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Slurry bed hydrogenation catalyst, and preparation method and application thereof

A hydrogenation catalyst and slurry bed technology are applied in the field of slurry bed hydrogenation catalyst and its preparation, and can solve the problems of low hydrogenation efficiency, poor selectivity, and reduction of precious metal content, etc.

Inactive Publication Date: 2019-06-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] Aiming at the disadvantages of low hydrogenation efficiency and poor selectivity in existing slurry bed hydrogenation catalysts, the object of the present invention is to provide a highly dispersed supported catalyst for hydrogenation of anthraquinone to produce hydrogen peroxide and a preparation method thereof, Improve single-pass hydrogen efficiency and effective anthraquinone selectivity, and further reduce the content of precious metals

Method used

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  • Slurry bed hydrogenation catalyst, and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1) Preparation of Silica Hydrogenation Catalyst

[0045] Weigh 2 g of spherical silicon oxide powder with a particle size of 200-400 mesh, place the above powder in a tubular calcining furnace, and then perform nitridation treatment on the silicon oxide carrier through the following procedure.

[0046] a) First, the gas in the roasting tube is replaced by nitrogen gas for 30 minutes, and the oxygen content in the tail gas of the detection device is lower than 0.5%.

[0047] b) feeding into the mixed gas of nitrogen and ammonia with a volume flow of 30ml / min, wherein the volume concentration of ammonia is 70%;

[0048] c) adopt the heating rate to be 5 ℃ / min and be heated to 750 ℃, and obtain the nitrided silicon oxide carrier after maintaining this temperature for 24hr;

[0049] D) configure the palladium nitrate aqueous solution of 2mg / ml, then add above-mentioned palladium nitrate solution 5ml in the silicon oxide carrier of nitridation, then carry out 120 ℃ of dryin...

Embodiment 2

[0057] Preparation of Silica Hydrogenation Catalyst

[0058] The preparation of the hydrogenation catalyst supported by silicon oxide is similar to the above-mentioned method for supporting the active components of silicon nitride oxide. Briefly, prepare 20ml of 10mg / ml palladium nitrate aqueous solution, then weigh 2g of spherical silicon oxide powder with a particle size of 200-400 mesh, add 5ml of palladium nitrate solution of the above-mentioned concentration to the above-mentioned silicon oxide powder, and then carry out 120 ° C. Dry, 350 ℃ of calcinations 3hr obtain the palladium catalyst of oxidation state; Put the palladium catalyst of above-mentioned oxidation state into the tubular furnace, pass into the hydrogen that volume flow is 30ml / min, at temperature, be obtained after reducing 5hr at 80 ℃ Hydrogenation palladium catalyst.

[0059] The physical parameters of amorphous silica are shown in Table 1. The comparative results of hydrogenation evaluation are as fol...

Embodiment 3

[0061] Preparation of Silica Hydrogenation Catalyst

[0062] The preparation steps are as described in Example 1; other conditions are the same, the concentration of ammonia gas in the mixed gas of nitrogen gas and ammonia gas is 10%, and the nitriding time is kept at 1 hr. The physical parameters of silicon oxide after nitridation are shown in Table 1.

[0063] The silicon oxide nitrogen content after nitridation measured by the alkali fusion method was 0.9%. The evaluation results of the hydrogenation catalyst are as follows: figure 1 shown.

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Abstract

The invention provides a slurry bed liquid phase hydrogenation catalyst and an application thereof. The catalyst adopts one or a combination of more than one of noble metals Pd, Pt and Rh as a main active component, the carrier of the catalyst is mainly a nitrogen-containing silicon oxide carrier, the average pore diameter of the catalyst carrier is more than 10 nm, and the pore volume of the catalyst carrier is not higher than 0.7 cc / g. The introduction of an amino group to the carrier greatly increases the dispersity of the noble metal(s), so the hydrogenation activity is improved, and the use amount of the noble metal(s) is reduced; and the modification of the surface of the nitrogen-containing silicon oxide carrier with the amino group further improves the desorption of a hydrogenationintermediate, thereby the selectivity, activity and stability of anthraquinone hydrogenation are improved. The catalyst of the invention can be used in the process of catalytic hydrogenation of anthraquinone in a slurry bed to produce hydrogen peroxide, and the hydrogenation catalyst has a very high hydrogenation activity and good stability at a reaction temperature of 40-60 DEG C under a pressure of 0.05-0.3 MPa and at a liquid space velocity of 60-300 h<-1>.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and particularly relates to a slurry bed hydrogenation catalyst and a preparation method and application thereof. Background technique [0002] The final product decomposed during the use of hydrogen peroxide is mainly water, which does not produce secondary pollutants and is an environmentally friendly chemical. As a green chemical product, hydrogen peroxide can be used as oxidant, bleach, disinfectant, polymer initiator, etc., and is widely used in chemical synthesis, papermaking, textile, environmental protection, food, electronics, aerospace and other industries. With the continuous development of green chemical process and the increasingly strict national environmental protection regulations, especially hydrogen peroxide as a green oxidant and an environmentally friendly bleaching agent and disinfectant are widely used. For example, in the field of green chemicals: caprolactam, cyclohe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C01B15/023
Inventor 王树东苏宏久杨晓野李大卫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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