Method for preparing carbon molecular sieve by intercalation of petrol coke
A technology of carbon molecular sieve and petroleum coke, which is applied in the field of chemical production, can solve the problems of wide pore size distribution of CMS, severe equipment corrosion, and high production cost, and achieve the effects of narrow pore size distribution range, easy operation and control, and low production cost
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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 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 flow rate of carrier gas N2 was 130 ml / min; after carbonization, water was activated at a rate of 0.45 ml / min for 0.5 h; When the temperature was 750°C, benzene was introduced for 1 hour to adjust the pores, the flow rate of benzene was 0.135ml / min, and CMS was 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 conc...
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, and then wash with deionized water until the pH value is 5 ~ 6. Dry at about 80°C for 2 hours, and finally dry it in a steel retort for 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, and then wash with deionized water until the pH value is 5 ~ 6. Dry at about 80°C for 2 hours, and finally dry it in a steel retort for 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 2The 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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