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Titanium-silicon molecular sieve catalyst as well as preparation method and application thereof

A titanium-silicon molecular sieve and catalyst technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of poor catalyst stability, uneven distribution of catalyst active centers, fast deactivation rate, etc. Production cost and cycle time, excellent selectivity and stability, effectiveness in solving mass transfer problems

Inactive Publication Date: 2016-11-16
JIANGSU RUICHEN CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the uneven distribution of catalyst active centers and poor surface hydrophobicity of Ti-HMS catalytic materials, when organic peroxides are used as oxidants for olefin epoxidation, the product yield is low, the catalyst stability is poor, and the deactivation rate is fast.

Method used

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  • Titanium-silicon molecular sieve catalyst as well as preparation method and application thereof
  • Titanium-silicon molecular sieve catalyst as well as preparation method and application thereof
  • Titanium-silicon molecular sieve catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] At room temperature and under stirring, add a mixed solution of silicon source tetraethyl orthosilicate, bis(triethoxysilyl)methane and trimethoxysilane, which accounts for 70% of the total amount to be added, to the template agent 16 Alkyltrimethylammonium bromide, mineralizer tetraethylammonium hydroxide and water mixed solution for hydrolysis to form a colorless and transparent solution I; the remaining 30% silicon source tetraethyl orthosilicate, di( Triethoxysilyl)methane and trimethoxysilane are mixed and then fully mixed with titanium source tetrabutyl titanate to form a mixed solution II; at -5°C and under rapid stirring, slowly add solution II to the solution In Ⅰ, a light yellow transparent solution was formed, and continued to stir for 1 hour, which was recorded as solution Ⅲ; solution Ⅲ was transferred to a stainless steel autoclave for crystallization treatment, the crystallization temperature was 140°C, and the crystallization time was 72 hours. Filter and...

Embodiment 2

[0032] Compared with Example 1, only in the molecular sieve preparation process, the amount of tetrabutyl titanate added was reduced. The composition relationship of the amount of each substance is [(CH 3 ) 3 CH 3 (CH 2 ) 15 N + ]Br - : [(CH 3 CH 2 ) 4 NH 4 ] + Oh - :Si(OC 2 h 5 ) 4 :(C 2 h 5 O) 3 Si-CH 2 -Si(OC 2 h 5 ) 3 : CH 3 Si(OCH 3 ) 3 :Ti(OC 4 h 9 ) 4 :H 2 O =0.3:0.4:1:0.3:0.1:0.03:10 (molar ratio).

[0033] The ultraviolet-visible (UV-Vis) spectrum of the titanium-silicon molecular sieve catalyst has a strong absorption peak around 215 nm, and no absorption peak exists at other wavelengths. Its infrared (FT-IR) spectrum is at 960cm -1 There is an obvious absorption peak. More than 95% of the pores have a pore size greater than 2 nm.

Embodiment 3

[0035] Compared with Example 1, only in the molecular sieve preparation process, reduce (C 2 h 5 O) 3 Si-CH 2 -Si(OC 2 h 5 ) 3 added amount. The composition relationship of the amount of each substance is [(CH 3 ) 3 CH 3 (CH 2 ) 15 N + ]Br - : [(CH 3 CH 2 ) 4 NH 4 ] + Oh - :Si(OC 2 h 5 ) 4 :(C 2 h 5 O) 3 Si-CH 2 -Si(OC 2 h 5 ) 3 : CH 3 Si(OCH 3 ) 3 :Ti(OC 4 h 9 ) 4 :H 2 O =0.3:0.4:1:0.2:0.1:0.04:10 (molar ratio).

[0036] The ultraviolet-visible (UV-Vis) spectrum of the titanium-silicon molecular sieve catalyst has a strong absorption peak around 215 nm, and no absorption peak exists at other wavelengths. Its infrared spectrum (FT-IR) is at 960cm -1 There is an obvious absorption peak. More than 95% of the pores have a pore size greater than 2 nm.

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Abstract

The invention relates to a titanium-silicon molecular sieve catalyst. The titanium-silicon molecular sieve catalyst is prepared from a silicon resource, a titanium source, a template agent, a mineralizer and a solvent, wherein the silicon resource is Si(OR1)4, (R2O)3Si-(CH2)n1-Si(OR3)3 and (R4)n2Si(OR5)4-n2; the titanium source is Ti(OR6)4; the template agent is [(CH3)3CH3(CH2)n3N<+>]X<->; the mineralizer is [(CH3Cn4H2n4)4NH4]<+>OH<->; the solvent is water; and hydrothermal crystallization is performed, so that the titanium-silicon molecular sieve catalyst with a composite hole structure and high hydrophobic characters is prepared. The titanium-silicon molecular sieve catalyst disclosed by the invention has the following advantages that the catalyst is simple in preparation process, and high in production efficiency; besides, a molecular sieve structure contains organic functional groups of Si-(CH2)n1-Si, Si-O-Si(R4)n2 and Ti-O-Si(R4)n2 and composite holes having hydrophobic characters and anti-carbon-deposition functions, so that the catalyst has excellent hydrophobic character and mass transfer performance, is high in activity and selectivity and good in stability, can be used in the process of producing corresponding epoxides from alkenes through epoxidation by using H2O2, ethylbenzene hydroperoxide, cumene hydroperoxide, tert-butyl hydroperoxide and the like as oxidizers.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a titanium-silicon molecular sieve catalyst and its preparation method and application. 2 ) n1 -Si, Si-O-Si(R 4 ) n2 and Ti-O-Si(R 4 ) n2 In situ assembly into titanium-silicon molecular sieve catalysts with composite pore structure. Background technique [0002] Titanium porous molecular sieve materials have good catalytic activity for the selective oxidation of hydrocarbons, the ammoxidation of ketones / aldehydes and the hydroxylation of aromatics, etc., and can be used as catalysts for olefin epoxidation and other reactions, and have broad industrial application prospects . [0003] After searching, the patent US4410501 disclosed the synthesis method of TS-1 molecular sieve for the first time. In the method, a titanium-silicon mixed colloid solution is prepared by using an aqueous solution of tetrapropylammonium hydroxide, an organic titanate and an organic silic...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07D303/04C07D301/12C07D301/19C01B39/04
CPCB01J29/89C01B39/04C07D301/12C07D301/19C07D303/04
Inventor 陈祥宋宇飞张勇郭鹏程
Owner JIANGSU RUICHEN CHEM
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