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Stepped-type crystallization preparation method of titanium-containing molecular sieve

A titanium molecular sieve and stepped technology, which is applied in the synthesis field of titanium-containing molecular sieve, can solve the problems of increasing the dosage of TPAOH and high cost, and achieve the effects of reducing dosage, high production efficiency and stable performance.

Active Publication Date: 2014-06-18
TAIYUAN DACHENG ENVIRONMENTAL ENERGY CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method effectively solves the problem of titanium polymerization in the synthesis process, but the introduction of acid will neutralize a part of TPAOH in the synthesis, which will increase the amount of TPAOH in the system, resulting in high cost

Method used

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  • Stepped-type crystallization preparation method of titanium-containing molecular sieve
  • Stepped-type crystallization preparation method of titanium-containing molecular sieve
  • Stepped-type crystallization preparation method of titanium-containing molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 50g of silica sol (mass fraction 30%) into 85g of tetrapropylammonium hydroxide (mass fraction 25%) solution, stir vigorously to obtain a gel, transfer it to an autoclave, and keep it at 100°C for 24 hours to obtain a Directing agent: Slowly add 3.3g tetrabutyl titanate to the above-mentioned directing agent dropwise within 3 hours, then raise the temperature to 160°C and keep for 36 hours to obtain the product, and obtain Ti-MFI molecular sieve after separation, washing, drying and roasting , the product is labeled A. Its X-ray diffraction pattern has figure 1 Characteristics.

Embodiment 2

[0032] Add 45g of silica sol (mass fraction 30%) to 82g of tetrapropylammonium hydroxide (mass fraction 25%) solution, stir vigorously to obtain a gel, transfer to an autoclave, and keep at 110°C for 24 hours to obtain a Directing agent: Slowly add 3.0g tetraethyl titanate to the above directing agent dropwise within 5 hours, then raise the temperature to 170°C and keep for 24 hours to obtain the product, and obtain Ti-MFI molecular sieve after separation, washing, drying and roasting , the product is labeled B. Its X-ray diffraction pattern has figure 1 Characteristics.

Embodiment 3

[0034] Add 68g of silica sol (mass fraction 30%) to 80g of tetrapropylammonium hydroxide (mass fraction 25%) solution, stir vigorously to obtain a gel, transfer to an autoclave, and keep at 120°C for 12 hours to obtain a Directing agent: Slowly add 4.5g tetrabutyl titanate to the above-mentioned directing agent dropwise within 3 hours, then raise the temperature to 170°C and keep for 30 hours to obtain the product, and obtain Ti-MFI molecular sieve after separation, washing, drying and roasting , the product is labeled C. Its X-ray diffraction pattern has figure 1 Characteristics.

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Abstract

The invention relates to a synthesis method of a titanium-containing molecular sieve, and particularly relates to a method for preparing a titanium-containing molecular sieve by adopting a stepped crystallization also called as a lattice vacancy filling method. The invention provides a method for fast preparing a TS-1 molecular sieve, which is simple and feasible and relatively low in cost. According to the technical scheme, the stepped crystallization preparation method of the titanium-containing molecular sieve comprises the following steps: 1, sufficiently hydrolyzing a tetrapropylammonium hydroxide solution added with an inorganic silicon source to prepare gel; 2, transferring the gel to a sealed reaction kettle, carrying out pre-crystallization to prepare a pure silicon molecular sieve guiding agent, then slowly dropwise adding a titanium source to the pure silicon molecular sieve guiding agent, and continuously pre-crystallizing for 1-6 hours to obtain a mixture to be crystallized; 3, crystallizing the mixture to be crystallized, controlling the temperature to rise to 160-200 DEG C, and carrying out hydrothermal crystallization for 6-48 hours to obtain the titanium-containing molecular sieve.

Description

technical field [0001] The invention relates to a method for synthesizing titanium-containing molecular sieves, in particular to a method for preparing titanium-containing molecular sieves by adopting stepwise crystallization or filling vacant positions in crystal lattices. Background technique [0002] Titanium-containing molecular sieves are heteroatom molecular sieves developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MFL structure, and TS-48 with larger pore structure have been synthesized. This type of molecular sieve framework contains transition metal titanium atoms with variable valence characteristics, which enables it to form redox catalysis and has shape-selective functions, so it has excellent directional catalytic oxidation performance and can be used as a new generation of green chemical catalysts for selective oxidation. For example, titanium-silicon molecular sieves have excellent catalytic activity and directional oxidation performa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/89C07C39/08C07C37/60
Inventor 李晓峰窦涛狄春雨张军亮
Owner TAIYUAN DACHENG ENVIRONMENTAL ENERGY CHEM TECH
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