Method for removing template agent in titanium-silicon molecular sieve raw powder, titanium-silicon molecular sieve and its preparation method and application

A technology of titanium-silicon molecular sieve and template agent, which is applied in the direction of molecular sieve catalysts, preparation of organic compounds, chemical instruments and methods, etc. It can solve the problems of molecular sieve skeleton collapse and damage, high energy consumption, and high requirements for roasting process control, and achieve relative crystallinity Improved effect

Active Publication Date: 2017-03-01
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, when removing the organic base template in titanium-silicon molecular sieves, especially TS-1 molecular sieves, the method of roasting is mostly used. This method is to remove the organic base template by burning, and the template is completely removed. The main problems are: (1) high energy consumption, and the combustion of organic base templates produces NO x and NH 3 (2) The roasting process requires high control, and careless operation will lead to the collapse and damage of the molecular sieve framework

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  • Method for removing template agent in titanium-silicon molecular sieve raw powder, titanium-silicon molecular sieve and its preparation method and application

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preparation example Construction

[0041] According to the method for preparing titanium-silicon molecular sieves of the present invention, it is preferred that the templating agent contains a main templating agent and an auxiliary templating agent, and the main templating agent is selected from one or more of tetraalkyl ammonium hydroxide, alcohol amine and alkyl amine A variety of, the auxiliary templating agent is a surfactant. The surfactant may be a cationic surfactant, an anionic surfactant or a nonionic surfactant. In this way, the titanium-silicon molecular sieve prepared by the method of the present invention has higher relative crystallinity, and the efficiency in the process of synthesizing the molecular sieve is higher.

[0042] According to the method for preparing a titanium-silicon molecular sieve of the present invention, further preferably, the molar ratio of the main template agent to the assistant template agent is 1-10000:1, preferably 2-7500:1, more preferably 3-750: 1.

[0043] According...

Embodiment 1

[0066] (1) Mix tetraethyl orthosilicate and tetrabutyl titanate evenly, and then add the mixed liquid to the aqueous solution of tetrapropyl ammonium hydroxide and mix evenly, among them, tetraethyl orthosilicate, tetrabutyl titanate The molar ratio of ester, tetrapropylammonium hydroxide and water is 1:0.035:0.25:85, stirred at normal pressure and 40°C for 8h to obtain a gel mixture;

[0067] (2) Transfer the gel mixture into a sealed stainless steel reaction kettle, crystallize at 170°C under autogenous pressure for 48 hours, filter the obtained crystallized product, wash with water, and dry at 110°C for 120 minutes to obtain Titanium silicate molecular sieve raw powder of template agent;

[0068] (3) Utilize CO at 50°C and 8.0MPa 2 Extract the aforementioned titanium-silicon molecular sieve raw powder containing template agent for 3 hours, wherein, CO 2 The weight ratio to the original powder of titanium-silicon molecular sieve containing template agent is 10:1 to obtain ...

Embodiment 2

[0072] (1) Mix tetraethyl orthosilicate and tetrabutyl titanate evenly, then add the mixed solution to the aqueous solution of tetrapropylammonium hydroxide and cetyltrimethylammonium bromide and mix evenly, wherein, The molar ratio of tetraethyl orthosilicate, tetrabutyl titanate, tetrapropylammonium hydroxide, cetyltrimethylammonium bromide and water is 1:0.035:0.25:0.01:85, under normal pressure and Stirring at 60° C. for 6 h to obtain a gel mixture;

[0073] (2) Transfer the gel mixture into a sealed stainless steel reaction kettle, crystallize at 170°C under autogenous pressure for 48 hours, filter the obtained crystallized product, wash with water, and dry at 110°C for 120 minutes to obtain Titanium silicate molecular sieve raw powder of template agent;

[0074] (3) Utilize CO at 50°C and 8.0MPa 2 Extract the aforementioned titanium-silicon molecular sieve raw powder containing template agent for 3 hours, wherein, CO 2 The weight ratio to the original powder of titani...

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Abstract

A method for removing templates from original powder of a titanium silicalite comprises: letting the template-containing original powder of the titanium silicalite contact a fluid under supercritical conditions of the fluid, wherein the fluid is a substance which can make the templates enter the fluid from the original powder of the titanium silicalite either through chemical reactions or not. The invention also provides a titanium silicalite obtained by the method, a preparation method thereof, and applications of the titanium silicalite in phenol hydroxylation. The method solves the problems that template removal through roasting in the prior art is high in energy consumption and causes severe environmental pollution, etc. Compared to titanium silicalites prepared by the roasting method in the prior art, the titanium silicalite obtained by removing the templates according to the provided method is improved in relative crystallinity.

Description

technical field [0001] The present invention relates to a method for removing the template agent in the original powder of titanium-silicon molecular sieve and a titanium-silicon molecular sieve prepared by the method for removing the template agent in the original powder of titanium-silicon molecular sieve. The invention also relates to a titanium-silicon molecular sieve A method for preparing a molecular sieve, a titanium-silicon molecular sieve prepared by the method for preparing a titanium-silicon molecular sieve of the present invention, and an application of the titanium-silicon molecular sieve of the present invention in phenol hydroxylation. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. The titanium-silicon molecular sieves that have been synthesized so far include TS-1 with an MFI structure, TS-2 with a MEL structure, and TS-48 with a larger pore structure. These titanium-si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08B01J29/89C07C37/60
CPCY02P20/54
Inventor 林民朱斌舒兴田史春风汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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