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Noble metal modified titanium-silicon molecular sieve and preparation method and application thereof, and method for direct oxidation of olefins

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

Active Publication Date: 2017-07-04
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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  • Noble metal modified titanium-silicon molecular sieve and preparation method and application thereof, and method for direct oxidation of olefins
  • Noble metal modified titanium-silicon molecular sieve and preparation method and application thereof, and method for direct oxidation of olefins
  • Noble metal modified titanium-silicon molecular sieve and preparation method and application thereof, and method for direct oxidation of olefins

Examples

Experimental program
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preparation example Construction

[0028] Therefore, as previously mentioned, the present invention provides a method for preparing the noble metal-modified titanium-silicon 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, The acid solution contains peroxide and nitric acid;

[0030] (2) The second heat treatment is performed after mixing the first solid, the titanium source, 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 c...

Embodiment approach

[0044] According to a preferred embodiment of the present invention, the preferred stage (1) and stage (3) meet one or both of the following conditions:

[0045] Condition 1: the temperature of stage (1) is lower than the temperature of stage (3), preferably, the temperature of stage (1) is 10-50°C lower than the temperature of stage (3), preferably 20-40°C lower;

[0046] Condition 2: the time of stage (1) is less than the time of stage (3), preferably, the time of stage (1) is 5-24 hours shorter than the time of stage (3), preferably 6-12 hours shorter.

[0047] According to a preferred embodiment of the present invention, the temperature in stage (2) is lowered to not higher than 50°C, preferably 30-50°C, and the residence time is at least 1 hour, preferably 1-5h.

[0048] According to the method of the present invention, the heating rate and cooling rate for adjusting the temperature to the temperature of each stage can be selected according to the type of the reactor used...

Embodiment 1

[0112] This example illustrates the methods and products provided by the invention.

[0113] Under normal temperature (20 DEG C, all the other comparative examples are the same as the examples) and normal pressure (0.1MPa, all the other comparative examples are the same as the examples), the deactivated cyclohexanone oximation catalyst SH-2 and acid solution (containing nitric acid and the aqueous solution of hydrogen peroxide, the concentrations of nitric acid and hydrogen peroxide are both 4mol / L) mixed and beaten, and then the mixed slurry was mixed and stirred at 80°C for 12h; after solid-liquid separation, the solid, precious metal source palladium chloride, titanium After mixing the source titanium sulfate and sodium hydroxide aqueous solution (pH 12), put the mixed solution into a stainless steel sealed reaction kettle, and go through the first stage at 140°C for 6h, then cool the mixture down to 30°C and go through the second stage for 2h, then continue Go through the ...

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Abstract

The invention relates to the field of molecular sieves, and mainly provides a noble metal modified titanium-silicon molecular sieve, and a preparation method and an application thereof. The molecular sieve comprises a noble metal element, a titanium element, a silicon element and an oxygen element; the molecular sieve has a pore volume of 0.3 cm3 / g or above, a total specific surface area of 200 m2 / g or above and an outer surface area of 30 m2 / g or above, wherein the outer surface area accounts for 7 to 55% of the total specific surface area; the benzene adsorption capacity measured by the molecular sieve under the conditions of 25 DEG C, P / P0 of 0.10 and the adsorption time of 1 hour is at least 75 mg / g molecular sieves, and micropore size distribution is in a range of 0.9 to 1.5 nm under N2 static adsorption testing; and the molecular sieve has a surface silicon-to-titanium ratio no less than a bulk phase silicon-to-titanium ratio. The invention also provides a method for direct oxidation of olefins. The noble metal modified titanium-silicon molecular sieve with a special physical-chemical characteristic structure provided by the invention has the advantages of high benzene adsorption capacity and micropore size distribution in a range of 0.9 to 1.5 nm, and can obtain better catalytic effect when applied to reaction with cyclic molecules and olefin molecules involved or generated, for example.

Description

technical field [0001] The present invention relates to a noble metal-modified titanium-silicon molecular sieve and its preparation method and application, more specifically to a method for preparing a noble metal-modified titanium-silicon molecular sieve using an inactivated titanium-silicon molecular sieve catalyst. The invention also relates to an olefin direct oxidation method. 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 exc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/89C07D301/08C07D303/04
CPCB01J29/89B01J2229/20C01B39/08C01P2006/16C07D301/08C07D303/04
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP