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An adsorbent for separating low-concentration methane based on attapulgite nanorod crystal composite two-dimensional metal-organic framework and its preparation method

A metal-organic framework and nanorod crystal technology, which is applied in separation methods, methane capture, and dispersed particle separation, can solve the problems of no mention of methane/nitrogen separation ratio, no advantages, complex processes, etc., and achieve high-efficiency selection Excellent adsorption capacity, low cost, and wide range of raw material sources

Active Publication Date: 2019-08-06
常州市金坛区溶解乙炔有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses micropowdered phenolic resin as a raw material, carbonizes and then carbonizes a carbon molecular sieve with a pore-adjusting agent, wherein the pore-adjusting agent is an organic compound such as benzene, toluene, xylene, etc., which causes problems such as complex process and environmental pollution.
[0010] CN102363117A discloses a special carbon adsorbent for methane in pressure swing adsorption. The carbon adsorbent uses coal powder, coal tar, potassium hydroxide, potassium nitrate, calcium carbonate and magnesium chloride as raw materials, and has a complex composition. Although the methane adsorption capacity reaches 25.0mL / g, but does not mention the separation ratio of methane / nitrogen
[0013] CN105688870A discloses a preparation method of an X-type molecular sieve / LDHs composite adsorbent for pressure swing adsorption separation of methane and nitrogen, which enhances the performance of X-type molecular sieves on N in the PSA process. 2 adsorption effect, due to its preferential adsorption of N 2 , so it is not suitable for the selective separation of low-concentration methane and nitrogen
However, ordinary three-dimensional metal-organic framework adsorption is not advantageous for the selective adsorption of low-concentration methane.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] (1) reflux attapulgite nanorod crystals with a high aspect ratio greater than 20 and a silane coupling agent hydrolyzate in a mass-to-volume ratio of 50:1 g / ml for 2 h; filter, and wash with distilled water until neutral;

[0050] (2) 1g of 4,4'-bipyridine is dissolved in 100ml of ethanol to obtain solution A;

[0051] (3) 5g 2,5-dihydroxybenzoic acid and 0.8g copper nitrate trihydrate are dissolved in 100ml water to obtain solution B;

[0052] (4) adding 0.2 g of neutral attapulgite nanorod crystals prepared in step (1) into solution A, then slowly adding solution B to all of them, and mixing them uniformly with ultrasonic waves;

[0053] (5) put the mixed solution obtained in step (4) into an autoclave, let stand at 180°C for 24h, and filter to obtain green needle-like crystals;

[0054] (6) heating the green needle-like crystals to 110° C., vacuum drying for 5 hours, and preparing the finished adsorbent.

Embodiment 2

[0056] (1) The high aspect ratio attapulgite nanorod crystals with an aspect ratio greater than 20 and the silane coupling agent hydrolyzate are refluxed for 2h for 2h in a mass-to-volume ratio of 100:1g / ml; filter, and wash with distilled water until neutral;

[0057] (2) 1g of 4,4'-bipyridine is dissolved in 100ml of ethanol to obtain solution A;

[0058] (3) 5g 2,5-dihydroxybenzoic acid and 0.8g copper nitrate trihydrate are dissolved in 100ml water to obtain solution B;

[0059] (4) adding 0.2 g of neutral attapulgite nanorod crystals prepared in step (1) into solution A, then slowly adding solution B to all of them, and mixing them uniformly with ultrasonic waves;

[0060] (5) put the mixed solution obtained in step (4) into an autoclave, let stand at 200°C for 20h, and filter to obtain green needle-like crystals;

[0061] (6) heating the green needle-like crystals to 120° C. and vacuum drying for 6 hours to prepare the finished adsorbent.

Embodiment 3

[0063] (1) The high aspect ratio attapulgite nanorod crystals with an aspect ratio greater than 20 and the hydrolyzed solution of the silane coupling agent are refluxed for 2 h for 2 h in a mass volume ratio of 75:1 g / ml; filter, and wash with distilled water until neutral;

[0064] (2) 1g of 4,4'-bipyridine is dissolved in 100ml of ethanol to obtain solution A;

[0065] (3) 5g 2,5-dihydroxybenzoic acid and 0.8g copper nitrate trihydrate are dissolved in 100ml water to obtain solution B;

[0066] (4) adding 0.2 g of neutral attapulgite nanorod crystals prepared in step (1) into solution A, then slowly adding solution B to all of them, and mixing them uniformly with ultrasonic waves;

[0067] (5) put the mixed solution obtained in step (4) into an autoclave, let stand at 180°C for 24h, and filter to obtain green needle-like crystals;

[0068] (6) heating the green needle-like crystals to 110° C., vacuum drying for 5 hours, and preparing the finished adsorbent.

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Abstract

The invention discloses a low-concentration methane separation adsorbent based on compounding of attapulgite nanorod crystal and a two-dimensional metal organic framework and a preparation method of the low-concentration methane separation adsorbent. The adsorbent is prepared by compounding of high-aspect-ratio attapulgite nanorod crystal and a two-dimensional flexible organic framework material. The novel adsorbent prepared on the basis of compounding of the attapulgite nanorod crystal and the two-dimensional metal organic framework is low in adsorption opening pressure and high in adsorption capacity of methane gas in a methane and nitrogen system and is especially applicable to low-concentration methane adsorption. In addition, the preparation method is simple, convenient, extensive in raw material source, low in cost and promising in industrial application prospect.

Description

technical field [0001] The invention relates to an adsorbent for separating methane by pressure swing adsorption, in particular to an adsorbent for separating low-concentration methane based on attapulgite nanorod crystal composite two-dimensional metal-organic framework and a preparation method thereof. Background technique [0002] Coalbed methane, commonly known as coal mine gas, is mainly composed of methane (CH 4 ), with a small amount of ethane (C 2 H 6 ) and propane (C 3 H 8 ) and other light hydrocarbons and air mixture, is a valuable energy resource. There are many high-gas mines in my country, and coal mine gas has always been a major hidden danger in coal mine safety production. In recent years, major gas explosion accidents in coal mines have occurred from time to time, causing heavy losses to people's lives and properties. The explosion concentration range of methane is 4.5%-15%. The direct and effective method to prevent gas outburst is to extract gas bef...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30B01D53/047
CPCB01D53/047B01D2253/11B01D2253/204B01D2257/7025B01J20/12B01J20/226Y02C20/20
Inventor 胡涛陈静金叶玲钱运华汪玉祥陈铭予袁旭
Owner 常州市金坛区溶解乙炔有限公司
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