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Preparation method of palladium adsorbent for benzene refining desulfurization as well as product and application of palladium adsorbent

A kind of adsorbent and product technology, applied in the field of palladium adsorbent for refined desulfurization of benzene, which can solve the problems of short application life, failure to meet production requirements, and high operating conditions

Active Publication Date: 2014-05-21
YICHANG SUPENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, not only the equipment investment is large, but the operating conditions are high, and the sulfur content in benzene after hydrosulfurization can only reach the ppm level at the lowest level, which cannot meet the production requirements
Prepare Pd / Al by Existing Methods 2 o 3 The activity of the adsorbent is lower than that of the surface, so its application life in production is short, and the activation cycle is also short, which is not conducive to stable production

Method used

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Examples

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Effect test

preparation example Construction

[0014] The present invention is used for the preparation method of the palladium adsorbent of benzene refining desulfurization, and its steps are as follows:

[0015] 1. Use alumina as the carrier: the alumina carrier is made of alumina powder obtained by neutralizing aluminum sulfate and sodium aluminate and alumina powder obtained by quick-release method or carbonization method, which is formed by rolling ball or extrusion or dripping The spherical shape of ¢1-3mm is obtained by ball molding, kept in an oven at 80-200°C for 6-24 hours, and roasted at 300-800°C for 1-10 hours.

[0016] 2. Treat the alumina carrier prepared above with an alkali metal or alkaline earth metal salt, the weight ratio of the alkali metal or alkaline earth metal salt to the alumina carrier is 0.1 to 1:100, and dry it in an oven at 100 to 200°C for 2 ~24 hours. As the alkali metal or alkaline earth metal salt, choose one of sodium carbonate and potassium phosphate.

[0017] 3. Immerse or spray the ...

Embodiment 1

[0022] The alumina powder obtained by neutralizing sodium aluminate and aluminum sulfate and the alumina powder obtained by the quick-release method are mixed uniformly in a weight ratio of 1:1 to obtain a ¢1-3mm spherical alumina carrier. Dry for 12 hours, and bake at 650°C for 6 hours in an air atmosphere to obtain a carrier. Alumina carrier specific surface area 220~320m 2 , the pore volume is 0.5-0.8, the average pore diameter is 7.5-12nm, the bulk specific gravity is 0.40-0.55g / ml, and the strength is 10-40N / average per particle.

[0023] The weight ratio of the palladium salt to the carrier is 1.66:100, and the weight ratio of the co-active component transition metal salt to the carrier is 0.2:100. Na 2 CO 3 Dissolve in water to make a 2% concentration solution, immerse the alumina carrier in it for 15 minutes, wash with pure water until the pH value is 11, and then bake in an oven at 100°C for 10 hours to obtain alumina. Take 4.15gPdCl 2 Add HCl to dissolve, add 0....

Embodiment 2

[0027] The alumina powder obtained by neutralizing sodium aluminate and aluminum sulfate and the alumina powder obtained by the quick-release method are mixed uniformly in a weight ratio of 1:1 to obtain a ¢1-3mm spherical alumina carrier. Dry for 12 hours, and bake at 650°C for 6 hours in an air atmosphere to obtain a carrier. Alumina carrier specific surface area 220~320m 2 , the pore volume is 0.5-0.8, the average pore diameter is 7.5-12nm, the bulk specific gravity is 0.40-0.55g / ml, and the strength is 10-40N / average per particle.

[0028] The weight ratio of the palladium salt to the carrier is 1.3:100, and the weight ratio of the co-active component transition metal salt to the carrier is 0.2:100. Na 2 CO 3 Dissolve in water to make a 2% concentration solution, immerse the alumina carrier in it for 15 minutes, wash with pure water until the pH value is 11, and then bake in an oven at 100°C for 10 hours to obtain alumina. Take 3.25gPdCl 2Add HCl to dissolve, add 0.5g...

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PUM

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Abstract

The invention relates to a preparation method of a palladium adsorbent for benzene refining desulfurization as well as a product and application of the palladium adsorbent. Alumina powder prepared by two different methods is prepared into spherical alumina carriers with the dimension phi being 1.0 to 3.0mm in a ball rolling forming, extrusion forming or ball dripping forming mode, alkali metal and alkaline-earth metal treatment is carried out, active ingredient palladium and other transition metal salts are steeped or sprayed and coated on the carrier in two times, and reducing agent and other salts need to be used for reduction treatment after the steeping. The palladium adsorbent prepared by the method has the advantages that the bulk specific weight is 0.40 to 0.55 kg / l, the palladium content is 0.8 to 1.2 weight percent, the palladium adsorbent is used for the benzene refining sulfur suction process, the sulfur content in benzene is reduced to 1 to 2ppb after the adsorption, the use airspeed is 1 to 10 hr<-1>, the use temperature is 100 to 200 DEG C, and the use pressure is 8atm to 10 atm. The benzene treated by the product provided by the invention can meet the mass requirement of the benzene raw material in benzene hydrogenation cyclohexane production process.

Description

technical field [0001] The present invention relates to a palladium adsorbent for refined desulfurization of benzene, and in particular discloses a preparation method and application of a palladium adsorbent for the refined desulfurization of benzene in the production process of benzene hydrogenation to cyclohexane and its application. Activity specific surface of the palladium adsorbent. Background technique [0002] With the gradual manifestation of the superior performance of new chemical materials, the application of new chemical materials has developed rapidly. Caprolactam is also an important new chemical material. The production process of caprolactam is as follows: benzene undergoes hydrogenation, oxidation, separation of alcohol and ketone, ammoximation of cyclohexanone, and secondary rearrangement to produce caprolactam. [0003] Benzene is the raw material at the source of production. The benzene hydrogenation process requires the use of noble metal catalysts, so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/08B01J20/32C07C15/04C07C7/12
Inventor 傅骐
Owner YICHANG SUPENG TECH CO LTD
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