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Method for solid-phase synthesis of molecular sieves

A solid-phase synthesis, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc. The effect of reducing consumption, reducing the cost of reactants, and improving efficiency

Inactive Publication Date: 2016-03-30
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses traditional ammonium salts to provide a source of alkalinity (ie OH - group as a mineralizer) molecular sieve structure still has limitations; and in the traditional hydrothermal gel synthesis of ITQ-13 and F-ZSM-5 zeolite molecular sieves under alkaline conditions, brominated organic templates The agent needs to use silver oxide or ion exchange column to convert it into a hydroxide organic template agent, which increases the reaction cost; the hydrolysis process of silicon source and aluminum source in alkaline solution takes a long time, has low efficiency and high energy consumption; the amount of water cannot be accurately control, so it is very easy to obtain mixed products; at the same time, because it is necessary to add hydrofluoric acid to introduce fluorine ion mineralizers, it also brings harm to the health of experimenters, so a suitable way to reduce costs, improve efficiency and be safer is sought. Synthetic methods are necessary

Method used

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  • Method for solid-phase synthesis of molecular sieves
  • Method for solid-phase synthesis of molecular sieves
  • Method for solid-phase synthesis of molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1: ITQ-13 molecular sieve with pure silicon phase was synthesized in solid phase with hexamethyldiammonium bromide as a directing agent in a solvent-free method.

[0042] After mixing 0.54g of water with 1.22g of sodium metasilicate, recrystallize to form sodium metasilicate containing three crystal waters; Mix hexamethyldiammonium bromide and 0.59g ammonium fluoride in an agate mortar and grind for 5-10 minutes until the mixture is uniform, then put the ground mixture into a glass tube and seal it with flame; finally After the sealed glass tube was crystallized in an oven at 180°C for 4 weeks, the reaction product was washed and placed in an oven at 60°C for 12 hours to completely dry to finally obtain the product.

[0043] The proportioning of reaction raw material is as follows:

[0044] 1.0Na 2 SiO 3 ·3H 2 O:1.0SiO 2 (Silica): 0.15HMBr 2 : 1.6NH 4 f

[0045] X-ray diffraction ( figure 1 ) analysis of its structure as ITQ-13 zeolite molecular sieve, ...

Embodiment 2

[0046] Embodiment 2: Tetrapropylammonium bromide is the F-ZSM-5 molecular sieve of pure silicon phase synthesized by solid phase method without solvent as the guiding agent.

[0047] After mixing 0.54g of water with 1.22g of anhydrous sodium metasilicate, recrystallize to form sodium metasilicate containing three crystal waters; then mix 1.76g of trihydrate sodium metasilicate with 0.56g of white carbon black at room temperature, Mix 0.53g tetrapropylammonium bromide and 0.59g ammonium fluoride and place in an agate mortar, grind for 5-10 minutes until the mixture is uniform, then put the ground mixture into a glass tube and seal it with flame; Finally, the sealed glass tube was crystallized in an oven at 180° C. for 4 weeks, and the reaction product was washed and placed in an oven at 60° C. for 11 hours until it was completely dried to finally obtain the product.

[0048] The proportioning of reaction raw material is as follows:

[0049] 1.0Na 2 SiO 3 ·3H 2 O:1.0SiO 2 (...

Embodiment 3

[0051] Embodiment 3: Tetraethylammonium bromide is the F-ZSM-5 molecular sieve of pure silicon phase solid-phase synthesis as the directing agent solvent-free method

[0052] After mixing 1.08g of water with 1.22g of anhydrous sodium metasilicate, recrystallize to form sodium metasilicate containing six crystal waters; then mix 2.30g of hexahydrate sodium metasilicate with 0.56g of white carbon black at room temperature, Mix 0.88g of tetraethylammonium bromide and 0.59g of ammonium fluoride and place in an agate mortar, grind for 5-10 minutes until the mixture is uniform, then put the ground mixture into a glass tube and seal it with flame; Finally, place the sealed glass tube in an oven at 180°C for crystallization for 4 weeks, wash the reaction product, and place it in an oven at 60°C for about 10 hours to completely dry to finally obtain the product. The proportioning of reaction raw material is as follows:

[0053] 1.0Na 2 SiO 3 ·6H 2 O:1.0SiO 2 (Silica): 0.60TEABr: 1...

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Abstract

The invention discloses a method of synthesizing a molecular sieve by using a solid phase. In the method, ammonium fluoride is used as a mineralizing agent and a brominized organic template is used as a guiding agent; and the method comprises the following steps: mixing a certain amount of water with anhydrous sodium metasilicate and recrystallizing to form crystal water-containing sodium metasilicate; then, mixing and grinding the certain amount of crystal water-containing sodium metasilicate, white carbon black, the brominized organic template, ammonium fluoride and / or aluminum nitrate together till mixing uniformly, then putting the ground mixture into a glass tube and sealing with flame; and crystallizing the sealed glass tube in an oven at 180 DEG for 4 weeks, washing the reaction products and drying the reaction products in an oven with the temperature of 60 DEG C till the reaction products are completely dried. By using ammonium fluoride as the mineralizing agent, an ITO (Indium tin oxide)-13 molecular sieve which cannot be obtained in an alkaline synthesis route and an F-ZSM (Zeolite Socony Mobil)-5 zeolite molecular sieve are obtained, and good degree of crystallinity and purity are kept. The reactant cost is lowered, the energy consumption is reduced and the product purity is high.

Description

technical field [0001] The invention relates to a method for preparing molecular sieves, in particular to a 4 F. Solid-phase synthesis of ITQ-13 and ZSM-5 molecular sieves as mineralizers. Background technique [0002] Zeolite molecular sieves are widely used in petrochemical adsorption, separation and various catalytic processes due to their large specific surface area, high hydrothermal stability, adjustable surface acidity and alkalinity, and pore selectivity. The synthesis and catalytic application of zeolite molecular sieves have always been a hot spot in industrial applications and academic research. Among them, ITQ-13 (T.Boix, M.Puche, M.A.Camblor, A.Corma, US Patent 6471941B1, 2002) molecular sieve is a synthetic porous crystal material with a three-dimensional channel system, and has an ITH topology. This structure includes the first A group of usually parallel channels, each of which consists of ten-membered rings of tetrahedrally coordinated atoms, and a second ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40C01B39/04
Inventor 刘文涛丁丽红何素芹朱诚身刘浩
Owner ZHENGZHOU UNIV
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