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Method for preparing carbon molecular sieve by preoxidation of petrol coke

A pre-oxidation treatment, carbon molecular sieve technology, applied in the field of chemical production, can solve the problems of compact structure of petroleum coke and difficulty in pore formation, and achieve the effect of narrow pore size distribution, low ash content and abundant micropores

Inactive Publication Date: 2007-03-28
DALIAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of petroleum coke with dense structure and difficult pore formation, and provide a method for preparing CMS suitable for air separation by pre-oxidizing petroleum coke

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 (comparative example):

[0023] Take 300g of pulverized petroleum coke raw material, add an appropriate amount of 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 extruded. Dry at 110°C for 2 hours to make a diameter of 2 mm and a length of 3 ~ 5mm cylindrical pellets. 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; 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 N2 outlet conce...

Embodiment 2

[0025] Take 300g of coke powder and 300ml of 98% concentrated sulfuric acid, stir and mix evenly, react for 1h, and then wash with deionized water until the pH value is 5 ~ 6. Dry at about 100°C for 2 hours to obtain 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 99.1%, N 2 The total pore volume measured by adsorption is 0.060ml / g, and the air separation performance N 2 The export concentration is 97.2%.

Embodiment 3

[0027] Take 300g of coke powder and 300ml of 20% nitric acid solution, stir and mix evenly, react for 1h, and then wash with deionized water until the pH value is 5 ~6. Dry at about 100°C for 2 hours to obtain 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 99.1%, N 2 The total pore volume measured by adsorption is 0.062ml / g, and the air separation performance N2 outlet concentration measured by the double-tower pressure swing adsorption device is 97.9%.

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PUM

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Abstract

The invention relates to a method for preparing carbon molecular sieve by petroleum coke preoxidation treatment, comprising the steps of: firstly crushing petroleum coke, then adopting oxidant to make dipping oxidizing treatment on the petroleum coke powder to change its chemical composition and surface properties so as to benefit formation and development of hole structure in the follow-up carbonizing and activating courses; then adding in a proper amount of adhesive, bonding assistant and water to knead uniformly, moulding the kneaded matter, drying and carbonizing the moulded matter, and controlling activation and carbon deposition hole regulation treatments according to the requirements. And it has beneficial effects of: high product intensity, large micropore capacity, narrow aperture distribution, and the product can be used to make nitrogen by air separation with PSA process.

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 pre-oxidation treatment of petroleum coke. Background technique [0002] Carbon molecular sieve (CMS) refers to a carbon material with a relatively uniform developed microporous structure, and the pore size distribution is generally between 0.3 and 1.0nm. It is widely used in the fields of adsorption separation, purification and catalysis, such as pressure swing adsorption (PSA) The adsorbent of the process is 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, ran...

Claims

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Application Information

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IPC IPC(8): C01B31/08
Inventor 徐绍平卢春兰苏泉声刘书林刘淑琴刘长厚
Owner DALIAN UNIV OF TECH
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