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Molecular sieve containing precious metals, preparation method and applications thereof, and alkene direct oxidation method

A precious metal, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of poor stability and low activity of titanium-silicon material catalysts, and achieve good catalytic effect.

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

AI Technical Summary

Problems solved by technology

Although the method of supporting noble metals on titanium-silicon materials to generate H2O2 in situ for selective oxidation of organic matter has mild conditions and good selectivity (up to 95% ), but the titanium-silicon catalysts loaded with precious metals have low activity and poor stability

Method used

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  • Molecular sieve containing precious metals, preparation method and applications thereof, and alkene direct oxidation method
  • Molecular sieve containing precious metals, preparation method and applications thereof, and alkene direct oxidation method
  • Molecular sieve containing precious metals, preparation method and applications thereof, and alkene direct oxidation method

Examples

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preparation example Construction

[0028] Therefore, as previously mentioned, the present invention provides a preparation method of the noble metal-containing molecular sieve of the present invention, the method comprising:

[0029] (1) mixing the unloading agent with the acid solution for beating, carrying out the first heat treatment on the obtained slurry, and separating and obtaining the first solid, wherein the unloading agent is the unloading agent of a reaction device using titanium-silicon molecular sieve as a catalyst;

[0030] (2) The second heat treatment is performed after mixing the first solid, the noble metal source and the alkali source in the presence of an aqueous solvent.

[0031] In the present invention, the unloading agent of the reaction device using titanium-silicon molecular sieve as the catalyst can be the unloading agent unloaded from various devices using titanium-silicon molecular sieve as the catalyst, for example, it can be from the catalyst using titanium-silicon molecular sieve ...

Embodiment 1

[0102] This example illustrates the methods and products provided by the invention.

[0103] 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 is mixed and beaten, and then the mixed slurry is mixed and stirred at 80°C for 12 hours; after solid-liquid separation, the solid, precious metal source palladium chloride and sodium hydroxide aqueous solution (pH 12) are mixed, and the mixed solution is put into a stainless steel sealed reaction kettle , treated at 170°C for 12 hours, wherein, the mass composition of the material is deactivated cyclohexanone oxime catalyst: noble metal source: acid: alkali: water = 100:1:10:5:250, deactivated cyclohexanone oxime Catalyst with SiO 2 In terms of acid, H + In terms of alkali in OH - count. T...

Embodiment 2

[0108] This example illustrates the methods and products provided by the invention.

[0109] 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, The precious metal source palladium acetylacetonate 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, wherein the mass composition of the material is deactivated cyclohexanone oximation Catalyst: noble metal source: acid: base: water = 100: 0.5: 15: 15: 200, deactivated cyclohexanone oximation catalyst with 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 noble metal-containing molecular sieve, whose XRD crystal ph...

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Abstract

The invention relates to the field of molecular sieves, and mainly provides a molecular sieve containing precious metals, a preparation method and applications thereof. The molecular sieve containing precious metals comprises precious metal elements, a silicon element, and an oxygen element. The pore volume of the 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. The external surface area accounts for 7 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 1.0 to 1.8 nm. The invention also provides an alkene direct oxidation method. The provided molecular sieve containing precious metals has a special physico-chemical structure, the benzene absorption amount is high, and the micro pore size distribution is in a range of 1.0 to 1.8 nm. The molecular sieve can achieve a good catalytic effect, when being applied to reactions that generate circular molecules and alkene molecules or reactions that circular molecules and alkene molecules participate in.

Description

technical field [0001] The present invention relates to a molecular sieve containing noble metal and its preparation method and application, more specifically to a method for preparing molecular sieve containing noble metal by using deactivated titanium silicon molecular sieve catalyst, and also relates to a method for direct oxidation of olefins. Background technique [0002] Titanium-silicon molecular sieve is a molecular sieve whose skeleton is composed of silicon, titanium and oxygen elements, and 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 ...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07D301/06C07D303/04
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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