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Charcoal molecular sieve preparation method

A carbon molecular sieve and carbonization technology, applied in the field of chemical production, can solve the problems of wide pore size distribution of CMS, serious equipment corrosion and high production cost, and achieve the effect of narrow pore size distribution range, easy operation and control, and low production cost.

Inactive Publication Date: 2016-02-10
SHAANXI SHENGHUIYUAN INFORMATION SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the dense microstructure of petroleum coke, a large amount of activator (potassium hydroxide) is required for activation, resulting in high production costs, serious equipment corrosion, and large pollution; Chinese patent CN1462650A uses petroleum coke as raw material, and uses petroleum pitch, ethylene cracking tar or Coal tar is used as a binder, kneaded with water, formed, and after drying and carbonization, the pore size treatment process of the combination of controlled activation and two-component pore adjustment method is used to obtain CMS with rich micropores.
Tar or asphalt binders contain more harmful substances and pollute the environment; using benzene or gasoline impregnating agents to adjust pores, it is difficult to achieve fine control of micropore size and pore volume; it is difficult to open petroleum coke using physical activation methods Dense microporous structure, the produced CMS has a wide pore size distribution, which is not suitable for the separation of mixed components with similar molecular scales such as air
There is no report on foreign patents for producing CMS from petroleum coke

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take the pulverized petroleum coke raw material 300 8 , add binder (thermosetting phenolic resin), auxiliary agent (starch) and water and knead evenly, wherein coke powder: binder: auxiliary agent: water = 1: 0.2: 0.05: 0.6, and then extrude. Dry at 110°C for 2 hours to make cylindrical pellets with a diameter of 2 mm and a length of 3 to 5 mm. The shaped and dried particles were raised to 800°C at a heating rate of 5°C / min in an electric converter, carbonized for 1 hour, and the carrier gas N 2 The flow rate is 130ml / min; after carbonization, pass water at a rate of 0.45ml / min to activate for 0.5h, and finally pass benzene at a temperature of 750°C for 1h to adjust the pores. The flow rate of benzene is 0.135ml / min, and CMS is obtained after cooling. The strength of the prepared CMS measured by the drum reaches 99.5%, N 2 The total pore volume measured by adsorption is 0.021ml / g, and the air separation performance N 2 The export concentration is 88%. The test resul...

Embodiment 2

[0021] Take 300g of coke powder, 300ml of 98% concentrated sulfuric acid and 30ml of 30% hydrogen peroxide, stir and mix evenly, react for 1h, then wash with deionized water until the pH value is 5-6, dry at about 80°C for 2h, and finally place in a steel retort with 10- The heating rate is 20°C / min, and the temperature is rapidly raised to 750°C, staying for 0.5h, and the carrier gas N 2 The flow rate is 100ml / min to prepare pretreated petroleum coke powder. Then follow the molding, carbonization, activation, and deposition steps of Example 1. The strength of the prepared CMS measured by the drum reaches 99.4%, N 2 The total pore volume measured by adsorption is 0.043ml / g, and the outlet concentration of the air separation performance team measured by the double-tower pressure swing adsorption device is 96.8%.

Embodiment 3

[0023] Take 300g of coke powder, 300ml of 98% concentrated sulfuric acid and 15ml of 30% hydrogen peroxide, stir and mix evenly, react for 1h, then wash with deionized water until the pH value is 5~6, dry at about 80°C for 2h, and finally put it in a steel retort with 10~ The heating rate is 20°C / min, and the temperature is rapidly raised to 750°C, staying for 0.5h, and the carrier gas is N 2 The flow rate is 100ml / min to prepare pretreated petroleum coke powder. Then follow the molding, carbonization, activation, and deposition steps of Example 1. The strength of the prepared CMS measured by the drum reaches 99.6%, N 2 The total pore volume measured by adsorption is 0.048ml / g, and the air separation performance N 2 The export concentration is 98.1%.

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Abstract

The present invention discloses a charcoal molecular sieve preparation method, which is characterized by comprising: pre-crushing petroleum coke, carrying out an impregnated oxidation intercalation expansion treatment on the raw material with an oxidizing agent and an intercalation agent, carrying out further fine crushing on the sample, adding a right amount of an adhesive, an adhesive auxiliary agent and water, kneading, carrying out molding treatment on the kneaded material after the uniform kneading, carrying out drying treatment on the molded material, carrying out carbonization, and carrying out controlled physical activation and carbon deposition pore adjusting treatment according to the requirement so as to obtain the charcoal molecular sieve. According to the present invention, the intercalation pretreatment is performed on the petroleum coke, such that the size of the microcrystalline is reduced, the formed distance d002 vaoue between the layer sheets is incrased, the developed micropores are provided, the surface structure of the petroleum coke is changed, the further activation hole adjusting treatment is easily achieved, and the obtained product has characteristics of high strength, rich micropore and narrow pore size distribution, and can be used for nitrogen production through PSA air separation, and enrichment of methane in gas or natural gas.

Description

technical field [0001] The invention relates to the technical field of chemical production, and mainly relates to a method for preparing carbon molecular sieves. Background technique [0002] Carbon molecular sieve (CMS) refers to a microporous carbon material with pores close to the size of the adsorbed molecule and uniform pore size distribution. It is widely used in the fields of adsorption separation, purification and catalysis, and is mainly used as an adsorbent in the pressure swing adsorption (PSA) process. Widely used in small and medium-scale air separation to prepare N-rich 2 gas. The performance of CMS and its manufacturing cost are largely determined by the raw materials used and the process used. For the industrial production of CMS, the development of new raw materials to reduce production costs will bring huge economic and social benefits. There are a wide range of raw materials used to prepare CMS, ranging from carbon-containing plants or minerals (coal, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 陈彬曲维龙
Owner SHAANXI SHENGHUIYUAN INFORMATION SCI & TECH
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