Method for preparing noble metal/TiO2-C catalyst for hydrofining of crude terephthalic acid

A crude terephthalic acid, hydrogenation and refining technology, applied in the direction of metal / metal oxide / metal hydroxide catalyst, organic compound preparation, physical / chemical process catalyst, etc., can solve the problem of easy collapse of pore structure and specific surface area And the reduction of pore volume, the easy transformation of crystal structure, etc., to achieve the effect of enhancing affinity, improving hydrogenation performance, and simple process

Active Publication Date: 2013-02-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] TiO for the crude terephthalic acid hydrorefining process in the prior art 2 The carrier has poor thermal stability during calcination, easy collapse of pore structure, sharp decrease in specific surface area and pore volume, easy transformation of crystal structure, and Pd / TiO 2 The catalyst has disadvantages such as poor high-temperature activity, and the present invention provides a high-stability and high-activity noble metal / TiO for crude terephthalic acid hydrotreating 2 The preparation method of -C catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) 1g phenolic resin is added in 20g ethanol, obtain the ethanolic solution containing phenolic resin;

[0041] (2) The specific surface area of ​​20g is 300m 2 / g, pore volume 0.6cm 3 / g, anatase TiO 2 16g of the powder was added to the ethanol solution containing phenolic resin obtained in (1), stirred evenly at room temperature, and the excess ethanol was evaporated under reduced pressure at 80°C to obtain phenolic resin-modified TiO 2 Powder, crushed for later use;

[0042] (3) TiO modified with the phenolic resin obtained in (2) 2 powder and the remaining 4g TiO 2 After the powder is mixed evenly, it is mixed with 10 g of gel containing water, binder methylcellulose, and peptizing agent nitric acid, kneaded evenly on a kneader, and extruded. The obtained molding was cured at 120°C for 10h, and fired at 800°C for 4h under a nitrogen atmosphere to obtain TiO 2 -C composite carrier;

[0043] (4) the TiO obtained in (3) 2 -C composite support is impregnated wi...

Embodiment 2

[0047] (1) 2g phenolic resin is joined in 20g ethanol, obtain the ethanolic solution containing phenolic resin;

[0048] (2) The specific surface area of ​​20g is 300m 2 / g, pore volume 0.6cm 3 / g, anatase TiO 2 Add 10 g of the powder into the ethanol solution containing phenolic resin obtained in (1), stir evenly at room temperature, and evaporate excess ethanol at 80°C under reduced pressure to obtain phenolic resin-modified TiO 2 Powder, crushed for later use;

[0049] (3) TiO modified with the phenolic resin obtained in (2) 2 Powder and remaining 10g TiO 2 After the powder is mixed evenly, it is mixed with 10 g of gel containing water, binder methylcellulose, and peptizing agent nitric acid, kneaded evenly on a kneader, and extruded. The obtained molding was cured at 120°C for 10h, and fired at 800°C for 4h under a nitrogen atmosphere to obtain TiO 2 -C composite carrier;

[0050] (4) the TiO obtained in (3) 2 -C composite support is impregnated with a solution con...

Embodiment 3

[0054] (1) 0.2g phenolic resin is joined in 20g ethanol, obtain the ethanolic solution containing phenolic resin;

[0055] (2) The specific surface area of ​​20g is 300m 2 / g, pore volume 0.6cm 3 / g, anatase TiO 2 Add all the powder into the ethanol solution containing phenolic resin obtained in (1), stir evenly at room temperature, evaporate excess ethanol at 80°C under reduced pressure, and obtain phenolic resin-modified TiO 2 Powder, crushed for later use;

[0056] (3) TiO modified with the phenolic resin obtained in (2) 2 The powder is mixed with 10 g of gel containing water, binder methyl cellulose, and peptizer nitric acid, kneaded evenly on a kneader, and extruded. The obtained molding was cured at 120°C for 10h, and fired at 500°C for 4h under a nitrogen atmosphere to obtain TiO 2 -C composite carrier;

[0057] (4) the TiO obtained in (3) 2 -C composite support is impregnated with a solution containing palladium chloride, so that palladium chloride is loaded on ...

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Abstract

The invention discloses a method for preparing a noble metal / TiO2-C catalyst for hydrofining of crude terephthalic acid. The method sequentially comprises the following steps of: (1) adding a macromolecular compound into an organic solvent to obtain clarified solution containing the macromolecular compound; (2) adding TiO2 powder; (3) adding TiO2 powder and gel, and performing extrusion molding; and (4) soaking the TiO2-C composite carrier obtained in the step (3) into solution containing a noble metal compound, and performing calcination and hydrogen reduction to obtain the noble metal / TiO2-C catalyst for hydrofining of the crude terephthalic acid. The Pd / TiO2-C catalyst has high specific surface area and pore volume, stable crystal structure and high activity; and the terephthalic acid after hydrofining has low impurity content. The preparation method is simple in process, does not produce any adverse influence on the catalyst, and is suitable for industrialized production.

Description

technical field [0001] The present invention relates to a noble metal / TiO for hydrogenation reaction 2 -C Catalyst preparation method, especially related to noble metal / TiO for crude terephthalic acid hydrorefining 2 The preparation method of -C catalyst. Background technique [0002] Purified terephthalic acid (PTA) is a very important organic chemical raw material, and its downstream processing products are mainly polyester fibers, polyester films, packaging bottles and PET engineering plastics. In the crude terephthalic acid (CTA) produced by the liquid-phase oxidation of p-xylene (PX), it generally contains 2000-3000 μg / g of p-carboxybenzaldehyde (4-CBA), the main impurity, because its aldehyde group is relatively active, It will affect the color of polyester fiber. It is necessary to convert 4-CBA into p-toluic acid, which is easily soluble in hot water, by hydrogenation refining at a high temperature of 270-285 ° C. The refined terephthalic acid contains 25 μg / g of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/38B01J23/44B01J23/42B01J23/46B01J32/00B01J21/18C07C63/26C07C51/487
Inventor 卞伯同王继元曾崇余堵文斌陈韶辉杨爱武李晓强柏基业朱庆奋庞焱
Owner CHINA PETROLEUM & CHEM CORP
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