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Organic silicon micro-pore zeolite and synthesizing method thereof

A technology of microporous zeolite and synthesis method, applied in crystalline aluminosilicate zeolite, chemical instruments and methods, inorganic chemistry, etc., to achieve the effect of good technical effect

Active Publication Date: 2008-02-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The framework structure of the above-mentioned crystalline zeolite is all based on inorganic silica and inorganic alumina as basic elements, and the zeolite containing organic silicon in the framework structure and its synthetic method have not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 4.3 grams of aluminum nitrate in 540 grams of water, add 24.0 grams of sodium hydroxide to dissolve it, then add 66.5 grams of tetrapropylammonium bromide while stirring, then add 60.0 grams of solid silicon oxide, dimethyl dichloride Silane 2.6 grams, the material proportion (mol ratio) of reactant is:

[0024] SiO 2 / Al 2 O 3 =100

[0025] NaOH / SiO 2 =0.6

[0026] Dimethyldichlorosilane / SiO 2 =0.02,

[0027] Tetrapropylammonium bromide / SiO 2 =0.25

[0028] h 2 O / SiO 2 =30

[0029] After the reaction mixture was evenly stirred, it was put into a stainless steel reaction kettle, and crystallized at 185° C. for 60 hours while stirring. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / A1 2 O 3 The molar ratio was 95.5.

[0030] After drying the sample was determined, its Si 29The NMR solid-state nuclear magnetic spectrum peak appears at -18.5ppm. Its X-ray diffraction data are shown in Table 1.

[00...

Embodiment 2

[0034] Sodium aluminate (Al 2 o 3 42.0% by weight) 6.1 g was dissolved in 720 g of water, 1.6 g of sodium hydroxide was added to dissolve it, then 46.4 g of hexamethylenediamine was added while stirring, and then 60 grams of silicon oxide, 3.9 grams of hexamethylene diamine, trimethyl 2.2 grams of chlorosilanes, the material ratio (mol ratio) of reactant is:

[0035] SiO 2 / Al 2 o 3 =40

[0036] NaOH / SiO 2 =0.4

[0037] Chlorotrimethylsilane / SiO 2 =0.02,

[0038] Hexamethylenediamine / SiO 2 =0.40

[0039] h 2 O / SiO 2 =40

[0040] After the reaction mixture was stirred evenly, it was put into a stainless steel reaction kettle, and crystallized at 150° C. for 55 hours while stirring. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 41.

[0041] After drying the sample was determined, its Si 29 The NMR solid-state nuclear magnetic spectrum peak appears at 15.9ppm. Its X-ray diffraction da...

Embodiment 3

[0045] Dissolve 1.2 grams of aluminum sulfate in 450 grams of water, add 12.0 grams of sodium hydroxide to dissolve it, then add 79.8 grams of tetrapropylammonium bromide while stirring, then add 150 grams of silica sol (40% by weight of silicon oxide content) ), dimethyldiethoxysilane 5.9 grams, the material ratio (mol ratio) of reactant is:

[0046] SiO 2 / Al 2 o 3 =300

[0047] NaOH / SiO 2 =0.3

[0048] Dimethyldiethoxysilane / SiO 2 =0.04,

[0049] Tetrapropylammonium bromide / SiO 2 =0.30

[0050] h 2 O / SiO 2 =30

[0051] After the reaction mixture was stirred evenly, it was put into a stainless steel reaction kettle, and crystallized at 145° C. for 70 hours while stirring. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 281.3.

[0052] After drying the sample was determined, its Si 29 The NMR solid-state nuclear magnetic spectrum peak appears at -19.7ppm. Its X-ray diffraction data ar...

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Abstract

The present invention relates to a silicone microporous zeolite and the synthesis method of the silicone microporous zeolite, used to solve the problem that a frame structure of the microporous zeolite synthesized by the prior technology does not contain the silicone and to provide the microporous zeolite, in which the frame structure contains the silicone. The present invention contains the following mol relation: In the formula of (1 / n) Al2O3: SiO2: (m / n) R, n is equal to 5-1000 and m is equal to 0.01-300. R is an alkyl, an alkane alkenyl or a phenyl. A solid nuclear magnetic map of Si29NMR is between -80ppm and +50ppm and includes at least one nuclear magnetic resonance spectral peak of Si29. A diffraction pattern of x-ray has a d-spacing maximum at the position of 11.14 plus or minus 0.05, 9.99 plus or minus 0.05, 9.74 plus or minus 0.05, 6.36 plus or minus 0.05, 5.99 plus or minus 0.05, 5.70 plus or minus 0.05, 5.57 plus or minus 0.05, 4.98 plus or minus 0.05, 4.26 plus or minus 0.05, 3.83 plus or minus 0.05, 3.75 plus or minus 0.05, 3.72 plus or minus 0.05, 3.65 plus or minus 0.05, 3.44 plus or minus 0.05, 3.32 plus or minus 0.05 angstrom and 3.05 plus or minus 0.05 angstrom. The microporous zeolite can serve as a sorbent or an activator component used in the transformation of the organic compounds.

Description

technical field [0001] The invention relates to an organosilicon microporous zeolite and a synthesis method thereof. Background technique [0002] In industry, porous inorganic materials are widely used as catalysts and catalyst supports. Porous materials have relatively high specific surface area and smooth pore structure, so they are good catalytic materials or catalyst supports. Porous materials generally include: amorphous porous materials, crystalline molecular sieves, and modified layered substances. [0003] The basic framework structure of crystalline microporous zeolites is based on the rigid three-dimensional TO 4 (SiO 4 , A1O 4 etc.) unit structure; in this structure TO 4 Oxygen atoms are shared in a tetrahedral manner, and the skeleton tetrahedron is like A1O 4 The charge balance of is through surface cations such as Na + , H + existence is maintained. It can be seen that the framework properties of zeolite can be changed by cation exchange. At the same...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02C01B39/46B01J29/04B01J20/18
Inventor 高焕新魏一伦周斌方华顾瑞芳季树芳
Owner CHINA PETROLEUM & CHEM CORP
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