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A kind of preparation method of chabazite and chabazite membrane

A technology of chabazite and zeolite, which is applied in the field of preparation of chabazite and chabazite membrane, to achieve the effects of high pervaporation performance, good separation performance and good stability

Active Publication Date: 2011-12-21
JIANGXI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Summarizing the existing literature on the synthesis of chabazite and its membranes, at present, the method of adding organic templates is basically used to synthesize chabazite, and the synthesis of chabazite and chabazite polycrystalline membranes without adding templates has not been reported.

Method used

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  • A kind of preparation method of chabazite and chabazite membrane
  • A kind of preparation method of chabazite and chabazite membrane
  • A kind of preparation method of chabazite and chabazite membrane

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Embodiment 1

[0025] Example 1: Synthesis of chabazite crystals, using silica sol as the silicon source, sodium metaaluminate or aluminum hydroxide as the aluminum source, potassium hydroxide and sodium hydroxide as the alkali raw materials, and preparing the raw material liquid SiO 2 -Al 2 O 3 -K 2 O-Na 2 O-H 2 O system, the molar ratio of each component is: SiO 2 / Al 2 O 3 = 20, H 2 O / SiO 2 = 14, Na + / K + = 0.33, OH- / SiO 2 =0.85; After aging the prepared raw material solution at 50°C for 12 hours, add 0.2wt% nano T-type zeolite seed crystals (prepared as in Example 1), pour it into a stainless steel reactor, and hydrothermally synthesize at 120°C for 30 hours; After completion, it was boiled with deionized water at 100°C to wash off the surface lye, filtered with suction, washed to pH 7, and dried at 100°C for 12 hours to obtain a white solid powder.

[0026] The support body before synthesis and the membrane tube after synthesis were characterized by XRD with ADVANCE D-8 X-ray diffractometer...

Embodiment 2

[0028] Example 2: The synthesis and preparation process of chabazite crystals is the same as in Example 1, except that the sol H 2 O / SiO 2 Increase to 16, crystallize at 160°C for 10 hours, the crystal is chabazite, the crystal size is 4-6μm.

Embodiment 3

[0029] Example 3: Synthesis of Chabazite Membrane A porous mullite tube manufactured by Nikkato Co., Ltd. was used as a support for membrane synthesis, and the mullite composition was 67wt% Al 2 O 3 And 33wt% SiO 2 . The support body is pre-treated with 800 mesh sandpaper and ultrasonic cleaning, and then air-dried. A layer of chabazite powder (prepared in Example 1) is coated on the outer surface of the support body. The seed crystal loading density is 0.5-2mg / cm 3 , The support with pre-coated seed crystals is dried at 60°C for use.

[0030] Using aluminum hydroxide as the aluminum source and silicon powder as the silicon source, it is added to the mixed alkali solution of sodium hydroxide and potassium hydroxide, accompanied by heating and stirring. The ratio of the sol according to the molar ratio of oxides is: SiO 2 / Al 2 O 3 =15, OH- / SiO 2 = 0.9, Na + / K + = 0.8, H 2 O / SiO 2 = 30. After aging at 45℃ for 24 hours, the sol is poured into the reactor, and the support for pre-co...

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Abstract

The invention provides a method for preparing chabazite and a chabazite film in the absence of a template agent. Pure chabazite is formed through induction of out-of-phase crystal nucleus T-shaped zeolite under the condition of not adding an organic template agent. The chabazite molecular sieve film is formed through induction by loading formed chabazite on the outer surface of a porous support as a crystal seed. The method is characterized in that: silicon powder and sodium metaaluminate are used as a silicon source and an aluminum source; based on the molar ratio of oxides, the ratios of components which are prepared into sol are that: the molar ratio of SiO2 to Al2O3 is equal to 15-30, the molar ratio of OH<-> to SiO2 is equal to 0.9-1.5, the molar ratio of Na<+> to K<+> is equal to 0.1-1, and the molar ratio of H2O to SiO2 is equal to 18-40; the sol for coating the crystal seed is subjected to hydrothermal synthesis at the temperature of 100-160 DEG C for 16-72 hours; and a compact chabazite film is synthesized on a porous carrier. Through the method for preparing the chabazite and the chabazite film, the expensive organic template agent is prevented from being added, the synthesis process is simple, and the repeatability is high. The synthesized film shows better stability in an inspection acid medium and can be widely applied to a pervaporation separation process and a pervaporation film reactor of an acidic system.

Description

Technical field [0001] The invention provides a method for preparing chabazite and a chabazite membrane under the condition of no template agent, and belongs to the field of preparation and application of inorganic porous materials. Background technique [0002] Chabazite has a three-dimensional eight-membered ring pore system along crystallographic a-axis, b-axis and c-axis, and the diameter of the eight-membered ring pore is 0.38nm×0.38nm. Its structure contains cage columns (parallel to the c direction) composed of alternate D6R and CHA cages. The cage is large enough to contain the aromatic intermediates, while still allowing reactants and products to enter and exit the crystal's diffusion input and output through regularly interconnected window pores. It also maintains its own morphological characteristics under appropriate acid strength, and is widely used as a catalyst and adsorbent. The dense chabazite crystal layer (chabazite membrane) formed on the porous substrate w...

Claims

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Application Information

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IPC IPC(8): C01B39/02
Inventor 陈祥树周荣飞胡娜刘星生张乔
Owner JIANGXI NORMAL UNIVERSITY