Titanium silicate molecular sieve catalyst comprising organic functional group

A titanium-silicon molecular sieve, organic functional group technology, applied in the direction of molecular sieve catalyst, molecular sieve compound, molecular sieve characteristic silicate, etc., can solve the problem of uneven distribution of catalyst active centers, poor catalyst stability, poor surface hydrophobicity, etc., to achieve excellent selectivity and stability, solving mass transfer problems, reducing production costs and production cycle effects

CN106315607AInactive Publication Date: 2017-01-11QINGDAO WINCHANCE TECH
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2017-01-11
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to a titanium silicate molecular sieve catalyst comprising an organic functional group. The titanium silicate molecular sieve catalyst comprises a silicon source, a titanium source, a template, a mineralizer and a solvent, wherein the silicon source 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 is [(CH3)3CH3(CH2)n3N<+>]X<->, the mineralizer is [(CH3Cn4H2n4)4NH4]<+>OH<->, and the solvent is a mixture of water and alcohol. As the structure of a molecular sieve comprises the hydrophobic anti-carbon organic functional group and a composite hole, the hydrophobicity and the mass transfer performance of the catalyst are excellent, the activity and the selectivity are high, the stability is good, and the catalyst is applied to production of a corresponding epoxide through alkene epoxidation, wherein H2O2, hydrogen peroxide, cumyl hydroperoxide and tert-butyl hydroperoxide are taken as oxidizing agents in the alkene epoxidation.
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Description

technical field

[0001] The invention belongs to the technical field of chemical industry and relates to a titanium-silicon molecular sieve catalyst containing an organic functional group. 2 ) n1 -Si, Si-O-Si(R 4 ) n2 and Ti-O-Si(R 4 ) n2 In situ assembly into organofunctional group-containing 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 solution is prepared by using an aqueous solution of tetrapropylammonium hydroxide, an organ...

Examples

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. Filter and...

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) spectrogram of the titanium-silicon molecular sieve catalyst containing organic functional groups has a strong absorption peak at about 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 titanium-silicon molecular sieve catalyst containing organic functional groups has a strong absorption peak at about 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.