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Titanium silicalite molecular sieve as well as preparation method and application thereof

A titanium-silicon molecular sieve and molecular sieve technology, which is applied in the fields of molecular sieve and alkali exchange compound, molecular sieve catalyst, oxime preparation, etc., can solve the problems such as poor guiding ability of inorganic base structure, loss of molecular sieve structure yield, complicated preparation method and process, and easy to achieve. Implementation, good effect, high raw material conversion effect

Active Publication Date: 2022-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN1301599A discloses a method of treating TS-1 molecular sieves with a solution containing an organic base to obtain titanium-silicon molecular sieves with intracrystalline hollows, but the size of the hollows in the crystals is relatively large, resulting in partial molecular sieve structures being dissolved and destroyed, resulting in yield loss , and the existing preparation method has complex process, long process and high production cost
[0005] Using inorganic alkali solution such as sodium hydroxide solution for pore expansion treatment is more difficult than organic alkali treatment, mainly because organic alkali has structure-guiding ability, while inorganic alkali has poor structure-guiding ability, which easily leads to molecular sieve structure collapse during the treatment process
[0006] Silanization pore expansion is a method developed in recent years to use silanization reagents as synthetic pore expansion agents to efficiently expand pores. CN108726528A, CN106145147A, CN106145148A, and CN106145149A disclose the preparation of hierarchically porous titanium by improved silanization methods Silicon molecular sieves, titanium-silicon molecular sieves with larger mesoporous volumes can be prepared by the method described above, but titanium-silicon molecular sieves prepared by silanization and pore expansion are more suitable for activating organic peroxides. poor

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  • Titanium silicalite molecular sieve as well as preparation method and application thereof
  • Titanium silicalite molecular sieve as well as preparation method and application thereof
  • Titanium silicalite molecular sieve as well as preparation method and application thereof

Examples

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preparation example Construction

[0024] The present invention also provides a preparation method of titanium-silicon molecular sieve, which is characterized in that the preparation method comprises at least the first step of treatment and the second step of treatment on the titanium-silicon molecular sieve, and the first step of treatment is to treat the titanium-silicon molecular sieve The silica molecular sieve is treated for 0.5-3h under the conditions of external pressure and external addition of water, the apparent pressure is 0.01-1.0Mpa and 100-300°C; the second step of treatment is after the first step of treatment The material is treated for at least 0.5h under the conditions of external pressure and external addition of a liquid with a pH value > 9, a superficial pressure of 0.01-1.0Mpa and a temperature of 300-600°C.

[0025] The externally applied pressure refers to applying a certain pressure from the outside in the process of processing the prepared materials, for example, it can be carried out b...

preparation example 1

[0056] This preparation illustrates the preparation of TS-1-A molecular sieves containing templates.

[0057] About 3 / 4 of the tetrapropylammonium hydroxide (TPAOH, 20wt%) solution was added to the tetraethyl orthosilicate (TEOS) solution to obtain a liquid mixture with a pH of about 13, and then to the The required amount of n-butyl titanate [Ti(OBu) was added dropwise to the obtained liquid mixture 4 ] in anhydrous isopropanol and stirred for 15 minutes. Finally, the remaining TPAOH was slowly added to the mixture and stirred at 348-353K for about 3 hours to obtain a chemical composition of 0.02TiO 2 : SiO 2 :0.36TPA:35H 2 The sol of O was then crystallized at 443K for 3 days, and then the obtained solid was filtered, washed with distilled water, and dried at 373K for 5 hours to obtain a molecular sieve sample, numbered TS-1-A.

[0058] The weight loss of TS-1-A measured between 200-600° C. by thermogravimetric method is 15%.

preparation example 2

[0060] This preparation example illustrates the preparation of TS-1-B molecular sieves containing templates.

[0061] The difference from Preparation Example 1 is that the obtained chemical composition is 0.008TiO 2 : SiO 2 :0.36TPA:35H 2The sol of O, the molecular sieve sample number is TS-1-B.

[0062] The weight loss of TS-1-B at 200-600° C. was measured to be 12% by thermogravimetric method.

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Abstract

A titanium silicalite molecular sieve is characterized in that the total content of silicon dioxide and titanium dioxide is greater than 99% by weight through XRF analysis, the micropore specific surface area of the molecular sieve is 300-450 m < 2 > / g, the mesopore volume is 0.03-0.20 mL / g, pore size distribution is analyzed through a BJH method according to adsorption branches of an N2 adsorption curve, first mesopores in the range of 2-4 nm and second mesopores with the most probable pore size in the range of 4-16 nm exist, and TEM is used for characterization. A plurality of mesopores with the size range of 4-20 nm exist in the molecular sieve.

Description

technical field [0001] The invention relates to inorganic materials and their preparation and application, more specifically to a titanium-silicon molecular sieve and its preparation method and application. Background technique [0002] Molecular sieves have high activity and product selectivity in many reactions due to their unique pore structure and active centers. The insertion of titanium into the zeolite framework opens up new avenues to activate hydrogen peroxide and catalyze the transformation of organic matter under mild conditions. Among them, the discovery of TS-1 molecular sieve has laid a foundation for the development of many new oxidation reactions involving hydrogen peroxide, such as propylene epoxidation, cyclohexanone ammoximation, phenol hydroxylation, and thioether oxidation. [0003] However, the reaction substrate of TS-1 is limited to organic substances with smaller molecular size because the limitation of the pore size of the ten-membered ring of TS-1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/89C07C249/04C07C251/44
CPCC01B39/085B01J29/89C07C249/04C01P2002/85C01P2006/12C01P2006/14C01P2006/17C01P2004/04C01P2002/84C07C2601/14C07C251/44Y02P20/52
Inventor 彭欣欣夏长久王翔宇朱斌林民罗一斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP