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ERI configuration phosphorous-aluminum molecular sieve membrane, preparation method and applications thereof

A phospho-aluminum molecular sieve, molecular sieve technology, applied in molecular sieve and alkali exchange of phosphate, separation method, molecular sieve characteristic silicoaluminophosphate and other directions, can solve the problem of difficulty in preparing pure-phase SAPO-17 molecular sieve, unfavorable large-scale preparation, time required Long and other problems, to achieve the effect of shortening the crystallization time, high carbon dioxide separation performance, and complete coverage

Active Publication Date: 2016-12-21
南京方膜高科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adopt in-situ synthesis method (Zeolites, 13(1993) 549-556.) to be difficult to prepare pure phase SAPO-17 molecular sieve, and required time is longer, is unfavorable for large-scale preparation

Method used

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  • ERI configuration phosphorous-aluminum molecular sieve membrane, preparation method and applications thereof
  • ERI configuration phosphorous-aluminum molecular sieve membrane, preparation method and applications thereof
  • ERI configuration phosphorous-aluminum molecular sieve membrane, preparation method and applications thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1: SAPO-17 seed crystal preparation

[0051] Mix the template agent cyclohexylamine (CHA), aluminum isopropoxide, phosphoric acid and an appropriate amount of ultrapure water evenly, stir vigorously at room temperature for 1 hour, and then add T-type molecular sieves (200 nm, Si / Al= 3.2) As a silicon source. The sol was stirred and aged for 1-12 hours, the formed Al 2 o 3 -P 2 o 5 -SiO 2 -CHA-H 2 The molar ratio of each component in the O stable sol system is: P 2 o 5 / Al 2 o 3 = 1.0, CHA / Al 2 o 3 = 1.0, SiO 2 / Al 2 o 3 =0.1,H 2 O / Al 2 o 3 =50; the above sol was poured into a polytetrafluoroethylene-lined stainless steel reactor, and then the reactor was placed in an oven at 200°C for crystallization for 24 hours. The reaction product was separated by centrifugation, washed and dried, and then placed in a muffle furnace at 470°C for 6 h to remove the template agent to obtain the SAPO-17 molecular sieve.

[0052] The samples were characteriz...

Embodiment 2

[0053] Embodiment 2: Preparation of SAPO-17 molecular sieve membrane

[0054] The preparation of SAPO-17 molecular sieve membrane, the steps are as follows:

[0055] (1) support body pretreatment: the support body adopts the tubular mullite produced by Japan Nikkato Co., Ltd. (the composition is 67wt.%Al 2 o 3 and 33wt.% SiO 2 ) carrier with an average pore diameter of 1.3 μm and a porosity of 43%. After the support body was smoothed with 1000-grit sandpaper, it was cleaned with ultrasonic waves in deionized water and dried. Evenly coat the ground SAPO-17 molecular sieve seeds on the outer surface of the support, and the seed crystal loading density is 0.5-2mg / cm 2 .

[0056] (2) Preparation of SAPO-17 molecular sieve membrane: Mix the template agent (SDA) cyclohexylamine, aluminum sec-butoxide, phosphoric acid and ultrapure water, stir and age for 12 hours to form a uniform and stable sol, each component in the sol system The molar ratio is: P 2 o 5 / Al 2 o 3 = 1.0,...

Embodiment 3

[0063] Embodiment 3: Preparation of SAPO-17 molecular sieve membrane

[0064] Synthesize SAPO-17 molecular sieve membrane according to the method substantially identical with embodiment 2, difference is template agent (SDA) is N,N,N,N-tetramethyl-1,6-hexamethylene diammonium, and sol proportion is each The molar ratio of the components is: P 2 o 5 / Al 2 o 3 = 1.0, SDA / Al 2 o 3 =0.8,H 2 O / Al 2 o 3 =500, the synthesis time is 100h.

[0065] The synthesized molecular sieve membrane M2 was used at 25°C, CO 2 / CH 4 (50 / 50) and CO 2 / N 2 The gas separation performance was characterized in the (50 / 50) system, and the results of the gas separation experiment are shown in Table 1.

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Abstract

The invention discloses an ERI configuration phosphorous-aluminum molecular sieve membrane having a high CO2 separation performance. The ERI configuration phosphorous-aluminum molecular sieve membrane comprises a porous support body and is characterized in that a membrane formed from a SAPO-17 or AlPO-17 zeolite molecular sieve crystal covers the surface of the porous support body. According to the preparation method, a nanometer T type molecular sieve is adopted as a crystalline state silicon source to induce the synthesis of the high-crystallinity submicron SAPO-17 molecular sieve crystal, and the compact ERI configuration AlPO-17 or SAPO-17 molecular sieve membrane is synthesized on the surface of the porous support body by adopting the crystal as the crystal seed through a secondary hydrothermal method, wherein the molecular sieve membrane has advantages of uniform crystal size, compact growth, uniform thickness, high crystallinity, complete coverage, and high carbon dioxide separation performance, and is suitable for the separation of the carbon dioxide gas from natural gas and flue gas.

Description

technical field [0001] The invention belongs to the technical field of inorganic membrane materials, and relates to a molecular sieve membrane, in particular to an ERI configuration aluminum phosphorus molecular sieve membrane and its preparation and application. Background technique [0002] As the main impurity gas in natural gas, carbon dioxide not only reduces the calorific value of natural gas, but also causes corrosion to gas transmission equipment and pipelines in the presence of water vapor, so it must be removed. For such a process involving a large volume of gas separation treatment, the common organic amine absorption and separation process has disadvantages such as high energy consumption and large reagent consumption. Using membrane technology to separate carbon dioxide from natural gas can significantly reduce the cost of natural gas purification. [0003] As early as the 1980s, developed countries in Europe and the United States developed CO 2 Selective cell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08B01D71/02B01D53/22
CPCB01D53/228B01D71/028C01B37/08C01B39/54Y02C20/40Y02P20/151
Inventor 周俊静李莎莎
Owner 南京方膜高科技有限公司
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