IP Library Granted Patent US 10,011,575
Granted Patent B2
US 10,011,575 · App. 15/218,710 · Granted Jul 3, 2018

Method for fabricating titanium-containing silicon oxide material and application of the same

Inventors: Yu-Chuan Hsu (Kaohsiung, TW); Chia-Yao Tseng (Kaohsiung, TW); Po-Sung Wu (Kaohsiung, TW); Hsi-Chin Tsai (Kaohsiung, TW)
Assignee: Oriental Union Chemical Corp.
C07D301/19B01J21/08B01J37/0236B01J37/04
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Quick Facts
Patent No.
US 10,011,575
App. No.
15/218,710
Granted
Jul 3, 2018
Kind
B2
Abstract

A method for fabricating a titanium-containing silicon oxide material and an application of the same are disclosed. The method needn't use a template but directly use an amorphous silicon dioxide and a titanium source as the reactants. The reactants are mixed with a solvent and react in the solvent. The suspension generated by the reaction is processed by solid-liquid separation, flushing and drying to obtain a titanium-containing silicon oxide material. The method features a simplified fabrication process and a low fabrication cost. The titanium-containing silicon oxide material fabricated by the method has a superior catalytic activity, able to catalyze an epoxidation reaction of an olefin-group compound to generate an epoxide.

Claims (24)

1. A method for fabricating a titanium-containing silicon oxide material, comprising steps:

preparing a mixture liquid containing an amorphous silicon dioxide, a titanium source and a solvent;

enabling a reaction of said mixture liquid without using a template, and undertaking a solid-liquid separation process; and

drying a solid-state material obtained in said solid-liquid separation process to obtain a titanium-containing silicon oxide material, wherein in an anhydrous state, said titanium-containing silicon oxide material is expressed by Formula (I):

x TiO 2 (1− x )SiO 2   (I)

wherein x is a number within 0.002-0.2.

2. The method according to claim 1 , wherein said amorphous silicon dioxide is smoked silica, fumed silica, silica gel, or silica sol; said titanium source is a titanate or an inorganic titanium source; said solvent is an alcohol-group compound.

3. The method according to claim 2 , wherein said titanate is selected from a group consisting of tetramethyl titanate, tetraethyl titanate, tetrapropyl orthotitanate, tetra isopropyl titanate, tetrabutyl orthotitanate, tetra sec-butyl titanate, tetrabutyl isotitanate, tetra tert-butyl titanate, and combinations thereof; said inorganic titanium source is titanium trichloride or titanium tetrachloride; said solvent is selected from a group consisting of methyl alcohol, ethyl alcohol, isopropyl alcohol, butyl alcohol, and tert-butyl alcohol.

4. The method according to claim 1 , wherein a molar ratio of titanium to silicon ranges from 0.002 to 0.2.

5. The method according to claim 4 , wherein a molar ratio of titanium to silicon ranges from 0.01 to 0.1.

6. The method according to claim 1 , wherein said reaction of said mixture liquid is undertaken at a temperature of 20-100° C. for 0.5-3 hours; said solid-state material obtained in said solid-liquid separation process is persistently dried at a temperature of 30-120° C. for 0.5-6 hours.

7. The method according to claim 1 further comprising at least one of following steps:

calcining said titanium-containing silicon oxide material at a temperature of 300-800° C. for 1-9 hours;

silylating said titanium-containing silicon oxide material at a temperature of 25-200° C. for 0.5-3 hours; and

incorporating a transition metal into said titanium-containing silicon oxide material, wherein a concentration of said transition metal in said titanium-containing silicon oxide material is within 0.01-10 wt %.

8. The method according to claim 7 , wherein said concentration of said transition metal in said titanium-containing silicon oxide material is within 0.05-5 wt %.

9. A method for fabricating an epoxide, comprising a steps:

providing said titanium-containing silicon oxide material fabricated according to claim 1 as a catalyst to enable a reaction of an olefin-group compound and an oxide to form an epoxide.

10. The method according to claim 9 , wherein said olefin-group compound is a mono-olefin compound, a di-olefin compound, or a poly-olefin compound; said oxide is an organic peroxide or a hydroperoxide.

11. The method according to claim 10 , wherein said mono-olefin compound is selected from a group consisting of ethylene, propylene, 1-butene, isobutene, 1-hexene, 2-hexene, 3-hexene, 1-octene, 1-decene, styrene, and cyclohexene; said di-olefin compound is butadiene or isoprene; said organic peroxide is ethylbenzene hydroperoxide, cumene hydroperoxide, tertiary butyl hydroperoxide, or cyclohexyl hydroperoxide.

12. The method according to claim 9 , wherein a molar ratio of said olefin-group compound to said oxide ranges from 1:100 to 100:1.

13. The method according to claim 12 , wherein said molar ratio of said olefin-group compound to said oxide ranges from 1:10 to 10:1.

14. The method according to claim 9 , wherein said reaction of said olefin-group compound and said oxide is undertaken for 1 minute-48 hours at a temperature of 0-200° C. and at a pressure of 1-100 atm.

15. The method according to claim 14 , wherein said reaction of said olefin-group compound and said oxide is undertaken for 5 minute-8 hours at a temperature of 25-150° C. and at a pressure of 1-100 atm.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 4, 2016
From: HSU, YU-CHUAN; TSENG, CHIA-YAO; WU, PO-SUNG; TSAI, HSI-CHIN
To: ORIENTAL UNION CHEMICAL CORP.
Reel/Frame 039343/0716 →
Continuity (1)
Related Publication 20180022720A1 · Jan 25, 2018