Preparation method of molecular sieve primary structural unit pillared magnesium saponite

A technology of structural units and molecular sieves, applied in chemical instruments and methods, non-metallic elements, inorganic chemistry, etc., can solve problems such as layered pore structure damage, and achieve high hydrothermal stability

Active Publication Date: 2012-10-31
PETROCHINA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods use soapstone or clay as raw materials to further prepare microporous or me

Method used

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  • Preparation method of molecular sieve primary structural unit pillared magnesium saponite
  • Preparation method of molecular sieve primary structural unit pillared magnesium saponite
  • Preparation method of molecular sieve primary structural unit pillared magnesium saponite

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Experimental program
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Embodiment 1

[0030] This embodiment provides a preparation method of magnesium saponite supported by the primary structural unit of ZSM-5 molecular sieve, which comprises the following steps:

[0031] Intercalation reaction: Disperse 5g of stesterite into 100ml of deionized water, then add 15g of cetyltrimethylammonium bromide, react in a water bath at 60°C for 10h, then add 30g of tetrabutylammonium hydroxide, Stir at 80°C for 24 hours to prepare solution A;

[0032] Preparation of pillared soapstone: 5.21gAl 2 (SO 4 ) 3 Soluble in 60g water and 5.88g H 2 SO 4 (concentrated sulfuric acid, the concentration is 98wt%), make a solution, then add 70g of silica sol and 20g of water, stir for 2h to make gel B; mix gel B with solution A, stir at 50°C for 15h , and finally crystallized at 90°C for 8 hours to obtain stesterite with pillared primary structural unit of ZSM-5 molecular sieve, and its XRD pattern is as follows figure 1 shown.

Embodiment 2

[0034] This embodiment provides a preparation method of magnesium saponite supported by the primary structural unit of ZSM-5 molecular sieve, which comprises the following steps:

[0035] Intercalation reaction: Disperse 5g of magnesium saponite into 100ml of deionized water, then add 10g of tetraethylammonium chloride, react in a water bath at 80°C for 5h, then add 20g of triethylamine, and stir at 40°C for 20h , to make solution A;

[0036] Preparation of pillared soapstone: 5.21gAl 2 (SO 4 ) 3 Soluble in 60g water and 5.88g H 2 SO 4 (concentrated sulfuric acid, the concentration is 98wt%), make a solution, then add 70g of silica sol and 20g of water, stir for 2h to make gel B; mix gel B with solution A, stir at 50°C for 15h , and finally crystallized at 90°C for 8 hours to obtain stesterite with pillared primary structural unit of ZSM-5 molecular sieve, and its XRD pattern is as follows figure 1 shown.

Embodiment 3

[0038] This embodiment provides a preparation method of magnesium saponite supported by the primary structural unit of ZSM-5 molecular sieve, which comprises the following steps:

[0039] Intercalation reaction: Disperse 5g of magnesium saponite into 100ml of deionized water, then add 20g of tetraethylammonium chloride and dihexadecyldimethylammonium bromide, react in a water bath at 70°C for 9h, and then add Add 20g of diethanolamine and stir at 60°C for 12h to prepare solution A;

[0040] Preparation of pillared soapstone: 5.21gAl 2 (SO 4 ) 3 Soluble in 60g water and 5.88g H 2 SO 4 (concentrated sulfuric acid, the concentration is 98wt%), make a solution, then add 70g of silica sol and 20g of water, stir for 2h to make gel B; mix gel B with solution A, stir at 50°C for 15h , and finally crystallized at 100°C for 12 hours to obtain the magnesium saponite supported by the primary structural unit of ZSM-5 molecular sieve, and its XRD pattern is as follows figure 1 shown. ...

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Abstract

The invention relates to a preparation method of molecular sieve primary structural unit pillared magnesium saponite. The preparation method comprises the following steps of: dispersing magnesium saponite in deionized water, adding a surfactant, heating to 30-90 DEG C for reaction for 1-26hours, then adding a template agent for synthesizing a ZSM-5 molecular sieve, and stirring for 1-26hours at 40-100 DEG C to obtain a mixed solution; and adding gel for synthesizing the ZSM-5 molecular sieve in the mixed solution, stirring for 2-30hours at 0-80 DEG C, and conducting crystallization treatment at 80-200 DEG C to obtain the molecular sieve primary structural unit pillared magnesium saponite. The preparation method provided by the invention takes a primary structural unit of the ZSM-5 molecular sieve as a pillar for pillaring the magnesium saponite, and the prepared pillared magnesium saponite has higher hydrothermal stability.

Description

technical field [0001] The invention relates to a preparation method of pillared saponite, in particular to a preparation method of pillared magnesium saponite, a molecular sieve primary structural unit, and belongs to the technical field of preparation of saponite materials. Background technique [0002] Soapstone is a three-octahedral clay mineral, and its structural formula can be written as M n+ (x-y)n (Si 8-x Al x )(Mg 6-y R y ), R is ion Al 3+ or Fe 3+ . Soapstone has a two-dimensional layered silicate structure, and its single layer is generally composed of T-O-T layers, that is, a sandwich structure composed of two silicon-oxygen tetrahedral layers sandwiching an aluminum-oxygen octahedron in the middle, and the octahedral layers are composed of 6 magnesium Atoms are filled, and the center of the silicon-oxygen tetrahedron is replaced by atoms such as Al to form a layer charge. The interlayers of such layered column materials generally have exchangeable cati...

Claims

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Application Information

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IPC IPC(8): C01B33/40
Inventor 张强崔秋凯李春义杨文慧徐少军山红红杨朝合常新华李凤义
Owner PETROCHINA CO LTD
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