# US 2018/0022720 A1 · Method for fabricating titanium-containing silicon oxide material and application of the same

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- Number: US 2018/0022720 A1
- Document ID: US20180022720A1
- Status: Published application
- Kind: A1
- Application number: 15/218,710
- Filed: 2016-07-25
- Published: 2018-01-25
- Earliest claimed: 2016-07-25
- Assignees: Oriental Union Chemical Corp.
- Applicants: Oriental Union Chemical Corp.
- Inventors: Yu-Chuan Hsu; Chia-Yao Tseng; Po-Sung Wu; Hsi-Chin Tsai
- Web page: https://patentgrep.com/patent/US20180022720A1

## CPC

- C07D 301/19: with organic hydroperoxides
- B01J 21/08: Silica
- B01J 37/0203: {the impregnation liquid containing organic compounds}
- B01J 37/0209: {involving a reaction between the support and a fluid}
- B01J 37/035: {Precipitation on carriers}
- B01J 37/0236: {Drying, e.g. preparing a suspension, adding a soluble salt and drying}
- C07D: HETEROCYCLIC COMPOUNDS (macromolecular compounds C08)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## 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

### Claim 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, 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):
xTiO2(1−x)SiO2 (I)
wherein x is a number within 0.002-0.2.

### Claim 2 (depends on 1)

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.

### Claim 3 (depends on 2)

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 including methyl alcohol, ethyl alcohol, isopropyl alcohol, butyl alcohol, and tert-butyl alcohol.

### Claim 4 (depends on 1)

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

### Claim 5 (depends on 4)

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

### Claim 6 (depends on 1)

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.

### Claim 7 (depends on 1)

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 %.

### Claim 8 (depends on 7)

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 %.

### Claim 9 (depends on 1)

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.

### Claim 10 (depends on 9)

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.

### Claim 11 (depends on 10)

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

### Claim 12 (depends on 9)

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.

### Claim 13 (depends on 12)

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.

### Claim 14 (depends on 9)

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.

### Claim 15 (depends on 14)

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.
