Titanium silicalite molecular sieve, synthetic method and application of titanium silicalite molecular sieve, and cyclic ketone oxidation method

A titanium-silicon molecular sieve and a synthesis method technology are applied in molecular sieve compounds, molecular sieve catalysts, molecular sieve characteristic silicates, etc., which can solve the problems of poor stability and low catalyst activity of titanium-silicon materials, and achieve improved selectivity, easy industrial application, High utilization effect

Active Publication Date: 2018-04-06
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 m

Method used

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  • Titanium silicalite molecular sieve, synthetic method and application of titanium silicalite molecular sieve, and cyclic ketone oxidation method
  • Titanium silicalite molecular sieve, synthetic method and application of titanium silicalite molecular sieve, and cyclic ketone oxidation method
  • Titanium silicalite molecular sieve, synthetic method and application of titanium silicalite molecular sieve, and cyclic ketone oxidation method

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preparation example Construction

[0031] In the present invention, as long as the titanium-silicon molecular sieve has the aforementioned characteristics, the purpose of the present invention can be achieved, and its synthesis method can be various, as long as the titanium-silicon molecular sieve with the aforementioned characteristics can be synthesized. For the present invention, the titanium-silicon molecular sieve is preferably Silicon molecular sieves are synthesized as follows, the method comprising:

[0032] (1) mixing and contacting a precious metal source, an ammonia source, and optionally water to obtain a first mixture;

[0033] (2) In the presence of a templating agent, mixing the titanium source, the first mixture, and optionally water to obtain a second mixture;

[0034] (3) mixing the second mixture, the organic silicon source, and optionally water to obtain a third mixture;

[0035] (4) The third mixture is subjected to hydrothermal crystallization, and titanium-silicon molecular sieves are re...

Embodiment approach

[0042] According to a preferred embodiment of the present invention, the preferred stage (1) and stage (3) meet one or both of the following conditions:

[0043] 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;

[0044] 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.

[0045] 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.

[0046] 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

[0101] (1) Mixing and contacting noble metal source palladium chloride and ammonia water (concentration is 20% by weight) to obtain a mixture; noble metal source: ammonia source (weight ratio)=2:20, solute content is 1% by weight, and the conditions for mixing and contacting include: 30°C, normal pressure, 4h;

[0102] (2) The mixture is then mixed with tetrabutyl titanate and tetrapropyl ammonium hydroxide;

[0103] (3) Then add tetraethyl orthosilicate, mix and carry out hydrothermal crystallization, the hydrolysis rate of organosilicon source is 15%; silicon source: titanium source: precious metal source: templating agent: water=100:2:1:15 :1000;

[0104] Hydrothermal crystallization: go through the first stage at 140°C for 6 hours in a sealed reactor, then cool the mixture down to 30°C and experience the second stage for 2 hours, then continue to go through the third stage at a temperature of 170°C in a sealed reactor 12h (among them, the temperature rise rate from room ...

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Abstract

The invention relates to the field of catalytic materials and in particular provides a titanium silicalite molecular sieve, a synthetic method and application of the titanium silicalite molecular sieve. The titanium silicalite molecular sieve is composed of the following elements in percentage by mass: 0.01-5% of precious metals, silicon, 0.02-8% of titanium and oxygen, wherein the I960/I550 valueis 0.6-0.9; the U480/U330 value is 0.5-5; and the N-116/N-112 value is 0.01-0.2. The invention further provides a cyclic ketone oxidation method. The cyclic ketone oxidation method comprises the following step: contacting cyclic ketone, an oxidizing agent and a catalyst, wherein the catalyst contains the titanium silicalite molecular sieve disclosed by the invention. Compared with the prior art,the titanium silicalite molecular sieve disclosed by the invention has the advantages that diffusion of the reactants and product is facilitated in an oxidation reaction, so that oxidative activity isfully achieved, and the selectivity is improved. For example, when applied to a reaction in which ring molecules, particularly cyclic ketone molecules, participate or are produced, the titanium silicalite molecular sieve can achieve excellent catalytic effects. Moreover, filtration and separation of the catalyst after the reaction can be further facilitated, and industrialized application is easily realized.

Description

technical field [0001] The invention relates to a titanium-silicon molecular sieve, its synthesis method and application, and a method for oxidizing cyclic ketones. Background technique [0002] Hydrogen peroxide (H 2 o 2 ) is a recognized green oxidant, and its oxidation by-product is only water. But since H 2 o 2 Extremely unstable, rough surface, heavy metals and other impurities will decompose when exposed to heat and light, and it is corrosive. Special safety measures should be taken in packaging, storage and transportation. Therefore, the H 2 o 2 applied in-place, or the H 2 o 2 Production process and use H 2 o 2 The combination of downstream processes can make more effective use of this chemical product. Use H 2 and O 2 Can directly synthesize H 2 o 2 , and the utilization rate of atoms reaches 100%, and then people want to use H 2 and O 2 to in situ synthesis of H 2 o 2 reoxidation of organic feedstocks to address direct utilization of H 2 o 2 co...

Claims

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Application Information

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IPC IPC(8): C01B37/00B01J29/89C07C51/285C07C59/01
CPCB01J29/89C01B37/005C01P2002/82C01P2002/84C01P2004/61C01P2004/62C01P2006/12C01P2006/14C07C51/285C07C59/01
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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