CN105949066B - A kind of method of fat primary amine and fatty primary secondary amine in reduction fatty alkyl tertiary amine product - Google Patents
A kind of method of fat primary amine and fatty primary secondary amine in reduction fatty alkyl tertiary amine product Download PDFInfo
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- CN105949066B CN105949066B CN201610318906.7A CN201610318906A CN105949066B CN 105949066 B CN105949066 B CN 105949066B CN 201610318906 A CN201610318906 A CN 201610318906A CN 105949066 B CN105949066 B CN 105949066B
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- amine
- fatty
- brothers
- tertiary amine
- primary
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method of fat primary amine and fatty primary secondary amine in reduction fatty alkyl tertiary amine product, after the reaction of fatty alcohol one-step method terminates, paraformaldehyde is directly added in a kettle, special catalyst, hydrogen is passed through, is terminated after reacting 1h, you can be obvious to reduce brothers amine content in reactant.Compared with prior art, the present invention reaches the requirement of brothers amine content in tertiary amine product by the brothers amine content in adding specific medicament to reduce reactant after the completion of the reaction of fatty alcohol one-step method.The purpose of this method is to reduce brothers amine content excessive in reactant in the case where course of reaction control is bad, reach corresponding standard, or lower brothers amine content is further obtained by this method under conventional control, the fatty alkyl tertiary amine of more quality product matter is obtained, the value with popularization and application.
Description
Technical field
The present invention relates to fat primary amine and fat in a kind of chemical technology, more particularly to a kind of reduction fatty alkyl tertiary amine product
The method of fat secondary amine.
Background technology
Prior art is that fatty alcohol and dimethylamine normal pressure one-step method are reacted, and specific reaction mechanism and operation refer to text
Offer, wherein there are several details, i.e.,：Catalyst technology, this is the key entirely reacted, and it is related to activity and the selection of reaction
Property, catalyst is bad, and reactivity is low, reaction time length, and accessory substance is more；The disproportionation of dimethylamine, this is relevant with raw material dimethylamine,
Also it is relevant with the operation in course of reaction, such as reaction temperature, pressure etc., control it is good, the influence of dimethylamine disproportionation is just few, and it is most
Directly influence is exactly the generation of accessory substance i.e. fat primary amine and fatty primary secondary amine；Technology controlling and process in production process, using concentration
DCS control systems and advanced process equipment be reactor product quality guarantee.Existing fatty alcohol one is illustrated by Section 2
The thick tertiary amine that stage production technology reflects more or less contains certain accessory substance, and predominantly a certain amount of fat is primary, secondary
Amine and higher boiling product, the fatty brothers amine index request that the country is distilled in certified products tertiary amine are less than 0.7%, and high-class product requirement is more
Low, this requires that fatty brothers amine is more low better in the thick tertiary amine that reflects, but due to catalyst, diformazan in existing production technology
The generation that the reason fat brothers such as control in amine and production process amine can or can lack more, therefore a kind of, it is necessary to new side
Method is born.
The content of the invention
The purpose of the present invention is that to solve the above problems and provides fat in a kind of reduction fatty alkyl tertiary amine product
The method of fat primary amine and fatty primary secondary amine.
The present invention is achieved through the following technical solutions above-mentioned purpose：
The present invention method be：After the reaction of fatty alcohol one-step method terminates, paraformaldehyde is directly added in a kettle, it is special
Determine catalyst, be passed through hydrogen, terminate after reacting 1h, you can be obvious to reduce brothers amine content in reactant.
The beneficial effects of the present invention are：
The present invention is a kind of method of fat primary amine and fatty primary secondary amine in reduction fatty alkyl tertiary amine product, with prior art
Compare, the present invention is contained after the completion of the reaction of fatty alcohol one-step method by adding the brothers amine in specific medicament reduction reactant
Amount, reaches the requirement of brothers amine content in tertiary amine product.The purpose of this method is dropped in the case where course of reaction control is bad
Excessive brothers amine content in low reaction thing, reaches corresponding standard, or further pass through this method under conventional control
Lower brothers amine content is obtained, obtains the fatty alkyl tertiary amine of more quality product matter, the value with popularization and application.
Embodiment
The invention will be further described below：
The present invention method be：After the reaction of fatty alcohol one-step method terminates, paraformaldehyde is directly added in a kettle, it is special
Determine catalyst, be passed through hydrogen, terminate after reacting 1h, you can be obvious to reduce brothers amine content in reactant.
Case study on implementation 1：The thick tertiary amine (C12/14) that 400g reactions terminate, adds 5g formaldehyde, 1g catalyst, is passed through hydrogen pressure
Power scope is 0-1.0MPa, and at 120-200 DEG C of temperature, brothers amine content has 0.6% to be reduced in thick tertiary amine after 1 hour
0.05%；
Case study on implementation 2：The thick tertiary amine (C18/16) that 400g reactions terminate, adds 5g formaldehyde, 1g catalyst, is passed through hydrogen pressure
Power scope is 0-1.0MPa, and at 120-200 DEG C of temperature, brothers amine content has 0.5% to be reduced to 0.2% in thick tertiary amine after 1 hour；
Case study on implementation 3：The thick tertiary amine (C12/14) that 5 tons of reactions terminate, 10 ㎏ formaldehyde are added, 1Kg catalyst, are passed through hydrogen
Pressure limit is 0-1.0MPa, and at 120-200 DEG C of temperature, brothers amine content has 0.6% to be reduced in thick tertiary amine after 1 hour
0.2%；
Case study on implementation 4：The thick tertiary amine (C18/16) that 15 tons of reactions terminate, 25g formaldehyde is added, 1Kg catalyst, is passed through hydrogen
Pressure limit is 0-1.0MPa, and at 120-200 DEG C of temperature, brothers amine content has 0.6% to be reduced in thick tertiary amine after 1 hour
0.2%；
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (1)
1. a kind of method of fat primary amine and fatty primary secondary amine in reduction fatty alkyl tertiary amine product, it is characterised in that：In fatty alcohol
After one-step method reaction terminates, paraformaldehyde is directly added in a kettle, special catalyst, is passed through hydrogen, is terminated after reacting 1h,
It can obviously reduce brothers amine content in reactant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610318906.7A CN105949066B (en) | 2016-05-12 | 2016-05-12 | A kind of method of fat primary amine and fatty primary secondary amine in reduction fatty alkyl tertiary amine product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610318906.7A CN105949066B (en) | 2016-05-12 | 2016-05-12 | A kind of method of fat primary amine and fatty primary secondary amine in reduction fatty alkyl tertiary amine product |
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| Publication Number | Publication Date |
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| CN105949066A CN105949066A (en) | 2016-09-21 |
| CN105949066B true CN105949066B (en) | 2017-12-15 |
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| CN201610318906.7A Active CN105949066B (en) | 2016-05-12 | 2016-05-12 | A kind of method of fat primary amine and fatty primary secondary amine in reduction fatty alkyl tertiary amine product |
Country Status (1)
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816072A (en) * | 2011-06-09 | 2012-12-12 | 烟台万华聚氨酯股份有限公司 | Preparation method and application of N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine |
-
2016
- 2016-05-12 CN CN201610318906.7A patent/CN105949066B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816072A (en) * | 2011-06-09 | 2012-12-12 | 烟台万华聚氨酯股份有限公司 | Preparation method and application of N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine |
Non-Patent Citations (4)
| Title |
|---|
| Dimitra Kovala-Demertzi etal.RANEY® nickel-catalyzed reductive N-methylation of amines with paraformaldehyde: theoretical and experimental study.《RSC Advances》.2011,第4卷20140829. * |
| 烷基二甲基胺的研制;张建生;《河北化工》;19941231(第3期);第42-46页 * |
| 脂肪胺的生产与应用;孙在海;《中氮肥》;19911231(第2期);第27页 * |
| 脂肪醇常压一步法制叔胺新工艺的开发;冯正诗;《精细化工》;19871231;第4卷;第45页 * |
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| CN105949066A (en) | 2016-09-21 |
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