Preparation method and application of supported TS-1 catalyst

A technology of TS-1 and catalyst, which is applied in the field of preparation of supported TS-1 catalyst, can solve the problems of difficult separation and recovery of TS-1 catalyst, and achieve the effects of reducing the difficulty of loading, increasing stability and facilitating recycling and utilization.

Active Publication Date: 2022-06-28
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main purpose of the present invention is to provide a preparation method and application of a supported TS-1 catalyst to solve the problem that the TS-1 catalyst is not easy to separate and recover in the ammoximation reaction of ketones

Method used

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  • Preparation method and application of supported TS-1 catalyst
  • Preparation method and application of supported TS-1 catalyst

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Experimental program
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preparation example Construction

[0041]In the prior art, the preparation methods of the TS-1 catalyst mainly include: spray drying molding method, extrusion molding method, and direct roasting molding method. The spray drying method is to use the principle of spray drying to mix the crystallized TS-1 with the auxiliary agent, and then spray it into the drying chamber in the form of a mist to obtain a microspherical catalyst; the extrusion molding method is to mix water, binder and The TS-1 powder is fully mixed and sent to the extruder. Under the action of external pressure, it is extruded in a cylindrical or other shape; After the alcohol-propylene glycol copolymer is mixed into a slurry, it is directly calcined to obtain a TS-1 catalyst.

[0042] Heterogeneous nucleation principle: There are three forms of nucleation, namely primary homogeneous nucleation, primary heterogeneous nucleation and secondary nucleation. At high supersaturation, the process that the solution spontaneously generates crystal nuclei...

specific Embodiment 1

[0044] The embodiment of the present invention provides a preparation method of a supported TS-1 catalyst, figure 1 is a flow chart of the steps of the method, such as figure 1 As shown, the method includes:

[0045] S1: dissolving the templating agent and the silicon source compound in water respectively to obtain a templating agent solution;

[0046] Dissolve the templating agent and silicon source compound in water and stir vigorously until a clear, homogeneous templating agent solution is formed. The template agent is generally a reagent that plays a structure-oriented role in the preparation process of the molecular sieve catalyst. In the embodiment of the present invention, the template agent is tetrapropyl ammonium hydroxide (TPAOH), tetrapropyl ammonium bromide (TPABr), One or more of n-butylamine and inorganic alkali ammonia water, preferably tetrapropylamine hydroxide (TPAOH). The silicon source compound is tetraethyl silicate (TEOS).

[0047] S2: dissolving the ...

Embodiment approach

[0063] One implementation is:

[0064] Step S4 further includes, S4': adding the precursor mixture into the organic amine solution, and stirring, to obtain the organic amine-treated precursor mixture;

[0065] The step S5 is specifically as follows: adding the calcined oxide carrier into the organic amine-treated precursor mixture, and performing crystallization to obtain the solid precipitate.

[0066] The organic amine solution can be methylamine solution or ethylamine solution, which is not limited in this embodiment. TS-1 molecular sieve and ZSM-5 molecular sieve have the same MFI topology, belong to orthorhombic crystal system, and its skeleton contains two intersecting channel systems. in TS-1. TI atoms enter the molecular sieve framework and are highly dispersed, forming isolated -Si-O-Ti-O-Si- units without the existence of Ti-O-Ti structure. The excellent catalytic oxygen activity of TS-1 molecular sieve is not simply caused by the acidity and alkalinity of the mol...

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Abstract

The invention discloses a preparation method and application of a supported TS-1 catalyst, and belongs to the technical field of chemistry and chemical engineering. The preparation method comprises the following steps: preparing a template agent solution and a titanium source-containing solution, and roasting an oxide carrier at the roasting temperature of 120-720 DEG C for 1-3 hours, thereby obtaining the roasted oxide carrier; then, dropwise adding the titanium source-containing solution into the template agent solution to obtain a precursor mixed solution; then, adding a roasted oxide carrier into the precursor mixed solution, and crystallizing to obtain a solid precipitate; and washing, drying and roasting the solid precipitate to obtain the supported TS-1 catalyst. According to the preparation method provided by the invention, the oxide carrier is roasted for a period of time at a certain temperature in advance so as to change the surface appearance and property of the carrier and increase the specific surface area, so that the regulation and control of the TS-1 loading capacity and the particle size are realized.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical industry, in particular to a preparation method and application of a supported TS-1 catalyst. Background technique [0002] In the 1980s, Taramasso synthesized a new catalyst titanium-silicon molecular sieve TS-1 by adding Ti atoms to the ZSM-5 framework to replace the original Al atoms. TS-1 catalyst showed good selectivity and excellent catalytic properties in the selective oxidation of a series of organic compounds with hydrogen peroxide as the oxidant, especially in the ammoximation of ketones. Features: High conversion rate of ketones, mild reaction conditions, low equipment investment cost, and green by-products without pollution. Therefore, it is widely used in fine chemicals, environmental protection and other related fields. [0003] In actual industrial production, the TS-1 catalyst used in the ammoximation reaction of ketones is mostly raw powder, and the particle size ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C07C251/44C07C251/38C07C249/04
CPCB01J29/89C07C249/04B01J2229/60C07C2601/14C07C251/44C07C251/38
Inventor 骆广生杜晨灿王玉滨闫自飞
Owner TSINGHUA UNIV
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