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Method for preparing TiO2-C composite carrier for p-carboxybenzaldehyde hydrogenation process

A technology of p-carboxybenzaldehyde and composite carrier, which is applied in the preparation of organic compounds, carboxylate preparation, catalyst carrier, etc. It can solve the problems of reduced specific surface area and pore volume, easy collapse of pore structure, and poor thermal stability of the carrier. , to achieve the effect of improving hydrogenation performance, enhancing affinity and preventing aggregation

Active Publication Date: 2013-04-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] TiO for p-carboxybenzaldehyde hydrogenation process in the prior art 2 The carrier has disadvantages such as poor thermal stability, easy collapse of pore structure, sharp decrease in specific surface area and pore volume, and easy transformation of crystal structure during the calcination process. The present invention provides a high-stability TiO 2 The preparation method of -C composite carrier

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) 1g phenolic resin is added in 20g ethanol, obtain the ethanolic solution containing phenolic resin;

[0029] (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;

[0030] (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.

[0031] The composite carrier obtained in this embodiment has the following pr...

Embodiment 2

[0033] (1) 2g phenolic resin is joined in 20g ethanol, obtain the ethanolic solution containing phenolic resin;

[0034] (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;

[0035] (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.

[0036] The composite carrier obtained in this embodiment has the following properties: the sp...

Embodiment 3

[0038] (1) 0.2g phenolic resin is joined in 20g ethanol, obtain the ethanolic solution containing phenolic resin;

[0039] (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;

[0040] (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.

[0041] The composite carrier obtained in this embodiment has the following properties: the specific surface area is 144.7m 2 / g, pore volume 0.5cm 3 / g, the cr...

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Abstract

The invention discloses a method for preparing a TiO2-C composite carrier for a p-carboxybenzaldehyde hydrogenation process. The preparation 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 a part of TiO2 powder; and (3) mixing the macromolecular compound modified TiO2 powder obtained in the step (2), the reset TiO2 powder and gel uniformly, kneading the mixture uniformly, and performing extrusion molding. The obtained formed product is thermally solidified and roasted in nitrogen atmosphere to form the TiO2-C composite carrier. The TiO2-C composite carrier has high specific surface area and pore volume and stable crystal structure, a Pd / TiO2-C catalyst prepared by using the carrier has high activity, and the conversion rate of the p-carboxybenzaldehyde can reach 99.5 percent. The preparation method is simple in process and is suitable for industrialized production.

Description

technical field [0001] The present invention relates to a kind of TiO used for hydrogenation reaction 2 -A preparation method of a composite carrier, the carrier is mainly used as a carrier for hydrogenation catalysts of aromatic aldehydes such as p-carboxybenzaldehyde. 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 contain...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J32/00B01J21/18B01J23/44C07C63/26C07C51/487
Inventor 王继元曾崇余堵文斌卞伯同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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