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Preparation method for ZSM-5 molecular sieve membrane with high hydrophobicity

A ZSM-5 and molecular sieve technology, which is applied in the field of preparation of high-performance hydrophobic ZSM-5 molecular sieve membranes, can solve problems such as molecular sieve membrane cracks and molecular sieve membrane separation performance degradation, and achieve reduced production costs and improved pervaporation separation performance , Highly complete effect

Inactive Publication Date: 2012-09-05
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the different thermal expansion coefficients between the carrier and the ZSM-5 molecular sieve, it is easy to cause cracks in the molecular sieve membrane during the process of removing the template agent, which eventually leads to a decrease in the separation performance of the molecular sieve membrane.

Method used

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  • Preparation method for ZSM-5 molecular sieve membrane with high hydrophobicity
  • Preparation method for ZSM-5 molecular sieve membrane with high hydrophobicity
  • Preparation method for ZSM-5 molecular sieve membrane with high hydrophobicity

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preparation example Construction

[0027] It is an existing technology to prepare a pure silicon ZSM-5 molecular sieve crystal layer on a macroporous carrier. The high-speed spin coating method and the low-speed pulling method of the prior art are respectively used to prepare a layer of tightly covered molecular sieve seed crystals on the macroporous carrier. layer. The specific preparation method is as follows: ① When coating the seed layer, molecular sieve particle colloid is used, the particle size is 400-500nm, the colloid concentration is 0.2-1.0wt.%, and an appropriate amount of PVA is added as a binder at the same time; The carrier coated with the seed layer was placed in a programmable muffle furnace and calcined in an air atmosphere to remove PVA and organic templates. The maximum calcining temperature was 450°C, and the heating and cooling rates were both 1°C / min. The calcined molecular sieve seed layer can be directly used in the subsequent hydrothermal synthesis, but calcining is not a necessary ste...

Embodiment 1

[0030] (1) Adopt the high-speed spin-coating method of prior art, first with deionized water, the suspension liquid of nano-sized molecular sieve small particles is diluted to 0.2~0.5wt% seed liquid, then the seed liquid is quickly added dropwise to α -Al 2 o 3 On the carrier, rotate at a high speed for 30 seconds, and finally dry in an oven at 60°C for 12 hours to obtain a denser molecular sieve seed layer. Such as figure 1 As shown in A, by spin-coating molecular sieve seed liquid, the α-Al 2 o 3 The surface of the carrier is tightly covered with a layer of seed layer with a thickness of about 1.5 μm ( figure 1 B).

[0031] (2) Preparation of pure silicon ZSM-5 molecular sieve membrane

[0032] According to 1TEOS: 0.2TPAOH: 850H 2 The molar ratio of O was used to configure the synthesis solution, and the alumina carrier coated with the seed crystal was placed in an autoclave with a Teflon liner, and the synthesis solution was poured into the alumina carrier to cover; ...

Embodiment 2

[0040] (1) Preparation of Fe-ZSM-5 molecular sieve seed layer on flake alumina carrier

[0041] Nanoscale Fe-ZSM-5 molecular sieve particles were used to configure the seed liquid, and the specific method was the same as that in Example 1. The molecular sieve seed layer was calcined at 450° C. for 8 hours, and then used for the subsequent secondary growth.

[0042] (2) Preparation of Fe-ZSM-5 molecular sieve membrane

[0043] According to 1TEOS: 0.2TPAOH: 0.005Fe(NO 3 ) 3 : 750H 2 The molar ratio of O configures the synthesis solution.

[0044] Containing Fe 3+ After hydrothermal crystallization at 150°C for 4 hours, the molecular sieve seeds are well cross-linked to form a hOh-oriented ZSM-5 molecular sieve film layer with a thickness of about 1.5 μm ( image 3 A&B). From the SEM photos, it can be seen that the ZSM-5 molecular sieve membrane after one synthesis has been fully cross-linked, and there is almost no growth in the direction perpendicular to the support (out...

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Abstract

The invention relates to a preparation method for ZSM-5 molecular sieve membrane with high hydrophobicity, which comprises the following steps: (1) preparing a compact molecular sieve seed crystal layer; (2) putting a porous support with the molecular sieve seed crystal layer into a high pressure crystallized kettle, adding synthetic solutions, carrying out at least twice hydrothermal synthesis to promote full crosslinking growth between the molecular sieve seed crystals so as to finally form a complete molecular sieve membrane with orientation; and (3) adopting self catalysis property of heteroatom-containing ZSM-5 molecular sieve, adopting a hydrogenation deep catalytic cracking process to remove organic templates in the molecular sieve membrane under the lower temperature. The invention can effectively avoid the formation of intercrystalline defects of the molecular sieve membrane, also enables the cracked organic templates to form a single-walled carbon nano tube in the pore canal of the molecular sieve membrane, increases the hydrophobicity of the molecular sieve membrane, has mild process condition, simpler operation, lower cost and wide applicability, is not only suitable for planning production of the molecular sieve membrane, but also is benefit for the industrialization of the membrane separation technique with lower energy consumption of organic matter aqueous solution with low concentration.

Description

technical field [0001] The invention relates to a preparation method of a high-performance hydrophobic ZSM-5 molecular sieve membrane, belonging to the technical field of inorganic membrane materials and membrane separation. technical background [0002] Molecular sieve membrane is a new type of inorganic membrane material developed in recent years. It has excellent molecular sieving and shape-selective catalytic properties, and is widely used in membrane separation and membrane reaction processes. Compared with other membrane materials, molecular sieve membrane has the following advantages: 1) molecular sieve membrane has a regular pore structure and uniform pore size distribution, and many important industrial raw materials can be adsorbed and separated by molecular sieve or shape-selective diffusion; 2) molecular sieve membrane has a good Thermal stability, chemical stability, biological stability and mechanical stability. Compared with organic membranes, it has higher p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/02C01B39/40
Inventor 郎林阴秀丽吴创之
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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