Method for pretreating and using copper-based catalyst
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C07C-209/24
B01J-037/08
B01J-037/18
B01J-023/72
B01J-023/80
B01J-023/83
출원번호
US-0640016
(2015-03-05)
등록번호
US-9725403
(2017-08-08)
우선권정보
CN-2011 1 0151516 (2011-06-07)
발명자
/ 주소
Gao, Shiming
출원인 / 주소
Jiangsu Sinorgchem Technology Co., Ltd.
대리인 / 주소
Mei & Mark LLP
인용정보
피인용 횟수 :
0인용 특허 :
18
초록▼
Method for pretreating the copper-based catalyst having the steps of dehydrating the copper-based catalyst at an elevated temperature, reducing the dehydrated copper-based catalyst with hydrogen, and passivating the activated copper-based catalyst to obtain a catalyst suitable for N-alkylation. The
Method for pretreating the copper-based catalyst having the steps of dehydrating the copper-based catalyst at an elevated temperature, reducing the dehydrated copper-based catalyst with hydrogen, and passivating the activated copper-based catalyst to obtain a catalyst suitable for N-alkylation. The dehydration and reduction steps may be conducted simultaneously.
대표청구항▼
1. A method for pretreating a copper-based catalyst comprising dehydrating a copper-based catalyst at an elevated temperature,reducing the dehydrated copper-based catalyst with hydrogen to obtain an activated copper-based catalyst, andpassivating the activated copper-based catalyst to obtain a catal
1. A method for pretreating a copper-based catalyst comprising dehydrating a copper-based catalyst at an elevated temperature,reducing the dehydrated copper-based catalyst with hydrogen to obtain an activated copper-based catalyst, andpassivating the activated copper-based catalyst to obtain a catalyst suitable for N-alkylation by reacting with a sulfur- or halogen-containing compound,wherein the copper-based catalyst comprises about 10% to 70% copper oxide; andconcentration of the sulfur- or halogen-containing compound is about 1000 PPM to 10000 PPM for passivation; andthe sulfur- or halogen-containing compound is selected from the group consisting of carbon disulfide, chlorophenylamine, 2-mercaptobenzothiazole, thiophene, 2,4-dichloroaniline, and tetramethyl thiuram disulfide. 2. The method of claim 1, wherein the copper-based catalyst further comprises a carrier that is ZnO, Al2O3, SiO2, activated carbon, glass fiber net, ceramic ball, layered graphite, natural clay, cerium oxide, or a mixture thereof, and the carrier does not change its contents after the catalyst being pretreated. 3. The method of claim 1, wherein the copper-based catalyst is dehydrated at the elevated temperature of more than about 100° C. and under pressure of an inert gas at about 1 MPa to 5 MPa. 4. The method of claim 1, wherein the temperature is elevated at about 5° C. to 10° C. per hour during dehydration. 5. The method of claim 1, wherein the dehydrated copper-based catalyst is reduced with hydrogen in a liquid phase or a gas phase. 6. The method of claim 1, wherein the dehydrated copper-based catalyst is reduced at a temperature of about 110° C. to 280° C. and the hydrogen gas is fed at a volume concentration of about 0.1% to 100%. 7. The method of claim 1, wherein the temperature for reduction is elevated at about 1° C. to 15° C. per hour. 8. The method of claim 1, wherein the copper-based catalyst is dehydrated and reduced simultaneously. 9. The method of claim 1, wherein a ratio of the sulfur- or halogen-containing compound to the copper-based catalyst is about 0.05-1 mole per kilogram catalyst. 10. The method of claim 1, wherein the copper-based catalyst is passivated in a gas phase, and the sulfur- or halogen-containing compound is fed to the reaction with a carrier. 11. The method of claim 1, wherein the copper-based catalyst is passivated in a solution, and the sulfur- or halogen-containing compound is dissolved in an alcohol, ketone, or an amine solvent to form the solution for passivating the catalyst. 12. The copper-based catalyst pretreated by the method of claim 1. 13. The method for making alkylated derivatives of 4-aminodiphenylamine according to claim 1, comprising reacting 4-aminodiphenylamine with a ketone in presence of hydrogen and the copper-based catalyst pretreated by the method of claim 1. 14. The method of claim 13, wherein the reaction is conducted at a temperature of about 110° C. to 240° C. under a hydrogen pressure of about 2 MPa to 8 MPa. 15. The method of claim 13, wherein the reaction is conducted continuously, and a total feed amount of 4-aminodiphenylamine and ketone is about 10 to 25% by weight per hour of the weight of the catalyst.
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