Micro-pore zeolite, preparation method and application thereof

A technology of microporous zeolite and zeolite, applied in chemical instruments and methods, other chemical processes, inorganic chemistry, etc., to achieve good technical effects

Active Publication Date: 2008-08-13
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 basi

Method used

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  • Micro-pore zeolite, preparation method and application thereof
  • Micro-pore zeolite, preparation method and application thereof
  • Micro-pore zeolite, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0022] [Example 1]

[0023] Sodium aluminate (containing 42.0 wt% Al 2 O 3 ) 6.1 grams and 2.0 grams of sodium hydroxide are dissolved in 270 grams of water, then 34.7 grams of hexamethyleneimine are added while stirring, and then 150 grams of silica sol (containing 40% by weight SiO 2 ), 6.5 grams of dimethyldichlorosilane, the material ratio (molar ratio) of the reactant is:

[0024] SiO 2 / Al 2 O 3 = 40

[0025] NaOH / SiO 2 =0.05

[0026] Dimethyldichlorosilane / SiO 2 =0.05

[0027] Hexamethyleneimine / SiO 2 = 0.35

[0028] H 2 O / SiO 2 = 20

[0029] After the reaction mixture is uniformly stirred, it is put into a stainless steel reactor and crystallized at 150°C for 55 hours under stirring. After being taken out, it is filtered, washed and dried. SiO is obtained by chemical analysis 2 / Al 2 O 3 The molar ratio is 42.3.

[0030]The dried sample is determined, its Si 29 The NMR solid-state nuclear magnetic spectrum showed a nuclear magnetic resonance peak at -18.4 ppm. The X-ray di...

Example Embodiment

[0033] [Example 2]

[0034] Sodium aluminate (containing 42.0 wt% Al 2 O 3 ) 6.1 grams and 2.0 grams of sodium hydroxide are dissolved in 180 grams of water, then 6.6 grams of trimethylchlorosilane and 43.0 grams of hexahydropyridine are added while stirring, and then 150 grams of silica sol (containing 40% by weight SiO 2 ), the material ratio (molar ratio) of the reactant is:

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

[0036] NaOH / SiO 2 =0.05

[0037] Trimethylchlorosilane / SiO 2 =0.06

[0038] Hexahydropyridine / SiO 2 = 0.50

[0039] H 2 O / SiO 2 = 15

[0040] After the reaction mixture is uniformly stirred, it is put into a stainless steel reactor and crystallized at 152°C for 50 hours under stirring. After being taken out, it is filtered, washed and dried. SiO is obtained by chemical analysis 2 / Al 2 O 3 The molar ratio is 42.1.

[0041] The dried sample is determined, its Si 29 The NMR solid-state nuclear magnetic spectrum showed a nuclear magnetic resonance peak at 15.2 ppm. The X-ray dif...

Example Embodiment

[0044] [Example 3]

[0045] Dissolve 5.1 g of alumina and 2.0 g of sodium hydroxide in 540 g of water, then add 42.5 g of hexamethyleneimine under stirring, then add 60 g of solid silica and 3.2 g of hexamethyldisilazane , The material ratio (molar ratio) of the reactant is:

[0046] SiO 2 / Al 2 O 3 = 20

[0047] NaOH / SiO 2 =0.05

[0048] Hexamethyldisilazane / SiO 2 = 0.04

[0049] Hexamethyleneimine / SiO 2 =0.5

[0050] H 2 O / SiO 2 = 30

[0051] After the reaction mixture is uniformly stirred, it is put into a stainless steel reactor and crystallized at 163°C for 50 hours under stirring. After being taken out, it is filtered, washed and dried. SiO is obtained by chemical analysis 2 / Al 2 O 3 The molar ratio is 17.7.

[0052] The dried sample is determined, its Si 29 The NMR solid-state nuclear magnetic spectrum showed a nuclear magnetic resonance peak at 15.8 ppm. The X-ray diffraction data are shown in Table 3.

[0053] table 3

[0054]

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Abstract

The present invention provides an organosilicone porous zeolite, synthetic method and its application, mainly resolves the problem of organosilicone-free in the porous zeolite structure by the present technology, provides a porous zeolite containing organosilicone in structure. It includes constitute of following mol relation: (1/n)Al2O3:SiO2:(m/n)R, n=10-350, m=0.02-50, R is at least one of alkyl, alkanes and alkenes or phenyl; wherein Si29NMR between -80-+50ppm containing at least a Si29 NMR peak, X-ray diffraction pattern computer has d-distance max in 13.2+/-0.2, 12.3+/-0.1, 10.9+/-0.3, 9.1+/-0.3, 6.8+/-0.2, 6.1+/-0.2, 5.6+/-0.2, 4.4+/-0.3, 4.0+/-0.3, 3.6+/-0.2, 3.4+/-0.1 and 3.3+/-0.2. The porous zeolite may catalyst component or absorption agent for organic compound conversion.

Description

technical field [0001] The invention relates to a microporous zeolite, a preparation method and application 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 , AlO 4 etc.) unit structure; in this structure TO 4 Oxygen atoms are shared in a tetrahedral manner, and the skeleton tetrahedron such as AlO 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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IPC IPC(8): C01B39/46B01J20/18B01J29/04
Inventor 魏一伦高焕新周斌方华顾瑞芳季树芳
Owner CHINA PETROLEUM & CHEM CORP
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