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Preparation method for palladium-on-carbon catalyst used for purifying terephthalic acid

A palladium-carbon catalyst, terephthalic acid technology, applied in catalyst activation/preparation, organic compound preparation, carboxylate preparation and other directions, can solve the problems of many washing steps, short life, large water consumption, etc., and achieve competitive adsorption Improve, strengthen competitive adsorption, improve the effect of dispersion

Inactive Publication Date: 2013-06-19
大连科诺催化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing methods for producing palladium-carbon catalysts are relatively complicated, including: water washing, pickling, water washing and neutralization, and drying treatment of activated carbon, palladium adsorption, water washing and neutralization, reduction, water washing and neutralization, and drying to obtain finished products. Steps, the preparation process is complicated, there are many washing steps, and the water consumption is large. Most processes cannot be carried out at room temperature, and the temperature requirements are strict. It is necessary to configure corresponding equipment suitable for this process. The equipment investment is large. The particles are relatively large, generally above 4-15 nanometers, so the dispersion of the catalyst is low and the service life is short

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 520g of 4-8 mesh activated carbon into the reactor, add 1000mL of water, stir and polish for 2 hours, wash with water until there is no carbon powder, and control the water. This process does not require circulating water washing; add phosphoric acid with a concentration of 0.1N into the reactor The solution was 1500mL, so that the liquid level was 1cm higher than the activated carbon plane, and circulated for 12 hours; hydrogen peroxide was added according to the molar ratio of oxidant and carrier carbon of 1:50, and circulated for 1 hour to complete the treatment of the carrier activated carbon.

[0028] Continue to add 250 grams of palladium compound solution (containing 2.5 grams of palladium according to the preparation conversion) and glyceryl laurate in the reaction kettle, the mol ratio of palladium and glyceryl laurate is 100: 0.1, circulate for 6 hours; then add in the solution of potassium carbonate And to pH 7.0, circulate for 1 hour; dissolve 5 times P...

Embodiment 2

[0030] 1. Grinding for 4 hours;

[0031] 2. Use phosphoric acid solution with a concentration of 0.2N to make the liquid level 2cm higher than the activated carbon plane, and circulate for 10 hours;

[0032] 3. Add hydrogen peroxide according to the molar ratio of oxidant and carrier carbon of 1:100, and circulate for 2 hours;

[0033] 4. Add palladium solution, the molar ratio of palladium to dispersant is 100:0.5, and circulate for 8 hours. The dispersant uses glyceryl laurate and glyceryl myristate, and the molar ratio between the two is 1:1. ;

[0034] 5. Add potassium carbonate solution to neutralize to pH 7.5, and circulate for 3 hours;

[0035] 6. Use 10 times Pd 2+ moles of ascorbic acid, circulated for 42 hours;

[0036] 7. Washing.

[0037] Parts not listed in detail are the same as in Example 1.

Embodiment 3

[0039] 1. Grinding for 10 hours;

[0040] 2. Use 0.5N phosphoric acid solution to circulate for 8 hours;

[0041] 3. Add hydrogen peroxide according to the molar ratio of oxidant and carrier carbon of 1:400, and circulate for 4 hours;

[0042] 4. Add palladium solution, the molar ratio of palladium to glyceryl laurate is 100:1, and circulate for 12 hours;

[0043] 5. Add alkali to neutralize to a pH value of 8.0, and circulate for 6 hours. The alkali is composed of potassium carbonate and potassium hydroxide, and the weight ratio between the two is 1:1;

[0044] 6. Use 15 times Pd 2+ The reductant of the number of moles circulates for 36 hours, and the reductant adopts two components of ascorbic acid and sodium citrate, and the molar ratio between the two is 1:1;

[0045] 7. Washing.

[0046] Parts not listed in detail are the same as in Example 1.

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Abstract

The present invention relates to a preparation method for a palladium-on-carbon catalyst used for purifying terephthalic acid, and the method comprises processing steps of polishing and washing of a carrier activated carbon, the acid treatment and the oxidation-reduction treatment to the carrier activated carbon, and the palladium adsorption, alkali neutralization, reduction, washing, etc., to finally obtain the catalyst. The method is characterized in that: a dispersing agent having competitive adsorption and stabilizing effects and a reducing agent are selected, and saponified substances generated from the alkali neutralization are used, to together strengthen the competitive adsorption between ions, so metal palladium active components can be uniformly distributed on the activated carbon, thereby improving dispersion, and reducing particle sizes; and the various materials added during the preparation process are maintained in a reactor until the end of the reaction, and a high-performance catalyst is obtained with a final particle size of less than 2 nm.

Description

technical field [0001] The invention relates to a method for preparing a catalyst, in particular to a method for preparing a palladium-carbon catalyst for refining terephthalic acid. Background technique [0002] The method of industrial production of terephthalic acid is mainly completed by two steps of oxidation and hydrofinishing, wherein the palladium-carbon catalyst for hydrofinishing is one of the core technologies. Existing methods for producing palladium-carbon catalysts are relatively complicated, including: water washing, pickling, water washing and neutralization, and drying treatment of activated carbon, palladium adsorption, water washing and neutralization, reduction, water washing and neutralization, and drying to obtain finished products. Steps, the preparation process is complicated, there are many washing steps, and the water consumption is large. Most processes cannot be carried out at room temperature, and the temperature requirements are strict. It is ne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/16B01J37/02C07C63/26C07C51/487
Inventor 陈安尚邹德强韩继业
Owner 大连科诺催化有限公司
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