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Seed crystal-free self-assembly hydrothermal synthesis method of hydrophilic zeolite membrane

A zeolite membrane and hydrophilic technology, applied in the field of chemical separation, can solve the problems of high cost, high cost, low output, etc., and achieve the effects of easy repetition, modification of carrier pores, and smooth carrier surface.

Inactive Publication Date: 2013-07-10
北京鸿智嘉和科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cost of nanocrystals necessary for the preparation of thinner seed layers is inevitably high due to the low yield and the need for expensive templates in the preparation process (Science, 2011, 334, 767)

Method used

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  • Seed crystal-free self-assembly hydrothermal synthesis method of hydrophilic zeolite membrane
  • Seed crystal-free self-assembly hydrothermal synthesis method of hydrophilic zeolite membrane
  • Seed crystal-free self-assembly hydrothermal synthesis method of hydrophilic zeolite membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Hydrothermal preparation method of NaA zeolite membrane:

[0031] (1) Preparation of inorganic particle coating

[0032] α-Al after pretreatment by two-step thermal dipping 2 o3 Coating Continuous and Uniform Functionalized α-Al on Macroporous Support Tube 2 o 3 Particle coating: the pretreated α-Al 2 o 3 Both ends of the macroporous carrier tube are sealed with polytetrafluoroethylene plugs, heated in an oven at 150°C for 2 to 4 hours, and then quickly immersed in the dispersed large functionalized α-Al with a mass concentration of 3wt.%. 2 o 3 In the particle suspension I, after dipping for 20s, take it out at a constant speed, and dry it in an oven at 50°C for 3-6h, and then place it in an oven at 180°C for heating and curing for 3h. Large functionalized α-Al attached to the surface of the carrier tube with absorbent cotton 2 o 3 After the particle is wiped off, it is sealed with a Teflon stopper. After heating in an oven at 80°C for 3 hours, quickly immerse...

Embodiment 2

[0037] Microwave heating preparation method of T-type zeolite membrane:

[0038] (1) Preparation of inorganic particle coating

[0039] Same as Example 1, but replace α-Al with pretreated mullite carrier tube 2 o 3 carrier tube.

[0040] (2) T-type zeolite membrane microwave precrystallization

[0041] Weigh 2.683g of NaAlO 2 , 4.945g of NaOH and 3.205g of KOH were dissolved in 19.413g of deionized water. After stirring and clarification at room temperature, 64.841g of silica sol was added dropwise and vigorously stirred at 40°C for 12h. The molar composition was Al 2 o 3 :SiO2 2 :Na 2 O:K 2 O:H 2 O=1:25:6.5:2.25:350. Then, pour the synthesis liquid into the container coated with functionalized α-Al 2 o 3 Microwave crystallization at 100°C for 8h in the microwave reactor of the particle carrier tube. After the reaction is complete, cool to room temperature, take out the membrane tube, wipe off excess T-type zeolite crystals on the surface of the membrane tube, was...

Embodiment 3

[0046] The pervaporation performance test of the synthesized NaA zeolite membrane and T-type zeolite membrane was carried out using a pervaporation device to characterize the separation performance of the NaA zeolite membrane and T-type zeolite membrane. The composition of the feed liquid is 90wt.% ethanol / water mixed liquid, the temperature is kept at 70°C, and the product on the permeate side is collected with a cold trap. In the experiment, a vacuum pump was used to evacuate the inside of the membrane tube and keep the vacuum at 100-200Pa. Analyze the composition of the permeate product by gas chromatography, calculate the separation coefficient of the zeolite membrane, and calculate the flux of the zeolite membrane by weighing the mass before and after the cold trap. In this experiment, it was measured that the flux of the prepared NaA zeolite membrane was 3.42kg / m 2 h, separation factor > 10000, flux of T-type zeolite membrane is 1.33kg / m 2 h, the separation factor is 2...

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Abstract

The invention discloses a seed crystal-free self-assembly hydrothermal synthesis method of a hydrophilic zeolite membrane. The method comprises the steps of coating inorganic particles which are chemically modified by a silane coupling agent on the surface of a macropore support, putting the pre-processed macropore support into crystallized synthetic fluid under the condition of not using the seed crystal, and directly preparing the continuous, compact and ultra-thin hydrophilic zeolite membrane by hydrothermal synthesis. A layer of functionalized inorganic particle which is chemically modified by the silane coupling agent is coated on the macropore support; the functionalized inorganic particle plays the roles of modifying support ducts and smoothing the support surface, also plays the role of improving the zeolite heterogeneous nucleation point, overcomes two problems that the membrane is not easily formed on the macropore support, and the high-performance zeolite membrane is difficultly prepared if seed crystal synthesis is not used, and can obtain the hydrophilic zeolite membrane with an excellent performance by one-time hydro-thermal synthesis.

Description

technical field [0001] The invention belongs to the technical field of chemical separation, and relates to a method for preparing a hydrophilic zeolite membrane, in particular to a method for self-assembling a dense and continuous hydrophilic zeolite molecular sieve membrane on a macroporous carrier without crystal seeds. Background technique [0002] Zeolite molecular sieve membrane material is a kind of aluminosilicate crystal with regular microporous structure. It has the advantages of excellent thermal stability, mechanical stability, microbial erosion resistance and oxidation resistance inherent in inorganic membrane materials, and is more unique. What is remarkable is its uniform and regular crystalline channel system and its adjustable surface properties. These excellent properties endow zeolite molecular sieve membranes with incomparable uniqueness of organic membranes: high selectivity, high flux, solvent resistance, high temperature resistance, zeolite molecular si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D71/02
Inventor 杨建华王金渠李华征王作荣罗益韦许静孟祥娣鲁金明殷德宏张艳
Owner 北京鸿智嘉和科技有限公司
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