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A kind of preparation method of palladium adsorbent used for deep desulfurization of benzene

A deep desulfurization and adsorbent technology, applied in chemical instruments and methods, adsorption purification/separation, other chemical processes, etc., can solve the problem of low sulfur in palladium adsorbent, achieve the effect of improving desulfurization performance and reducing the cost of use

Active Publication Date: 2021-11-05
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of this, the present invention aims to propose a method for preparing a palladium adsorbent for deep desulfurization of benzene, to solve the problem that the sulfur capacity of the palladium adsorbent prepared by the existing process is low, and simultaneously realize the metal palladium on the carrier. Evenly dispersed, improving its deep desulfurization performance as a whole

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 300g of alumina pellets with a diameter of 1.5-2.0mm, the specific process is as follows:

[0026] S1: Place alumina pellets in 3000g of 5wt% Na 2 CO 3 After soaking in the aqueous solution for 1 hour at 25°C, take it out, remove the excess solution on the surface and wash until the washing water pH=8, and dry at 110°C for 8 hours to obtain the treated alumina carrier.

[0027] S2: Soak the treated carrier in 20wt% sucrose solution, dry at 80°C for 24h; carbonize in an autoclave at 220°C for 4h, cool naturally to room temperature to obtain an alumina carrier loaded with porous carbon spheres.

[0028] Repeat the above soaking and carbonization process for a total of 2 times.

[0029] S3: Accurately weigh palladium acetate according to the Pd content of 1.0wt%, dissolve palladium acetate in acetone solution, soak at 25°C for 4h, and dry at 100°C for 12h.

[0030] S4: Calcining the palladium adsorbent precursor obtained in step S3 in a pure oxygen atmosphere at 25...

Embodiment 2

[0032] Take 300g of alumina pellets with a diameter of 1.5-3.0mm, the specific process is as follows:

[0033] S1: Place alumina pellets in 6000g of 2wt% Na 2 CO 3 After soaking in an aqueous solution for 3 hours at 50°C, take it out, remove excess solution on the surface and wash until the pH of the washing water is 8, and dry at 100°C for 12 hours to obtain a treated alumina carrier.

[0034] S2: Soak the treated carrier in 10wt% sucrose solution, dry at 60°C for 24h; carbonize in an autoclave at 180°C for 6h, cool naturally to room temperature to obtain an alumina carrier loaded with porous carbon spheres.

[0035] Repeat the above soaking and carbonization process for a total of 4 times.

[0036] S3: Accurately weigh palladium nitrate according to the Pd content of 0.9wt%, dissolve palladium nitrate in water, soak at 40°C for 1h, and dry at 80°C for 24h,

[0037] S4: Calcining the palladium adsorbent precursor obtained in step S3 in a 50vol% oxygen atmosphere at 350° C....

Embodiment 3

[0039] Take 100g of alumina pellets with a diameter of 2.0-4.0mm, the specific process is as follows:

[0040] S1: Place alumina pellets in 2000g of 3wt% K 2 CO 3 After soaking in an aqueous solution for 1 hour at 25°C, take it out, remove excess solution on the surface and wash until the pH of the washing water is 8, and dry at 110°C for 8 hours to obtain a treated alumina carrier.

[0041] S2: Soak the treated carrier in 15wt% sucrose solution, dry at 80°C for 24h; carbonize in an autoclave at 200°C for 6h, cool naturally to room temperature to obtain an alumina carrier loaded with porous carbon spheres.

[0042] Repeat the above soaking and carbonization process for a total of 3 times.

[0043] S3: Accurately weigh palladium acetate according to the Pd content of 1.0wt%, dissolve palladium acetate in acetone solution, soak at 25°C for 4h, and dry at 90°C for 18h.

[0044] S4: Calcining the palladium adsorbent precursor obtained in step S3 in an atmosphere of 40vol% oxyge...

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Abstract

The invention relates to a preparation method of a palladium adsorbent used for deep desulfurization of benzene. The method utilizes a carbon template agent that can leave reductive groups after carbonization to increase the sulfur capacity of the palladium adsorbent, comprising: in the palladium adsorbent precursor In the preparation process, the solution of the carbon template agent is used to impregnate the adsorbent carrier, and then it is dried and calcined to obtain the loaded palladium adsorbent. The invention can realize the uniform dispersion of the active component palladium, which can be used for the deep desulfurization of refined benzene, and can reduce the thiophene in refined benzene to below 10ppb, and the sulfur capacity of the adsorbent is relatively large, up to 1.9g thiophene / kg Adsorbent. The invention can realize high dispersion of metal palladium, weaken the strong interaction between metal palladium and alumina carrier, and is more conducive to improving the desulfurization performance of the palladium adsorbent, especially in the process of deep desulfurization of benzene. The use cost of the palladium adsorbent is reduced.

Description

technical field [0001] The invention relates to the technical field of palladium adsorbents, in particular to a preparation method of a high-sulfur-capacity palladium adsorbent used for deep desulfurization of benzene. Background technique [0002] Caprolactam is an important chemical monomer, and its demand is also increasing year by year. In recent years, the process of producing cyclohexene by partial hydrogenation using ruthenium-zinc as a catalyst is the core link of caprolactam production. The ruthenium catalyst is very sensitive to sulfur, and a trace amount of thiophene will reduce its catalytic performance and even lead to catalyst deactivation. Therefore, the content of thiophene in the raw material benzene should be strictly controlled below 100ppb, even below 10ppb. [0003] Conventional desulfurization methods such as sulfuric acid refining, extractive distillation, freezing crystallization, hydrodesulfurization, etc. are difficult to completely remove trace t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30C07C15/04C07C7/12
CPCB01J20/02B01J20/08B01J20/20B01J20/28021C07C7/12C07C15/04
Inventor 张媛王绍伟吕睿袁海朋王志文刘新伟王聪刘文刚陈云祥
Owner CHINA TIANCHEN ENG
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