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Heterogeneous composite structure adsorption materials, and preparation method and application thereof

A composite structure and adsorption material technology, applied in other chemical processes, chemical instruments and methods, separation methods, etc., can solve problems such as control accuracy limitations

Active Publication Date: 2017-05-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As far as the current adsorption and separation materials for methane are concerned, the control accuracy of the pores and surface properties of various materials is limited by technological means. It is difficult to realize the surface properties and separation window while ensuring the well-developed pores inside the material itself Strict control of size

Method used

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  • Heterogeneous composite structure adsorption materials, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1: Preparation of activated carbon@Al-BDC composite material

[0039] Weigh 20g Al(SO 4 ) 3 18H 2 O, dissolved in 300ml water, then weighed 0.8g specific surface area 1000m 2 / g of activated carbon powder was put into the solution, stirred for 30min, then 30mL of 28% ammonia water was added dropwise, the mixed solution was transferred into a flask, and heated to 80°C for 10h; the temperature was naturally lowered and filtered to obtain the activated carbon composite intermediate , washed twice with 50ml of water, then dried at 80°C for 6h;

[0040] Weigh 15g terephthalic acid (H 2 BDC) in 300ml DMF, stirred for 20min until uniformly mixed, transferred to an autoclave, then put the above-mentioned activated carbon composite intermediate into the solution, and reacted at 130°C for 12h under stirring conditions; naturally lowered the temperature, took out the activated carbon composite, and then The activated carbon@Al-BDC composite adsorption material was pre...

Embodiment 2

[0043] Example 2: Preparation of activated carbon fiber@CuBTC composite material

[0044] Weigh 12g Cu(NO 3 ) 2 ·3H 2 O, dissolved in 300ml water, then weighed 0.5g specific surface area 1000m 2 1 / g of activated carbon fiber was put into the solution, stirred for 30min, then 15g of sodium bicarbonate was added dropwise, the mixture was transferred to a flask, and heated to 100°C for reflux for 8h; the temperature was naturally lowered to form an activated carbon fiber composite intermediate, and Wash twice with 50ml of water, then dry at 80°C for 6h;

[0045] Take by weighing 15g p-trimesic acid (H 2BTC) was dissolved in 300ml of ethanol and water (1:1) mixture, stirred for 20min until evenly mixed, transferred to an autoclave, and then the above activated carbon fiber composite intermediate was vertically inserted into the solution, and the reaction kettle was placed in an oven React at 60°C for 24h; cool down naturally, take out the activated carbon fiber composite, the...

Embodiment 3

[0048] Example 3: Preparation of SAPO-34@[Co 3 (HCOO) 6 ] composite material

[0049] Weigh 10g SAPO-34, 2.81g CoSO 4 ·7H 2 O, 10g of ammonium bicarbonate in 300ml of water, stirred for 30min until evenly mixed, transferred to a three-necked flask, reacted at 75°C for 8h; cooled naturally, filtered, washed twice with 40ml of water, and dried at 110°C for 12h , to obtain the compound intermediate of SAPO-34;

[0050] Weigh 10g of formic acid in 120ml of DMF, add the above-mentioned SAPO-34-metal precipitate precursor into the solution, stir for 30min until the mixture is uniform, transfer it to an autoclave, and place it in a rotary oven at 100°C for 12h; cool down naturally, filter , and then washed twice with 50ml DMF and acetone respectively, the filter cake was dried at 60°C for 2h, and then dried and activated at 160°C and vacuum (0.2bar) for 12h to obtain SAPO-34@[Co 3 (HCOO) 6 ] Composite adsorption material.

[0051] The obtained adsorbent material N 2 The speci...

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Abstract

The invention provides metal-organic framework composite structure adsorption materials, and a preparation method and a methane separation application thereof. The above composite structure adsorbents are heterogeneous coated structures, adopt a metal-organic framework material as a coating layer, and adopt porous active carbon, molecular sieve or a molecular sieve and active carbon compound as an internal coated layer. The invention also provides the preparation method of the heterogeneous composite structure materials. The method adopts a two-step technology, and comprises the following steps: growing a metal compound precursor on an inner layer substrate through using a chemical precipitation technology, converting the metal compound into the metal-organic framework coating layer by using a water / dissolving heat process, and carrying out washing, drying and activation to form the adsorbents. The surface area of the adsorbents is 200-2000 m<2> / g, the average aperture of the adsorbents is 0.4-1 nm, and the adsorbents have excellent CH4-N2 and CH4-CO2 adsorption separation performances, and can be used in methane purification adsorption materials; and the preparation method has the advantages of simplicity, good repeatability and easiness in industrialization.

Description

technical field [0001] The invention relates to the design and preparation of novel adsorbents and the technical field of adsorption and separation engineering of mixed gases, in particular to a novel composite structure adsorption material for adsorption and separation of methane and a preparation method thereof. Background technique [0002] Natural gas accounts for about 24% of the world's current energy consumption, and has become the most important low-carbon clean fuel and chemical raw material. It is estimated that by 2035, the proportion of natural gas in primary energy consumption will exceed that of coal and oil, becoming the world's largest energy consumption. In 2014, the apparent consumption of natural gas in my country was 180 billion cubic meters, of which 58 billion cubic meters were imported, and the degree of dependence on foreign countries reached 32.2%. According to the "Energy Development Strategic Action Plan 2014-2020" issued by the State Council, by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01D53/02
CPCY02C20/40
Inventor 王树东孙天军刘小伟胡江亮李德伏赵生生
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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