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An efficient titanium silicalite molecular sieve catalyst

A titanium-silicon molecular sieve and catalyst technology, used in molecular sieve catalysts, molecular sieves and alkali exchange compounds, physical/chemical process catalysts, etc., can solve the problems of poor catalyst stability, uneven distribution of catalyst active centers, and fast deactivation rate. Reduced production cost and cycle time, excellent selectivity and stability, more feasible and economical results

Inactive Publication Date: 2017-02-08
QINGDAO WINCHANCE TECH
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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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  • An efficient titanium silicalite molecular sieve catalyst
  • An efficient titanium silicalite molecular sieve catalyst
  • An efficient titanium silicalite molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 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. The crysta...

Embodiment 2

[0021] 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).

[0022] The ultraviolet-visible (UV-Vis) spectrum of the high-efficiency 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 larger than 2 nm.

Embodiment 3

[0024] 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).

[0025] The ultraviolet-visible (UV-Vis) spectrum of the high-efficiency 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 an efficient titanium silicalite molecular sieve catalyst. The catalyst comprises a silicon source, a titanium source, a template, a mineralizer and a solvent, wherein the silicon source is Si(OR1)4, (R2O)<3>Si-(CH2)<n1>-Si(OR3)<3> and (R4)<n2>Si(OR5)<4-n2>, the titanium source is Ti(OR6)4, the template is [(CH3)<3>CH<3>(CH2)<n3>N<+>]X<->, the mineralizer is [(CH3C<n4>H<2n4>)<4>NH<4>]<+>OH<->, and the solvent is a mixture of water and ethanol. The molecular sieve structure comprises hydrophobic and carbon-deposition-preventing organic functional groups and composite pores, and therefore the catalyst has excellent hydrophobicity and mass transfer performance, high activity, high selectivity and high stability, and the catalyst can be used for alkene epoxidation processes adopting H2O2, 1-hydroperoxyethylbenzene, cumene hydroperoxide, tert-butyl hydroperoxide, and the like as oxidants to produce corresponding epoxides.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a high-efficiency titanium-silicon molecular sieve catalyst, in particular to the hydrothermal crystallization method for combining four-coordination active titanium species and Si-(CH 2 ) n1 -Si, Si-O-Si(R 4 ) n2 and Ti-O-Si(R 4 ) n2 In situ assembly into highly efficient titanium-silicon molecular sieve catalysts with composite pore structures. 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 solutio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/88C01B39/08C07D301/19C07D303/04
CPCB01J29/88C01B39/085C07D301/19C07D303/04
Inventor 苏建丽
Owner QINGDAO WINCHANCE TECH
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