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The preparation method of sapo-34 molecular sieve membrane

A technology of SAPO-34 and molecular sieves, which is applied in the field of preparation of SAPO-34 molecular sieve membranes, can solve the problems of low density of molecular sieve membranes, many defects of molecular sieve membranes, unfavorable gas mixture separation, etc., and achieve good compactness, good continuity, The effect of less defects

Active Publication Date: 2020-10-16
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the preparation method of the above-mentioned molecular sieve membrane, the silicon source is used directly, the crystal grains are uneven, the particles are large, and the formed molecular sieve membrane has many defects, which is not conducive to the separation of mixed gases; the in-situ generation method and the secondary growth method Molecular sieves are nucleated and grown through a hydrothermal system, so the shape of the particles and the density of the crystal nuclei on the carrier cannot be controlled, which makes the film on the carrier uneven. In addition, due to the large amount of synthetic liquid used, the preparation cost is high and waste liquid The in-situ generation method does not use seed crystals, resulting in low compactness of molecular sieve membranes; the research on molecular sieve membranes mainly focuses on silicon-aluminum oxide materials, and there are few studies on silicon-phosphorus-aluminum molecular sieve membranes. There is still a big gap between the cost and separation effect and the requirements of industrial applications, and further research is needed to solve the problem

Method used

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  • The preparation method of sapo-34 molecular sieve membrane
  • The preparation method of sapo-34 molecular sieve membrane
  • The preparation method of sapo-34 molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 12.3g of aluminum isopropoxide and mix it in deionized water, add 11.97g of phosphoric acid while stirring, stir vigorously for 3-4 hours to completely hydrolyze and obtain a white milky homogeneous solution. Then add 6g of silica sol after reflux treatment in alkali solution, stir at room temperature for 0.5h, then add 60g of template agent R1, and stir for 2h. After sealing the two ends of the pretreated carrier tube, put it vertically into the above mixed solution, pull it several times, dry it at room temperature and place it on the upper part of a stainless steel reaction kettle with a polytetrafluoroethylene liner, add water to the bottom of the reaction kettle , After sealing, it was statically crystallized under its own pressure for 24h. After the crystallization is completed, the carrier is taken out, and then repeatedly washed with deionized water for several times until the value of the solution is neutral, then dried and calcined to obtain a SAPO-34 mo...

Embodiment 2～14

[0029] According to the various steps and conditions of [Example 1], the SAPO-34 molecular sieve membrane was prepared, but the parameters such as raw materials, raw material ratio, template type, crystallization temperature, etc. were changed, which are specifically listed in Table 1. The synthesized product has been characterized to have a crystal structure similar to that of [Example 1] and the product.

[0030] Table 1

[0031]

Embodiment 15

[0032] [Example 15] Preparation of molecular sieve membrane by traditional method

[0033]Weigh 12.3g of aluminum isopropoxide, 11.97g of phosphoric acid, 6g of silica sol, and 60g of template agent R1, mix them, and stir for 3 hours to form a mixed solution A. After sealing the two ends of the carrier tube coated with the seed crystal, put it vertically into a stainless steel reaction kettle with a polytetrafluoroethylene liner, then pour the mixed solution A into it, and after the stainless steel reaction kettle is sealed, the crystallization is still under its own pressure. 24h. After the crystallization is completed, the carrier is taken out, and then washed several times with deionized water until the value of the solution is neutral, then dried and calcined to obtain the SAPO-34 molecular sieve membrane prepared by the traditional method. The weight ratio of each component is: SiO 2 / Al 2 o 3 =0.4;P 2 o 5 / Al 2 o 3 = 1.1; H 2 O / Al 2 o 3 =7; R1 / Al 2 o 3 =10 ...

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Abstract

The invention relates to a preparation method for a SAPO-34 molecular-sieve membrane to overcome technical problems in preparation of SAPO-34 molecular-sieve membranes in the prior art. The preparation method comprises the following steps: subjecting a silicon source in coating liquid to alkali treatment at first; then coating a carrier with the silicon-aluminum-phosphorus oxide precursor coatingliquid; and carrying out gas-phase in-situ crystallization to prepare the SAPO-34 molecular-sieve membrane. The preparation method is simple to operate; the prepared SAPO-34 molecular-sieve membrane has good reproducibility, high quality and low preparation cost; and the method is beneficial for cyclic utilization of templates and can be applied to industrial production of molecular-sieve membranes.

Description

technical field [0001] The invention relates to a preparation method of SAPO-34 molecular sieve membrane. Background technique [0002] Membrane separation technology is a new separation, purification and purification technology, which has been widely used in food, beverage, metallurgy, papermaking, textile, pharmaceutical, automobile, biological and chemical industries. According to different membrane materials, it can be divided into inorganic membrane and organic membrane. Compared with organic membrane, inorganic membrane has excellent chemical stability, thermal stability and mechanical strength. Molecular sieve membrane, as a representative type of inorganic membrane, has a certain shape and controllable structure of pores, adjustable pore size and uniform distribution, and the pore size is similar to the molecular size. Due to the specific pore structure of the molecular sieve membrane, it has selective permeability and shape-selective catalysis, and the molecular si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54
CPCC01B39/54C01P2002/72C01P2004/03
Inventor 杨贺勤刘志成高焕新
Owner CHINA PETROLEUM & CHEM CORP