Preparation method of eggshell type anthraquinone hydrogenation fixed bed catalyst

A fixed bed catalyst, eggshell technology, applied in chemical instruments and methods, inorganic chemistry, peroxides/peroxyhydrates/peroxyacids/superoxides/ozone oxides, etc., can solve the problem of increasing catalyst production costs , reduce the catalyst hydrogenation activity, complex catalyst components and other problems, to achieve the effect of low production cost, simple preparation process and high catalyst activity

Inactive Publication Date: 2014-04-09
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The problems in the above-mentioned patents are mainly that the catalyst components are complex and the preparation process is cumbersome, which increases the production cost of the catalyst; in addition, most catalysts are directly dried and calcined after the impregnation operation. Experiments have shown that this will leave impurity ions on the surface of the catalyst, thereby Cover the active center of the catalyst surface to reduce the hydrogenation activity of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 10g spherical alumina carrier, the carrier is θ-Al 2 o 3 , the specific surface area is 98m 2 / g, pore volume 0.5ml / g, average pore diameter 14nm, bulk density 0.45g / ml, Na content 0.07%, Fe content 0.07%, particle size 2-3mm, compressive strength 50N / particle, and tested at 150℃ Spherical alumina was dried for 12 hours. A certain amount of palladium chloride PdCl 2 Mix with dilute hydrochloric acid, and fully stir and dissolve in a water bath at 50°C to form a 0.003g / mL chloropalladium acid solution, and then use 1mol / L sodium hydroxide solution to adjust the pH of the above solution to make the final chloropalladium The pH of the acid solution is 3.0, and this solution is the dipping solution. The aforementioned 10 g of spherical alumina carrier was put into 20 ml of the aforementioned impregnating solution, and carried out in a water bath at 30° C. for 2 h. After the impregnation, the catalyst was washed with desalted water with a conductivity of 0.5 μS / cm...

Embodiment 2

[0036] Weigh 10g spherical alumina carrier, the carrier is δ-Al 2 o 3 , the specific surface area is 150m 2 / g, pore volume 1.2ml / g, average pore diameter 11nm, bulk density 0.5g / ml, Na content 0.05%, Fe content 0.05%, particle size 3mm, compressive strength 30N / particle, and spherical oxidation at 180°C Aluminum was dried for 12 hours. A certain amount of palladium chloride PdCl 2 Mix with dilute hydrochloric acid, and fully stir and dissolve in a water bath at 60°C to form a 0.0032g / mL chloropalladium acid solution, and then use 0.5mol / L sodium hydroxide solution to adjust the pH of the above solution to make the final chlorine The pH of the palladium acid solution is 3.5, which is the immersion solution. Put the aforementioned 10 g of spherical alumina carrier into 20 ml of the aforementioned impregnating solution, and carry out 45 min under the condition of a water bath at 50° C. After the impregnation, the catalyst was washed with desalted water with a conductivity o...

Embodiment 3

[0038] Weigh 10g spherical alumina carrier, the carrier is δ-θ-mixed crystal phase Al 2 o 3 , with a specific surface area of ​​70m 2 / g, pore volume 0.3ml / g, average pore diameter 25nm, bulk density 0.5g / ml, Na content 0.05%, Fe content 0.05%, particle size 2.8mm, compressive strength 50N / particle, and spherical at 170°C Aluminum oxide was dried for 6h. A certain amount of palladium chloride PdCl 2 Mix with dilute hydrochloric acid, and fully stir and dissolve in a water bath at 70°C to form a 0.004g / mL chloropalladium acid solution, and then use 1mol / L sodium carbonate solution to adjust the pH of the above solution to make the final chloropalladium acid The pH of the solution is 4.0, and the solution is an impregnation solution. The aforementioned 10 g of spherical alumina carrier was put into 18 ml of the aforementioned impregnating solution, and carried out in a water bath at 60° C. for 45 min. After the impregnation, the catalyst was washed with desalted water with ...

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Abstract

The invention relates to a preparation method of an eggshell type anthraquinone hydrogenation fixed bed catalyst, wherein the eggshell type anthraquinone hydrogenation fixed bed catalyst is prepared from a spherical Al2O3 carrier through the steps of pre-drying processing, medium temperature soaking, desalted water washing, drying, activation calcination and the like. The preparation method has the beneficial effects that the preparation process of the catalyst is simple, the production cost is low, the hydrogenation efficiency is high, the selectivity is good, the hydrogenation efficiency is greater than 9 g / L, and the selectivity is grater than 99.5%; active metal palladium of the catalyst is tightly attached to the outer surface of the catalyst and is distributed in an eggshell type, and the thickness of a soaking layer is 50-80 microns and is beneficial to efficient utilization of precious metal palladium. The working procedure of washing is introduced in the preparation process of the catalyst, and the washing process is quantified.

Description

technical field [0001] The invention belongs to the technical field of catalyst production, and in particular relates to a preparation method of an eggshell-type anthraquinone hydrogenation fixed-bed catalyst. Background technique [0002] Hydrogen peroxide is an aqueous solution of hydrogen peroxide. It is known as the cleanest oxidant because of its non-polluting characteristics during use. At present, hydrogen peroxide is mainly used to prepare products such as bleaching agent, disinfectant, deoxidizer, polymer initiator and crosslinking agent, and is widely used in papermaking, textile, medicine, environmental protection and other industries. In recent years, my country's hydrogen peroxide industry has developed rapidly, and its production capacity has grown at a rate of 15% per year. At present, the national production capacity has exceeded 7 million tons per year (calculated at a concentration of 27.5%). In addition, with the rapid promotion of hydrogen peroxide in va...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C01B15/023
Inventor 史文涛马国栋耿玉侠钱震左宜赞崔艳杰陈晨张蒙王海国石华王亮张舜光刘俊生李玉龙
Owner CHINA TIANCHEN ENG
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