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Titanium silicalite molecular sieves as well as synthesis method and application thereof

A technology of titanium-silicon molecular sieve and synthesis method, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of poor stability and low catalyst activity of titanium-silicon materials, and achieve selectivity improvement and preparation The process is simple and conducive to the effect of diffusion

Active Publication Date: 2018-05-04
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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  • Titanium silicalite molecular sieves as well as synthesis method and application thereof
  • Titanium silicalite molecular sieves as well as synthesis method and application thereof
  • Titanium silicalite molecular sieves as well as synthesis method and application thereof

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preparation example Construction

[0015] As previously mentioned, the present invention provides a kind of synthetic method of titanium silicon molecular sieve, this method comprises:

[0016] (1) mixing and contacting a precious metal source, an ammonia source, and optionally water to obtain a first mixture;

[0017] (2) In the presence of a templating agent, mixing the titanium source, the first mixture, and optionally water to obtain a second mixture;

[0018] (3) mixing the second mixture, the organic silicon source, and optionally water to obtain a third mixture;

[0019] (4) subjecting the third mixture to hydrothermal crystallization, and recovering titanium-silicon molecular sieves;

[0020] Wherein, at least one of step (1), step (2) and step (3) is carried out in the presence of vanadium source.

[0021] According to the present invention, preferably step (1) is carried out in the presence of a vanadium source, thereby improving the catalytic activity of the titanium-silicon molecular sieve.

[00...

Embodiment approach

[0028] According to a preferred embodiment of the present invention, the preferred stage (1) and stage (3) meet one or both of the following conditions:

[0029] 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;

[0030] 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.

[0031] 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.

[0032] 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

[0082] (1) The precious metal source palladium chloride, vanadium source vanadium nitrate and ammonia (concentration is 20% by weight) are mixed and contacted to obtain a mixture; precious metal source: ammonia source (weight ratio)=2:20, solute content is 1% by weight, mixed Contact conditions include: 30°C, normal pressure, 4h;

[0083] (2) The mixture is then mixed with tetrabutyl titanate and tetrapropyl ammonium hydroxide;

[0084] (3) Then add tetraethyl orthosilicate, carry out hydrothermal crystallization after mixing, the hydrolysis rate of organosilicon source is 15%; Silicon source: titanium source: precious metal source: vanadium source: templating agent: the molar ratio of water=100 :2:1:1:15:1000;

[0085] 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...

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Abstract

The invention relates to the field of catalysis materials and particularly provides titanium silicalite molecular sieves as well as a synthesis method and an application thereof. The method comprisessteps as follows: (1) a precious metal source, an ammonia source and optional water are mixed and contacted, and a first mixture is obtained; (2) a titanium source, the first mixture and the optionalwater are mixed in the presence of a template agent, and a second mixture is obtained; (3) the second mixture, an organosilicon source and optional water are mixed and a third mixture is obtained; (4)the third mixture is subjected to hydrothermal crystallization, recovering is performed, and the titanium silicalite molecular sieves are obtained; at least one of the step (1), the step (2) and thestep (3) is implemented in the presence of a vanadium source. Compared with the prior art, the titanium silicalite molecular sieves are favorable for diffusion of reactants and a product in an oxidation reaction, accordingly, the oxidation activity is sufficiently played, and the selectivity is improved. The method has no special requirements for raw materials and the preparation process is simple.

Description

technical field [0001] The invention relates to a titanium silicon molecular sieve and its synthesis method and application. 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 costs and safety issues. Since Pt, Pd, Au...

Claims

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Application Information

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IPC IPC(8): C01B39/08B01J29/89
CPCB01J29/89C01B39/08
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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