Method for preparing carbon molecular sieve by intercalation of petrol coke

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

Inactive Publication Date: 2010-05-12
DALIAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the compact microstructure of petroleum coke, a large amount of activator (potassium hydroxide) is required for activation, resulting in higher 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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  • Method for preparing carbon molecular sieve by intercalation of petrol coke

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1 (comparative example):

[0025] Take 300g of pulverized petroleum coke raw material, 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, 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 carbonized in an electric converter at a heating rate of 5 °C / min to 800 °C for 1 h, and the carrier gas was N 2 The flow rate is 130ml / min; after carbonization, pass water at a rate of 0.45ml / min for 0.5h to activate; 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 outlet concent...

Embodiment 2

[0027] 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 air separation performance N 2 The export concentration is 96.8%.

Embodiment 3

[0029] 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 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 99.6%, N2 The total pore volume measured by adsorption is 0.048ml / g, and the air separation performance N 2 The outlet concentration is 98.1%.

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Abstract

The invention relates to a method of preparing carbon molecular sieve by petroleum coke intercalation treatment, firstly precrushing petroleum coke, then adopting oxidiant and intercalator to make dipping oxidizing and intercalating expanding treatments on raw materials, further finly crushing the sample, then adding in a proper amount of adhesive agent, bonding assistant and water to knead uniformly, moulding the kneaded matter, drying and carbonizing the moulded matter, controlling physical activation and carbon deposition hole regulating treatments according to the requirements, and obtaining the carbon molecular sieve. And it has beneficial effects of: high product intensity, rich micropores, and narrow aperture distribution, and the product can be used to make nitrogen by air separation with PSA process, and enrich methane in gas or natural gas.

Description

technical field [0001] The invention belongs to the technical field of chemical production and relates to a method for preparing carbon molecular sieves through petroleum coke intercalation treatment. 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...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C01B31/08B01J20/20
Inventor徐绍平卢春兰苏泉声刘书林刘淑琴刘长厚
OwnerDALIAN UNIV OF TECH