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Porous titanium silicalite molecular sieve, modified titanium silicalite molecular sieve, modified molecular sieve and preparation method and application thereof

A titanium-silicon molecular sieve and silicon molecular sieve technology, applied in the fields of modified titanium-silicon molecular sieve, modified molecular sieve and its preparation, and porous titanium-silicon molecular sieve, can solve the problems of unclear specific role of amorphous titanium species, and achieve improved catalytic performance, The effect of high specific surface area and high hydrophobicity

Pending Publication Date: 2022-08-05
SHANDONG HUALU HENGSHENG CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, framework titanium species have been widely confirmed to be active centers in catalytic oxidation reactions, while anatase TiO 2 The existence of just decomposes H 2 o 2 , but the specific role of amorphous titanium species is still unclear and there is great controversy

Method used

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  • Porous titanium silicalite molecular sieve, modified titanium silicalite molecular sieve, modified molecular sieve and preparation method and application thereof
  • Porous titanium silicalite molecular sieve, modified titanium silicalite molecular sieve, modified molecular sieve and preparation method and application thereof
  • Porous titanium silicalite molecular sieve, modified titanium silicalite molecular sieve, modified molecular sieve and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Embodiment 1: The preparation method of Ti-DMS titanium-silicon molecular sieve C is as follows:

[0067] (1) Preparation of the first mixed solution: Weigh 0.64g of cetyltrimethylammonium bromide, 0.4g of urea and 50ml of high-purity water, and stir for 30 minutes until the cetyltrimethylammonium bromide is completely dissolved, forming the first a mixture.

[0068] (2) Preparation of the second mixed solution: Measure 1.5 ml of n-pentanol, 3.6 ml of ethyl orthosilicate, 0.2 ml of tetrabutyl titanate and 50 ml of cyclohexane to form a second mixed solution after they are fully mixed.

[0069] (3) The second mixed solution was quickly poured into the first mixed solution, kept at 25°C, and stirred at 700 rpm for 30 minutes to form a stable microemulsion system.

[0070] (4) The microemulsion obtained in step (3) was transferred to an autoclave with a Teflon substrate, and then the autoclave was placed in an oven at 120° C. and allowed to stand for 12 hours. After the ...

Embodiment 2

[0071] Example 2: Ti-DMS alkali-modified C1

[0072]The Ti-DMS titanium-silicon molecular sieve C prepared in Example 1 was modified with a weak alkaline mixed solution. Pipette 3.5ml of organic base (N,N-dimethyldecylamine) into 100ml of high-purity water and stir for 1 hour, then weigh 3g of Ti-DMS titanium-silicon molecular sieve C and disperse it in the above solution and continue to stir for 80min until it is fully dispersed After homogenization, the above-mentioned emulsion was transferred to an autoclave, and heated at a high temperature for 48 hours under the reaction conditions of 120° C. in a static state. After the reaction was completed, the synthesized product was centrifuged at 2000 r / min for 20 min, washed with water and anhydrous ethanol for 3 times, and vacuum-dried in a vacuum drying box at 60 ° C for 12 hours to obtain the modified titanium-silicon molecular sieve C1. The diameter is 1.5μm, and the specific surface area is 680m 2 / g, the ratio of titanium ...

Embodiment 3

[0073] Example 3: Ti-DMS hydrophilic and hydrophobic modified C2

[0074] The Ti-DMS titanium-silicon molecular sieve C prepared in Example 1 was modified with a silane coupling agent. Put 1.5g of Ti-DMS titanium-silicon molecular sieve C and 1ml of silane coupling agent (trimethylchlorosilane) in 120ml of dry toluene, and under the protection of nitrogen with a purity of 99.9%, stir and reflux in an oil bath at 100 ° C for 12 hours . After the reaction is finished, it is cooled to room temperature, and centrifugal sedimentation is carried out (rotating speed is 2000r / min, time is 20min) to obtain modified molecular sieve C2, its particle size is 1.7 microns, and the specific surface area is 110 m 2 / g, the ratio of titanium to silicon is 3.6.

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Abstract

The invention relates to a porous titanium silicalite molecular sieve, a modified titanium silicalite molecular sieve, a modified molecular sieve and a preparation method and application thereof, and the preparation method of the porous titanium silicalite molecular sieve comprises the following steps: S1, uniformly mixing a template agent, organic amine and high-purity water to form a first mixed solution; s2, uniformly mixing organic alcohol, a silicon source, a titanium source and an organic solvent to form a second mixed solution; and S3, pouring the obtained second mixed solution into the obtained first mixed solution to form a stable microemulsion, and carrying out a reaction under a hydrothermal condition to obtain the micron-sized porous titanium silicalite molecular sieve. The obtained modified molecular sieve is used for catalyzing caprolactam industrial cyclohexanone ammoximation reaction. According to the method, a non-titanium framework in the molecular sieve can be effectively removed, the multilayer porous titanium silicalite molecular sieve with high specific surface area and high hydrophobicity is obtained, and meanwhile, the catalytic performance of ammoximation reaction is improved.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and specifically relates to a porous titanium-silicon molecular sieve, a modified titanium-silicon molecular sieve, a modified molecular sieve, and a preparation method and application thereof. Background technique [0002] In the early 1960s, molecular sieves began to be used as catalysts in the chemical industry due to their shape-selective catalysis characteristics. In 1972, Mobil Company developed the ZSM series of zeolite molecular sieves, ZSM-5 is one of the more important ones. In 1983, Taramasso and his collaborators in Italy successfully introduced Ti atoms instead of Al atoms into the ZSM-5 molecular sieve framework by isomorphic substitution, and synthesized a new molecular sieve TS-1, which is considered to be catalyzed by molecular sieves. A milestone, the isolated skeleton tetracoordinate titanium has excellent catalytic selective oxidation activity, and its industrial ...

Claims

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Application Information

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IPC IPC(8): C01B39/08C01B39/04B01J29/89B01J35/10C07C249/04C07C251/44
CPCC01B39/085C01B39/04B01J29/89C07C249/04C07C2601/14C01P2004/62C01P2004/61C01P2006/12C01P2004/03B01J35/617B01J35/615C07C251/44Y02P20/584
Inventor 常怀春宋望一张帅李春美杨光影
Owner SHANDONG HUALU HENGSHENG CHEM IND
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