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Tin-titanium-silicon molecular sieve, preparation method and applications thereof, and cyclic ketone oxidation method

A technology of tin-titanium-silicon molecular sieve and cyclic ketone, which is applied in molecular sieve catalyst, oxidative preparation of carboxylic acid, chemical instruments and methods, etc., can solve the problems of occupying land resources and storage space, and achieve good catalytic effect.

Active Publication Date: 2016-10-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this way, valuable land resources and storage space are taken up, and the recovery and utilization technology development of deactivated ammoximation catalysts is urgently needed

Method used

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  • Tin-titanium-silicon molecular sieve, preparation method and applications thereof, and cyclic ketone oxidation method
  • Tin-titanium-silicon molecular sieve, preparation method and applications thereof, and cyclic ketone oxidation method
  • Tin-titanium-silicon molecular sieve, preparation method and applications thereof, and cyclic ketone oxidation method

Examples

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preparation example Construction

[0026] Therefore, as previously mentioned, the present invention provides a kind of preparation method of tin-titanium-silicon molecular sieve of the present invention, the method comprises:

[0027] (1) Mix the unloading agent with the acid solution for beating, carry out the first heat treatment to the obtained slurry, and separate and obtain the first solid, wherein the unloading agent is the unloading agent of the reaction device using titanium silicon molecular sieve as the catalyst active component. Dispensing;

[0028] (2) The second heat treatment is performed after mixing the first solid, the tin source, the titanium source and the alkali source in the presence of an aqueous solvent.

[0029]In the present invention, the unloading agent of the reaction device using titanium-silicon molecular sieve as the catalyst active component can be the unloading agent from various devices that use titanium-silicon molecular sieve as the catalyst active component, for example, it ...

Embodiment 1

[0105] This example illustrates the methods and products provided by the invention.

[0106] At normal temperature (20°C, the rest of the comparative examples are the same as the examples) and normal pressure (0.1MPa, the rest of the comparative examples are the same as the examples), the deactivated cyclohexanone oximation catalyst SH-2 and 1mol / L hydrochloric acid The aqueous solution was mixed and beaten, and then the mixed slurry was mixed and stirred at 80°C for 12 hours; after solid-liquid separation, the solid, tin source tin chloride pentahydrate, titanium source titanium sulfate and sodium hydroxide aqueous solution (pH 12) were mixed and mixed Put the liquid into a stainless steel sealed reaction kettle, and treat it at 170°C for 12 hours, wherein, the mass composition of the material is an inactivated cyclohexanone oximation catalyst: titanium source: tin source: acid: alkali: water = 100:1:2:10 :5:250, deactivated cyclohexanone oximation catalyst with SiO 2 In ter...

Embodiment 2

[0111] This example illustrates the methods and products provided by the invention.

[0112] At normal temperature and pressure, first mix the deactivated cyclohexanone oximation catalyst SH-3 with 5mol / L hydrochloric acid solution for beating, then mix and stir the mixed slurry at 60°C for 1 hour; after solid-liquid separation, separate the solid, Tin source tin chloride pentahydrate, titanium source tetrabutyl titanate and tetrapropyl ammonium hydroxide aqueous solution (pH 10) are mixed, and the mixture is put into a stainless steel sealed reaction kettle, and treated at 150°C for 12 hours, the mass of the material Composed of deactivated cyclohexanone oximation catalyst: titanium source: tin source: acid: alkali: water = 100: 2: 3.5: 15: 15: 200, the deactivated cyclohexanone oximation catalyst is SiO 2 In terms of acid, H + In terms of alkali in OH - count. Then the product was recovered according to the method of Example 1 to obtain a tin-titanium-silicon molecular si...

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Abstract

The invention relates to the field of molecular sieves, and mainly provides a tin-titanium-silicon molecular sieve, a preparation method and applications thereof. The tin-titanium-silicon molecular sieve comprises a tin element, a titanium element, a silicon element, and an oxygen element. The pore volume of the tin-titanium-silicon molecular sieve is 0.3 cm3 / g or more. The total specific surface area is 200 m2 / g or more, the external surface area is 30 m2 / g or more, and the external surface area accounts for 10 to 55% of the total specific surface area. The benzene absorption amount is at least 65 mg for each gram of molecular sieve under following conditions: temperature: 25 DEG C, P / P0=0.10, and absorption time: 1 hour. Under N2 static absorption tests, the micro pore size distribution is in a range of 0.9 to 2.0 nm. The invention also provides a cyclic ketone oxidation method. The provided molecular sieve has a special physico-chemical structure, the benzene absorption amount is high, and the micro pore size distribution is in a range of 0.9 to 2.0 nm. The molecular sieve can achieve a better catalytic effect, when being applied to reactions that generate circular molecules (especially cyclic ketone molecules) or reactions that circular molecules (especially cyclic ketone molecules) participate in.

Description

technical field [0001] The invention relates to a tin-titanium-silicon molecular sieve and a preparation method of the tin-titanium-silicon molecular sieve, and also relates to the application of the tin-titanium-silicon molecular sieve and a method for oxidizing cyclic ketones. Background technique [0002] Titanium-silicon molecular sieve is a molecular sieve whose skeleton is composed of silicon, titanium and oxygen elements. It has broad application prospects in petroleum refining and petrochemical industry. Among them, TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. [0003] TS-1 not only has the catalytic oxidation of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve, and has successfully realized industrial application in the proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/04C07C51/31C07C59/01
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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