CN1775736A - Method for preparing sec-butylamine - Google Patents
Method for preparing sec-butylamine Download PDFInfo
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- CN1775736A CN1775736A CN 200510061485 CN200510061485A CN1775736A CN 1775736 A CN1775736 A CN 1775736A CN 200510061485 CN200510061485 CN 200510061485 CN 200510061485 A CN200510061485 A CN 200510061485A CN 1775736 A CN1775736 A CN 1775736A
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- butylamine
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Abstract
The invention relates to a method for preparing sec-butyl amine by continuous fixed bed solid phase catalysis, feeding raw materials sec-butyl alcohol, ammonia and hydrongen into a fixed bed reactor in the molar concentration of 1 to (1-5) to (2-6), and producing the sec-butyl amine by reacting under the action of catalyst, at temperature 110-180 deg.C, at pressure 1.0-2.0 MPa, and at airspeed 0.2-0.6h-1, where sec-butyl amine per ton consumes 0.4kg of catalyst. The effects of the invention: the invention uses Al and Ba containing denatured cobalt as catalyst and the sec-butyl alcohol conversion is up to 100%, and the sec-butyl amine yield can be up to 98.5%, higher than that of each of methyl alcohol aminating method and butylenes aminating method.
Description
Technical field
The present invention relates to a kind of preparation method of sec-butylamine, especially a kind ofly face the method that the hydrogen ammonification prepares sec-butylamine about sec-butyl alcohol.
Background technology
Sec-butylamine (sec-butylamine, di-sec-butylamine) is important organic chemical industry's intermediate, is widely used in agricultural chemicals, medicine, auxiliary chemicals, dyestuff, rubber industry etc.
The industrialized preparing process of sec-butylamine mainly contains: methylethylketone ammoniation process, butylene amination method.
According to document announcement: the methylethylketone ammoniation process is to be raw material with the methylethylketone, with Ni-Cr-HPO
3Make catalyzer, at 115 ℃ of temperature of reaction, air speed 0.15h
-1, raw material methylethylketone: hydrogen: sec-butylamine is produced in serialization under the condition of ammonia=1: 3.5: 4.5mol.The methylethylketone transformation efficiency is 98%, and the yield of sec-butylamine is lower, is about 90%.Its reaction velocity is relatively low, and under higher air speed condition, the yield of sec-butylamine is lower.Butylene amination method: make catalyzer with basic metal or alkalimetal oxide, by butylene and the direct amination of ammonia and get, the pressure of this process need 98Mpa, yield is on the low side, is about 29.4%.
Summary of the invention
The technical problem of solution required for the present invention is the lower defective of yield that overcomes existing technology long reaction time, severe reaction conditions, sec-butylamine, and a kind of method for preparing sec-butylamine is provided.This method is faced the hydrogen ammonification by sec-butyl alcohol and is generated sec-butylamine, has still to reach the high characteristics of sec-butylamine yield under reaction conditions gentleness, the reaction velocity conditions of higher.
The present invention solves the technical scheme that its technical problem adopts.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: this method for preparing sec-butylamine, adopt continuous fixed bed gas and solid phase catalytic, raw material sec-butyl alcohol: ammonia: hydrogen feeds fixed-bed reactor with molar concentration rate 1: 1～5: 2～6, under the effect of catalyzer, temperature of reaction is 110～180 ℃, and reaction pressure is 1.0～2.0Mpa, and reaction velocity is 0.2～0.6h
-1React the generation sec-butylamine under the condition, sec-butylamine product wherein per ton consumes the 0.4kg catalyzer.
In the technique scheme, the preferential scope of temperature of reaction is 120～170 ℃, is 1.2～1.8Mpa in the gauge pressure reaction pressure, and the preferential scope of reaction velocity is 0.25～0.55h
-1
In the technique scheme, described catalyzer is made up of carrier, active constituent Co and Al, Ba, and wherein active constituent shared weight percent in catalyzer is: 25%～60%; And active constituent Co: Al: Ba=1: 0.02: 0.05, all the other were carrier.Carrier can adopt at least a in silicon-dioxide, silicon oxide, the diatomite.
Employed method for preparing catalyst is as follows among the present invention:
At first with Al
2O
3Powder is heated to about 700 ℃ through the carrier of caustic soda compression leg moulding, and heats 3～4 hours under this temperature, make the aperture of carrier reach best, preparing a certain proportion of nitrate solution that contains cobalt, aluminium, palladium then, is under 30～40 ℃ the condition in temperature, dipping Al
2O
31～2 day time, carry out drying again, after the drying once more to Al
2O
3Be heated to 400 ℃, make the NO in the nitrate solution
2, NO etc. discharges, and uses H when using at last
2Reduce, promptly get the modified cobalt catalyst of Al, Ba.
Effect of the present invention is: using method of the present invention, face the hydrogen aminating reaction by sec-butyl alcohol, is catalyzer with the modification cobalt that contains Al, Ba, 110～180 ℃ of temperature of reaction, and under the condition of reaction pressure 1.0～2.0Mpa, reaction velocity 0.2～0.6h
-1, the sec-butyl alcohol transformation efficiency reaches 100%, and the sec-butylamine yield can reach 98.5%, yield height than document announcement first and second pure ammoniation processes in the past and these two kinds of technology system sec-butylamines of butylene amination method, the reaction conditions gentleness still can reach higher yield under the reaction velocity conditions of higher, has obtained effect preferably.
Embodiment
Below in conjunction with embodiment the present invention is further described.
[embodiment 1]
Adopt fixed-bed reactor, the reactor specification is 30 * 500mm, interior dress 45g modified cobalt catalyst, and active constituent is a cobalt in the catalyzer, promotor comprises Al, Ba, wherein with respect to the Co atomic ratio measuring, Co: Al: Ba=1: 0.02: 0.05.Raw material sec-butyl alcohol: ammonia: hydrogen is 1: 2.5: 5 with mol ratio, and 130 ℃ of temperature of reaction, reaction pressure is counted 1.5Mpa with gauge pressure, and reaction velocity is 0.45h
-1, the sec-butyl alcohol transformation efficiency is 98%, the sec-butylamine yield is 97.5% (weight).
[embodiment 2]
Each operation steps and condition according to embodiment 1.Just temperature of reaction is 145 ℃ in the reaction conditions, and reaction pressure is counted 1.4Mpa with gauge pressure, and reaction velocity is 0.3h
-1, the sec-butyl alcohol transformation efficiency is 99.5%, the sec-butylamine yield is 99.2% (weight).
[embodiment 3]
Each operation steps and condition according to embodiment 1.Change charging proportioning sec-butyl alcohol: ammonia: hydrogen=1: 3: 4.5, temperature of reaction is 160 ℃, and reaction pressure is counted 1.7Mpa with gauge pressure, and reaction velocity is 0.4h
-1, the sec-butyl alcohol transformation efficiency is 99%, the sec-butylamine yield is 99% (weight).
[embodiment 4]
Each operation steps and condition according to embodiment 1.Change charging proportioning raw material sec-butyl alcohol: ammonia: hydrogen=1: 3: 6, temperature of reaction is 175 ℃, and reaction pressure is counted 1.6Mpa with gauge pressure, and reaction velocity is 0.55h
-1, the sec-butyl alcohol transformation efficiency is 99.3%, the sec-butylamine yield is 99% (weight).
[comparative example 1]
Each operation steps and reaction conditions according to embodiment 1, embodiment 2, embodiment 3, embodiment 4.Just catalyzer is general cobalt catalyst, and reaction result is as follows:
| Proportioning (sec-butyl alcohol: ammonia: hydrogen) | 1∶2.5∶5 | 1∶2.5∶5 | 1∶3∶4.5 | 1∶3∶6 |
| Temperature of reaction ℃ | 130 | 145 | 160 | 175 |
| Reaction pressure Mpa | 1.5 | 1.4 | 1.7 | 1.6 |
| Reaction velocity h -1 | 0.45 | 0.3 | 0.4 | 0.55 |
| Sec-butyl alcohol transformation efficiency % | 90 | 89.5 | 90 | 91.3 |
| Sec-butylamine yield % | 90.5 | 90.2 | 91 | 92 |
Claims (6)
1, a kind of method for preparing sec-butylamine, it is characterized in that: by the raw material sec-butyl alcohol: ammonia: hydrogen is with molar concentration rate 1: 1～5: 2～6, and under the effect of catalyzer, temperature of reaction is 110～180 ℃, reaction pressure is 1.0～2.0Mpa, and reaction velocity is 0.2～0.6h
-1React the generation sec-butylamine under the condition, sec-butylamine product wherein per ton consumes the 0.4kg catalyzer.
2, the method for preparing sec-butylamine according to claim 1 is characterized in that: described catalyzer is made up of carrier, active constituent Co and Al, Ba, and wherein active constituent shared weight percent in catalyzer is: 25%-60%; And active constituent Co: Al: Ba=1: 0.02: 0.05, all the other were carrier.
3, according to the described method for preparing sec-butylamine of claim 1, it is characterized in that: temperature of reaction is 120～170 ℃.
4, according to the described method for preparing sec-butylamine of claim 1, it is characterized in that: in the gauge pressure reaction pressure is 1.2～1.8Mpa.
5, according to the described method for preparing sec-butylamine of claim 1, it is characterized in that: reaction velocity is 0.25～0.55h
-1
6, according to the described method for preparing sec-butylamine of claim 1, it is characterized in that: described carrier is at least a in silicon-dioxide, silicon oxide, the diatomite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510061485 CN1775736A (en) | 2005-11-08 | 2005-11-08 | Method for preparing sec-butylamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510061485 CN1775736A (en) | 2005-11-08 | 2005-11-08 | Method for preparing sec-butylamine |
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| Publication Number | Publication Date |
|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648874B (en) * | 2009-09-21 | 2012-09-05 | 浙江新化化工股份有限公司 | Method for separating sec-butylamine |
| CN114436859A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Method for preparing sec-butylamine through etherified C4 |
| CN114436827A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Method for coproducing ethylamine and sec-butylamine |
| CN114436826A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Method for preparing sec-butylamine through post-etherification C4 by supergravity method |
-
2005
- 2005-11-08 CN CN 200510061485 patent/CN1775736A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648874B (en) * | 2009-09-21 | 2012-09-05 | 浙江新化化工股份有限公司 | Method for separating sec-butylamine |
| CN114436859A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Method for preparing sec-butylamine through etherified C4 |
| CN114436827A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Method for coproducing ethylamine and sec-butylamine |
| CN114436826A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Method for preparing sec-butylamine through post-etherification C4 by supergravity method |
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Open date: 20060524 |