Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Titanium silicon molecular sieve, synthetic method and applications thereof, and cyclic ketone oxidation method

A titanium-silicon molecular sieve and synthesis method technology, applied in molecular sieve compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of small grain size, insufficient reactivity, complex process, etc., and achieve improved selectivity and good catalytic activity. The effect of stability and high utilization rate

Active Publication Date: 2018-01-05
CHINA PETROLEUM & CHEM CORP +1
View PDF11 Cites 20 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, follow-up research is devoted to the development of technologies for increasing the particle size of molecular sieves. For example, US5500199, US6106803 and US6524984, etc. use inorganic binders to gather small particle molecular sieves and then spray dry and granulate them to make the catalyst particles larger. The center is covered by the binder and the active components are diluted, resulting in insufficient reactivity and other problems
[0004] CN101696019B relates to a large block TS-1 molecular sieve with high catalytic activity and its synthesis method. The large block TS-1 molecular sieve has an MFI structure and is formed by stacking nanometer-level TS-1 grains, and the block size is larger. 20-100μm, the mesopore volume is 0.55cm 3 / g; with ethyl orthosilicate as silicon source, n-butyl titanate as titanium source, tetrapropylammonium hydroxide as template, water and isopropanol as solvent, H 2 o 2 It is synthesized by hydrothermal crystallization of inorganic additives, and the process is complicated
Although the obtained molecular sieve has high activity, the grain size is less than 1 μm

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Titanium silicon molecular sieve, synthetic method and applications thereof, and cyclic ketone oxidation method
  • Titanium silicon molecular sieve, synthetic method and applications thereof, and cyclic ketone oxidation method
  • Titanium silicon molecular sieve, synthetic method and applications thereof, and cyclic ketone oxidation method

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0032] 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:

[0033] In the presence of a water-containing solvent, the silicon source, the titanium source and the alkali source are mixed and then hydrothermally crystallized under airtight conditions to recover titanium-silicon molecular sieves; wherein, the hydrothermal crystallization goes through stage (1) and stage ( 2) and stage (3), stage (1) is crystallized at 80-120°C, stage (2) is heated to 180-220°C for crystallization, and stage (3) is cooled to 140-180°C for crystallization.

[0034]According to a preferr...

Embodiment approach

[0037] According to a preferred embodiment of the present invention, silicon source: titanium source: alkali source: the molar ratio of water is 100: (0.5-5): (10-50): (500-5000), preferably 100: (2 -4): (15-35): (1000-3000) Among them, the silicon source is SiO 2 Meter, titanium source as TiO 2 In terms of alkali source in N or OH - count.

[0038] According to the method of the present invention, the aqueous solvent basically contains water, and a co-solvent may also be added as required. In an embodiment of the present invention, the aqueous solvent is water.

[0039] In the present invention, the silicon source may be an inorganic silicon source and / or an organic silicon source.

[0040] Specifically, the organosilicon source can be, for example, one or more selected from the silicon-containing compounds shown in formula I,

[0041]

[0042] In formula I, R 1 , R 2 , R 3 and R 4 Each is C 1 -C 4 Alkyl groups, including C 1 -C 4 straight-chain alkyl and C 3 ...

Embodiment 1

[0090] Add 20 grams of silicon source tetraethyl orthosilicate to tetrapropyl ammonium hydroxide aqueous solution and stir to mix evenly, then add tetrabutyl titanate and mix evenly to obtain the molar composition: silicon source: titanium source: alkali source: Water = 100:2:15:1000 mixture. Put the mixture in a sealed stainless steel reaction kettle, raise the temperature of the kettle from room temperature to 100°C at a heating rate of 2°C / min and perform hydrothermal treatment at this temperature for 24 hours, and then raise the temperature of the kettle to 190°C at a heating rate of 15°C / min And hydrothermal treatment at this temperature for 6 hours; then reduce the temperature of the kettle to 170 °C at a cooling rate of 10 °C / min and hydrothermal treatment at this temperature for 48 hours, and finally cool down to room temperature and release the pressure, the product in the reactor is filtered, Washing, drying and calcination at 550° C. for 5 hours to obtain titanium s...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
particle diameteraaaaaaaaaa
particle diameteraaaaaaaaaa
particle diameteraaaaaaaaaa
Login to View More

Abstract

The invention belongs to the field of titanium silicon molecular sieve, and more specifically provides a titanium silicon molecular sieve, and a synthetic method and applications thereof. The titaniumsilicon molecular sieve is composed of crystal particles with a particle size ranging from 5 to 200nm via aggregation; the particle size of the titanium silicon molecular sieve ranges from 0.3 to 5<mu>m; the I960 / I550 value ranges from 0.7 to 0.85. The invention also provides a cyclic ketone oxidation method. The cyclic ketone oxidation method comprises a step of contact of cyclic ketone, and anoxidizing agent with a catalyst. The catalyst contains the titanium silicon molecular sieve. The crystal of the titanium silicon molecular sieve is high in I960 / I550 value, and is large in effective framework ti content. When the titanium silicon molecular sieve is used in oxidation reaction, the catalytic oxidation activity, and the reaction product selectivity are increased obviously, and excellent catalytic stability is achieved. The titanium silicon molecular sieve is capable of realizing aggregation of small crystal particles in crystallization growth process instead of simple physical aggregation of the small crystal particles, and micron order is achieved.

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] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. Among them, titanium-silicon molecular sieve TS-1 not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 zeolite. Titanium silicate molecular sieves are used as catalysts to catalyze various types of organic oxidation reactions, such as epoxidation of alkenes, partial oxidation of alkanes, oxidation of alcohols, hydroxylation of phenols, ammoxidation of cyclic ketones, etc. As a catalyst for the selective oxidation of organic matter, titanium-silicon molecular sieves are considered to be a milestone in the field of molecular sieve catalysis. [0003] However, according to the classic method such as the ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/00B01J29/89B82Y30/00
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products