Process for preparing catalyst Pd/TiO2 for hydrogenation of p-carboxybenzaldehyde

A technology of p-carboxybenzaldehyde and hydrogenation process, which is applied in the direction of physical/chemical process catalysts, organic compound preparation, carboxylate preparation, etc. It can solve the problems of poor high-temperature activity of catalysts, lower compressive strength, etc., and achieve conversion rate High, prevent aggregation, improve the effect of compressive strength

Active Publication Date: 2009-01-21
SINOPEC YANGZI PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Pd/TiO for the hydrogenation process of p-carboxybenzaldehyde in the prior art 2 The compressive strength of the catalyst is significantly reduced in a high-temperature, high-pressure aqueous environment, and the high-te

Method used

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  • Process for preparing catalyst Pd/TiO2 for hydrogenation of p-carboxybenzaldehyde
  • Process for preparing catalyst Pd/TiO2 for hydrogenation of p-carboxybenzaldehyde

Examples

Experimental program
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Embodiment 1

[0032] (1) Add 1 part of ground alkali-free glass fiber to 20 parts of TiO 2 In the powder, mix on a high-speed pulverizer for 30 minutes. Add 1 part of binder methyl cellulose to 10 parts of deionized water at 85°C. After the methyl cellulose swells, cool to room temperature, then add 0.3 parts of peptizing agent nitric acid, and stir evenly to form a gel. Add the resulting gel to the above-mentioned E-glass fiber and TiO 2 In the powder, after kneading on the kneader for 1h, extrude with extruder (extrusion diameter 1.5mm), cut into strips of 5-6mm, and then dry at 100°C for 10h, at 2.5°C / min The heating rate was raised to 700 °C and kept at a constant temperature for 5 hours to prepare ground alkali-free glass fiber doped TiO 2 molding carrier.

[0033] (2) According to the volume ratio of titanium-containing precursor tetrabutyl titanate and absolute ethanol as 1:1, tetrabutyl titanate was added into absolute ethanol, and stirred for 30 minutes to obtain a uniform and t...

Embodiment 2

[0038] According to the volume fraction ratio of the titanium-containing precursor isopropyl titanate and absolute ethanol as 1:3, the isopropyl titanate was added into the absolute ethanol, and stirred for 30 minutes to obtain a uniform and transparent solution. Other steps are the same as in Example 1, making 0.5%Pd / TiO of the present invention 2 catalyst.

Embodiment 3

[0040] According to the volume fraction ratio of the titanium-containing precursor ethyl titanate and absolute ethanol as 1:5, the ethyl titanate was added into the absolute ethanol and stirred for 30 minutes to obtain a uniform and transparent solution. Other steps are the same as in Example 1, making 0.5%Pd / TiO of the present invention 2 catalyst.

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Abstract

The invention relates to a Pd/TiO2 catalyst used in the hydrogenation of 4-carboxybenzaldehyde; the catalyst takes TiO2 forming material, which is doped with ground alkali-free glass fibers and adopts titanium-containing precursors for surface modification, as the carrier, and is loaded with an active component, metal Pd; the content of metal Pd in the catalyst is 0.2-1.0%, the titanium-containing precursor can be any one of or the combination of tetrabutyl titanate, tetraisopropyl titanate and tetraethyl titanate. The compressive strength of the catalyst is 110-160N/cm; after reaction, the compressive strength of the catalyst is reduced by less than 13%; in the high-temperature and high-pressure water phase environment, the hydrogenation activity of the catalyst is high, and the transformation rate of 4-carboxybenzaldehyde is higher than 99.0%. The preparation method of the catalyst of the invention has simple technique, and the adopted method does not cause any negative impact on the catalyst and is suitable for the industrial production.

Description

technical field [0001] The present invention relates to a kind of Pd / TiO for hydrogenation reaction 2 Catalyst preparation method, especially related to the supported Pd / TiO used in the hydrogenation process of p-carboxybenzaldehyde under high temperature and high pressure 2 Catalyst preparation method. 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 and refining at a high temperature of 270-285 ° C...

Claims

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Application Information

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IPC IPC(8): B01J23/42C07C63/26C07C51/487B01J21/06
Inventor 姚小利王继元曾崇余陈韶辉李晓强柏基业汪洋堵文斌卞伯同
Owner SINOPEC YANGZI PETROCHEM
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