Preparation method for CNT (carbon nano tube)-SAPO (silicoaluminophosphate)-5 molecular-sieve composite membrane

A -SAPO-5, carbon nanotube technology, applied in the field of preparation of new carbon nanotube-SAPO-5 molecular sieve composite membrane, can solve the problems of natural gas and biogas calorific value reduction, unfavorable transportation and storage, etc., to promote directional growth , the effect of improving completeness and reducing production costs

Active Publication Date: 2012-07-18
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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AI Technical Summary

Problems solved by technology

[0005] The presence of carbon dioxide will reduce the calorific value of natural gas and biogas. At the same time, under the condition of water, it is highly acidic and corrosive, which is not conducive to transportation and storage.
However, carbon nanotubes are prepared in SAPO-5 molecular sieve membranes, that is, a new type of carbon nanotube-SAPO-5 molecular sieve composite membrane is synthesized and applied to CO 2 / CH 4 Separation, there is no literature report yet

Method used

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  • Preparation method for CNT (carbon nano tube)-SAPO (silicoaluminophosphate)-5 molecular-sieve composite membrane
  • Preparation method for CNT (carbon nano tube)-SAPO (silicoaluminophosphate)-5 molecular-sieve composite membrane
  • Preparation method for CNT (carbon nano tube)-SAPO (silicoaluminophosphate)-5 molecular-sieve composite membrane

Examples

Experimental program
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Effect test

Embodiment 1

[0028] (1) Preparation of non-oriented FeSAPO-5 molecular sieve membrane on flake alumina support

[0029] According to 1Al 2 o 3 : 1.3P 2 o 5 : 0.5SiO2 2 :3TPABr:1000H 2 O:0.3FeCl 3 (mol) ratio of materials to prepare synthetic liquid. The aluminum source in the reaction is aluminum isopropoxide. In order to fully dissolve it, aluminum isopropoxide is added to an aqueous phosphoric acid solution (50%-85% by mass), and stirred and dissolved at 60°C for about 5 hours. , the dissolved aluminum isopropoxide aqueous solution is basically a transparent liquid. Then FeCl 3 It was added to an aqueous phosphoric acid solution in which aluminum isopropoxide was dissolved, and stirred at room temperature for 2 hours. Then TPABr and tetraethyl orthosilicate were gradually added dropwise to the mixed solution, and stirred for two hours. After all substances were completely dissolved, the pH of the reaction solution was adjusted to about 6. The reaction solution was aged at room ...

Embodiment 2

[0039] (1) Preparation of NiSAPO-5 molecular sieve membrane on a sheet-like alumina carrier

[0040] According to 1Al 2 o 3 : 0.8P 2 o 5 : 0.05SiO2 2 : 0.5TPAOH : 45H 2 O: 0.075Ni(NO 3 ) 2 (mol) ratio of materials to prepare synthetic liquid. The aluminum source in the reaction is sodium aluminate, and the fully dissolved sodium aluminate aqueous solution is basically a transparent liquid. Then, phosphoric acid dissolved with a certain amount of nickel nitrate was added dropwise to the sodium aluminate aqueous solution, and stirred at room temperature for 24 hours. Then TPAOH and silica sol were gradually added dropwise to the mixed liquid in sequence, and the stirring was continued for 2 hours. After all the substances were completely dissolved, the pH of the reaction liquid was adjusted to about 2. The reaction solution was aged at room temperature for 20 hours before being added to the reactor. Then 30ml of synthetic solution and α-Al 2 o 3 The carrier is placed...

Embodiment 3

[0047] (1) Preparation of NiSAPO-5 molecular sieve membrane on tubular alumina carrier

[0048] Using the prior art-low-speed pulling method, first use 0.1-1.5wt% PVA aqueous solution to make the prepared NiSAPO-5 molecular sieve small particles (synthesized by microwave method) into 0.5-1wt% seed liquid; then The tubular alumina carrier is immersed in the seed liquid, and the carrier is pulled at a constant speed of 0.1-1cm / min; after standing for 1 hour at room temperature and in a low-dust environment, it is dried in an oven at 80°C for 24 hours. Repeat this operation 1-2 times, and a denser NiSAPO-5 molecular sieve seed layer can be prepared. Then, according to the steps described in Example 2, a complete tubular NiSAPO-5 molecular sieve membrane was prepared, the Ph value of the synthesis solution was adjusted to 4.5, and the mixed solution of tetraethylorthosilicate and silica sol was used as the silicon source of the synthesis solution.

[0049] (2) Detection of the in...

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Abstract

The invention discloses a preparation method for a CNT (carbon nano tube)-SAPO (silicoaluminophosphate)-5 molecular-sieve composite membrane. The preparation method comprises the following steps that: (1) synthetic liquid is prepared, and the molar composition of raw materials of the synthetic liquid is that Al2O3: P2O5: SiO2: Template: H2O: X equals to 1: a: b: c: d: e, wherein a is equal to 0.8-1.3, b is equal to 0.05-1, c is equal to 0.15-1, d is equal to 45-1000, and e is equal to 0.075-0.3; (2) a porous support is put into a high-pressure crystallization reaction kettle, the synthetic liquid is added to promote full crosslinking growth among molecular sieve crystals, and finally, the complete molecular sieve membrane is formed; and (3) an organic template is removed by the catalytic property of a heteroatoms-containing SAPO-5 molecular sieve. According to the invention, intergranular defects can be effectively prevented from forming in the molecular sieve membrane, and a split organic template agent can form a CNT tube in a molecular sieve pore passage so as to improve the hydrophobic property of the molecular sieve membrane. According to the invention, technological conditions are moderate, the operation is simpler, costs are lower, the applicability is wider, and not only is the large-scale production of molecular sieve membranes facilitated, but also the industrialized application of the molecular sieve membranes in separation of gas and separation of low-concentration organics is facilitated.

Description

technical field [0001] The invention belongs to the technical field of inorganic membrane materials and membrane separation, and in particular relates to a preparation method of a novel carbon nanotube-SAPO-5 molecular sieve composite membrane. technical background [0002] Molecular sieve membrane is a new type of microporous inorganic membrane developed in the past ten years. Because of its good integrity, it can meet the requirements of high flux, high selectivity, heat resistance, and solvent corrosion resistance. It has better performance than organic membranes. Therefore, it has been valued by people and has become the fastest-growing and one of the most promising membrane materials in the membrane field. The pores of the molecular sieve membrane have a certain shape and controllable structure, the pore size is adjustable and evenly distributed, and the pore size is similar to the molecular size. Due to the specific pore structure of the molecular sieve membrane, it h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54
Inventor 杨文申郎林阴秀丽吴创之
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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