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US 9,006,489 B2Granted
Method for pretreating and using copper-based catalyst
AssigneeJiangsu Sinorgchem Technology Co., Ltd.
InventorShiming Gao
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Abstract
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.
Claims40
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, and
- passivating the activated copper-based catalyst by reacting the activated copper-based catalyst with a ketone and a mixture comprising 4-aminodiphenylamine, said mixture made by a formanilide method, in presence of hydrogen at a temperature of about 100° C. to 180° C. and a hydrogen gas pressure of about 2 MPa to 6 MPa for about 20 to 40 hours, to obtain a passivated copper-based catalyst,
- wherein the mixture made by the formanilide method is prepared by
- reacting formic acid with aniline to form formanilide,
- reacting the formanilide with para-nitrochlorobenzene to form 4-nitrodiphenylamine, and
- reducing the 4-nitrodiphenylamine to the 4-aminodiphenylamine, optionally in presence of sodium sulfide as a reduction agent.
4 more elements
A method for pretreating a copper-based catalyst comprising
- dehydrating the copper-based catalyst at an elevated temperature,
- reducing the dehydrated copper-based catalyst with hydrogen to obtain an activated copper-based catalyst, and
- passivating the activated copper-based catalyst by reacting the activated copper-based catalyst with a compound comprising sulfur or a halogen in a mixture comprising 4-aminodiphenylamine, said mixture made by a nitrobenzene method, and a ketone in presence of hydrogen gas,
- wherein the passivation reaction is conducted in the mixture having a molar ratio of the 4-aminodiphenylamine made by the nitrobenzene method to the ketone at about (1:1) to (1:4);
- reaction temperature is about 100° C. to 180° C.;
- reaction time is about 20 to 40 hours;
- pressure of the hydrogen gas is about 2 MPa to 8 MPa, and
- wherein the mixture made by the nitrobenzene method is prepared by
- reacting aniline with nitrobenzene to make 4-nitrodiphenylamine and 4-nitrosodiphenylamine, and
- reducing the 4-nitrodiphenylamine and 4-nitrosodiphenylamine to the 4-aminodiphenylamine.
7 more elements
Dependencies are inferred from the claim text.