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Preparation of medium-temperature renewable hydrogen sulfide adsorbent and cyclic desulfurization method

A technology of hydrogen sulfide and adsorbent, which is applied in the direction of hydrogen sulfide, chemical instruments and methods, sulfur compounds, etc., can solve the problems of high operating cost, complicated process flow, and aggravated solid waste pollution, so as to reduce the impact, simple process, The effect of enhancing hydrophobicity

Inactive Publication Date: 2020-04-17
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the wet method has disadvantages such as high operation cost, large power consumption, complicated process flow, and secondary pollution caused by running, emitting, dripping, and leaking; while the dry method has high precision, but the desulfurizers are all discarded, and the desulfurization agent is discarded after the adsorption / reaction is saturated. State new adsorbent, aggravating solid waste pollution

Method used

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  • Preparation of medium-temperature renewable hydrogen sulfide adsorbent and cyclic desulfurization method

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Example 1: Preparation of coal-based reversible desulfurization activated carbon

[0034] The preparation method of the reversible desulfurization activated carbon taking anthracite and lignite as raw materials is as follows:

[0035] Take an appropriate amount of coal-based activated carbon and place it in a high-pressure reactor, place the reactor in a nickel protective device, and vacuumize it at 100°C for 2 hours; heat it to 120°C, and mix high-purity nitrogen and fluorine at a ratio of 7:3 Then pass through the reaction, and fluoride for 10 minutes. Add a beaker containing a mixed liquid of simethicone oil and tetraethyl orthosilicate to the reactor, the volume ratio of the two is 10:1, and place it separately from the activated carbon. The ratio of liquid to activated carbon is 0.5ml / g. The gas inlet and outlet of the reactor were closed, and under airtight conditions, the temperature of the reactor was controlled at 200° C., and a constant temperature heating t...

Embodiment 2

[0036] Example 2: Preparation of Coconut Shell Reversible Desulfurization Activated Carbon

[0037] The finished coconut shell activated carbon is placed in a high-pressure reactor, and the reactor is placed in a nickel protective device, vacuumized at 50°C for 2 hours; heated to 100°C, and mixed with high-purity nitrogen and fluorine at a ratio of 5:1 Then pass through the reaction, and fluoride for 10 minutes. Add a beaker containing a mixed liquid of simethicone and ethyl orthosilicate to the reactor, the volume ratio of the two is 20:1, and place it separately from the activated carbon. The ratio of liquid to activated carbon is 0.1ml / g. Close the gas inlet and outlet of the reactor, control the temperature of the reactor at 200°C under airtight conditions, and heat at a constant temperature for 60 minutes to obtain activated carbon for reversible desulfurization of coconut shells.

Embodiment 3

[0038] Example 3: Reversible desulfurization of dry-based coal-based shift gas

[0039] The vacuum pressure swing adsorption system for purification of dry-based coal-based shift gas consists of two desulfurization towers A and B, which are filled with coal-based reversible desulfurization activated carbon. 2 and CO 2(volume ratio 1:1) mixed gas for purging, and the purging pressure is normal pressure. The filling amount of activated carbon is configured according to the flow rate of raw gas.

[0040] After the shift gas enters the A desulfurization tower, the H in the gas 2 , CO 2 , CO, N 2 , CH 4 Outflow from the desulfurization tower outlet, H 2 S is adsorbed by the adsorbent. After about 1 hour, the adsorbent in A tends to be saturated, and it is replaced by B for adsorption. After the gas in A is reversed to normal pressure, the purge gas is reversed for 15 minutes, and vacuum desorption is performed for 15 minutes, and finally the purge is passed. Inflate the gas...

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Abstract

The invention discloses preparation of a medium-temperature renewable hydrogen sulfide adsorbent and a cyclic desulfurization method. The method comprises the steps: weighing a proper amount of activated carbon from coal or biomass and the like, putting into a reactor (such as a high-pressure reaction kettle), heating the reactor to 50-200 DEG C, and vacuumizing the reactor for 10 min or more; introducing the mixed gas of nitrogen and fluorine into the reactor, and fluorinating the activated carbon at the temperature of 40-120 DEG C for 5 min or more to obtain the fluorinated activated carbon;adding dimethicone and tetraethoxysilane as a mixed solution into a solution box, putting the solution box into the reactor, and heating at a constant temperature of 150-500 DEG C, enabling the fluorinated activated carbon to continuously react with mixed solution steam for 20 min or more, and thus obtaining the medium-temperature renewable hydrogen sulfide adsorbent; and filling the prepared adsorbent into a desulfurization tower, and carrying out medium-temperature vacuum pressure swing adsorption type desulfurization enrichment. The adsorbent has the advantages of adsorption-desorption regeneration function, high hydrogen sulfide recovery rate and the like.

Description

technical field [0001] The invention relates to the preparation of a medium-temperature renewable hydrogen sulfide adsorbent and its cycle desulfurization method, belonging to the technical field of gas purification. Background technique [0002] Synthesis gas / coke oven gas, etc. produced by gasification and coking processes using coal, natural gas, naphtha, heavy oil, etc. as raw materials, the main component is H 2 , CO, CO 2 , N 2 、CH 4 , water vapor, etc., for the convenience of desulfurization, after conversion or hydrolysis, the sulfur contained in coal generally exists in the state of hydrogen sulfide not greater than 2000ppm. Regardless of whether it is the use of subsequent purification links or environmental protection considerations, it is necessary to remove H through the purification section. 2 S is removed to obtain the ideal product gas. Generally, there are two kinds of purification methods: wet method and dry method. The representative technologies of w...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/30B01D53/04B01D53/047C01B3/56C10K1/32C01B17/16
CPCB01D53/04B01D53/047B01D2259/40043B01J20/20B01J2220/4806B01J2220/4812C01B3/56C01B17/167C01B2203/042C10K1/004C10K1/32
Inventor 史翊翔李爽蔡宁生郝培璇
Owner TSINGHUA UNIV