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Method for preparing MCM-22 molecular sieves

A technology of MCM-22 and molecular sieve, applied in the field of preparation of MCM-22 molecular sieve, can solve the problems of high cost and environmental pollution of nitrogen-containing organic matter, and achieve the effect of reducing synthesis cost and eliminating pollution

Inactive Publication Date: 2004-06-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is to provide a new method for preparing MCM-22 molecular sieves in order to overcome the high cost of preparing MCM-22 molecular sieves in the previous literature and the environmental pollution caused by nitrogen-containing organics in the crystallization mother liquor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Sodium aluminate (Al 2 o 3 35.21 wt%, Na 2 O31.12% by weight) 14.5 grams are dissolved in 990 grams of water, add 6.18 grams of sodium hydroxide and make it dissolve, then add organic amine template agent hexamethylene imine 49.5 grams under the situation of stirring, add silica sol (SiO 2 40% by weight) 150 grams, after being stirred evenly, the material proportion (mol ratio) of reactant is:

[0026] SiO 2 / Al 2 o 3 =20

[0027] Oh - / SiO 2 =0.3

[0028] R / SiO 2 =0.5

[0029] h 2 O / SiO 2 =60

[0030] After stirring for 30 minutes, put it into a stainless steel reaction kettle, and crystallize at 150° C. for 30 hours while stirring. It is then cooled, the crystallized solid product is filtered, and the mother liquor of crystallization is recovered. The above solid crystalline product was filtered, washed and dried. The obtained crystals were determined to be MCM-22 by X-ray diffractometer. SiO was obtained by chemical analysis 2 / Al 2 o ...

Embodiment 2

[0032] Sodium aluminate (Al 2 o 3 35.21 wt%, Na 2 O31.12% by weight) 14.5 grams are dissolved in 500 grams of water, add 6.18 grams of sodium hydroxide to make it dissolve, then add organic amine template agent hexamethyleneimine 39.6 grams and 499.9 grams of hexamethylene under the situation of stirring The crystallization mother liquor of 9.9 grams of imines, then add silica sol (SiO 2 40% by weight) 150 grams, after being stirred evenly, the material proportion (mol ratio) of reactant is:

[0033] SiO 2 / Al 2 o 3 =20

[0034] Oh - / SiO 2 =0.3

[0035] R / SiO 2 =0.5

[0036] h 2 O / SiO 2 =60

[0037] After stirring for 30 minutes, put it into a stainless steel reaction kettle, and crystallize at 150° C. for 30 hours while stirring. After taking out, it is filtered, washed and dried. The obtained crystals were determined to be MCM-22 by X-ray diffractometer. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 19.3.

Embodiment 3

[0039] Sodium aluminate (Al 2 o 3 35.21 wt%, Na 2(21.12% by weight) 14.5 grams are dissolved in 500 grams of water, add 18.18 grams of sodium hydroxide to make it dissolve, then add organic amine template agent hexamethyleneimine 59.5 grams and 2648.5 grams of hexamethylene under the situation of stirring The crystallization mother liquor of base imine 178.5 grams, add silica sol (SiO 2 40% by weight) 450.7 grams, after being stirred evenly, the material proportion (mol ratio) of reactant is:

[0040] SiO 2 / Al 2 o 3 =60

[0041] Oh - / SiO 2 =0.2

[0042] R / SiO 2 =0.8

[0043] h 2 O / SiO 2 =60

[0044] After stirring for 30 minutes, put it into a stainless steel reaction kettle, and crystallize at 150° C. for 50 hours while stirring. After taking out, it is filtered, washed and dried. The obtained crystals were determined to be MCM-22 by X-ray diffractometer. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 52.

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Abstract

The present invention relates to the preparation process of MCM-22 molecular sieve and solves the problems in the preparation process, including high synthesis cost and environmental pollution. The technological scheme of the present invention is that during the preparation of MCM-22 molecular sieve, partial or all the template agent comes from MCM-22 molecular sieve crystallizing mother liquid. The present invention may be used in industrial preparation.

Description

technical field [0001] The invention relates to a preparation method of MCM-22 molecular sieve. Background technique [0002] MCM-22 molecular sieve is a novel catalytic material reported in 1990. It has two independent ten-membered ring channel systems, one of which contains a large supercage of 0.71 nanometers × 0.71 nanometers × 1.82 nanometers. These supercages are stacked one on top of the other by overlapping six-membered rings, interspersed in approximately elliptical ten-membered ring windows. Another channel system forms two-dimensional sinusoidal waveform channels surrounded by coincident six-membered rings connected to supercages. Since MCM-22 has a different pore structure, unusual thermal stability and high specific surface area than previous molecular sieves, it has a very important application in industrial catalysis. For example, in the process of producing cumene from propylene and benzene, the extraordinary selectivity of MCM...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/06C01B39/04
Inventor 高焕新周斌顾瑞芳方华季树芳
Owner CHINA PETROLEUM & CHEM CORP
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