying. The refining unit finally gets the PTA product. The drying unit is an operating unit that consumes a lot of energy in the PTA production process. It is prone to tube wall formation and corrosion in the dryer, which seriously affects the quality and output of PTA. It is the bottleneck of PTA production increase and energy saving. And it is a very effective method to adopt solvent to wash CTA filter cake to remove acetic acid, wherein it is the most economical to wash CTA filter cake with P...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63C07C63/26C07C51/42C07C51/487
CPCY02P20/52
Inventor 朱庆才畅延青陈大伟
Owner CHINA PETROLEUM & CHEM CORP
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