CN105949066A - Method for reducing fatty primary amine and fatty secondary amine in fatty alkyl tertiary amine product - Google Patents
Method for reducing fatty primary amine and fatty secondary amine in fatty alkyl tertiary amine product Download PDFInfo
- Publication number
- CN105949066A CN105949066A CN201610318906.7A CN201610318906A CN105949066A CN 105949066 A CN105949066 A CN 105949066A CN 201610318906 A CN201610318906 A CN 201610318906A CN 105949066 A CN105949066 A CN 105949066A
- Authority
- CN
- China
- Prior art keywords
- amine
- fatty
- content
- secondary amine
- product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for reducing fatty primary amine and fatty secondary amine in a fatty alkyl tertiary amine product. After a one-step reaction of fatty alcohol ends, paraformaldehyde and a specific catalyst are directly added to a reaction kettle, hydrogen is introduced, and the content of primary amine and secondary amine in a reactant can be remarkably reduced after the mixture reacts for 1 h. Compared with the prior art, the content of primary amine and secondary amine in the reactant can be reduced by adding a specific chemical after the one-step reaction of fatty alcohol ends, and the requirements for the content of primary amine and secondary amine in a tertiary amine product are met. The method aims to reduce the content of excessive primary amine and secondary amine in the reactant under the condition that the reaction process is poorly controlled, corresponding standards are met or the content of primary amine and secondary amine can be reduced with the method under the conventional control, high-quality fatty alkyl tertiary amine is obtained, and the method has popularization and application value.
Description
Technical field
The present invention relates to a kind of chemical technology, particularly relate to fat primary in a kind of reduction fatty alkyl tertiary amine product
Amine and the method for fatty primary secondary amine.
Background technology
Prior art is fatty alcohol and the reaction of dimethylamine normal pressure one-step method, and concrete reaction mechanism can with operation
List of references, wherein has several details, it may be assumed that catalyst technology, and this is the key of whole reaction, its relation
To the activity and selectivity of reaction, catalyst is bad, and reactivity is low, and the response time is long, and by-product is many；
The disproportionation of dimethylamine, this is relevant with raw material dimethylamine, also relevant with the operation in course of reaction, such as reaction temperature
Degree, pressure etc., control good, the impact of dimethylamine disproportionation is the fewest, and it the most directly affects is exactly by-product
I.e. fat primary amine and the generation of fatty primary secondary amine；Technology controlling and process in production process, uses the DCS concentrated to control
System and advanced process equipment are the guarantees of reactor product quality.By Section 2, existing fatty alcohol one is described
The thick tertiary amine that stage production technology reflects the most more or less contains certain by-product, the most a certain amount of
The primary, secondary amine of fat and high boiling point product, the fatty brothers amine index request in domestic distillation certified products tertiary amine is little
In 0.7%, high-class product requires lower, and this will ask fat brothers amine in the thick tertiary amine reflected the lowest more good,
But due to reason fat such as the controls in catalyst, dimethylamine and production process in existing production technology
The generation how brothers amine all can or can lack, accordingly, it would be desirable to a kind of new method is born.
Summary of the invention
The purpose of the present invention is that providing a kind of to solve the problems referred to above reduces fatty alkyl tertiary amine product
Middle fat primary amine and the method for fatty primary secondary amine.
The present invention is achieved through the following technical solutions above-mentioned purpose:
The method comprise the steps that after the reaction of fatty alcohol one-step method terminates, add poly the most in a kettle.
Formaldehyde, special catalyst, it is passed through hydrogen, terminates after reaction 1h, i.e. can obviously reduce brothers amine in reactant
Content.
The beneficial effects of the present invention is:
The present invention is a kind of to reduce the method for fat primary amine and fatty primary secondary amine in fatty alkyl tertiary amine product, with existing
Having technology to compare, the present invention reduces reaction by the specific medicament of addition after fatty alcohol one-step method has been reacted
Brothers amine content in thing, reaches the requirement of brothers amine content in tertiary amine product.The purpose of this method is instead
Brothers amine content too much in reactant is reduced so that it is reach to mark accordingly in the case of answering process control the best
Standard, or obtain lower brothers amine content by this method further under conventional control, obtain more quality product matter
Fatty alkyl tertiary amine, there is the value of popularization and application.
Detailed description of the invention
The invention will be further described below:
The method comprise the steps that after the reaction of fatty alcohol one-step method terminates, add poly the most in a kettle.
Formaldehyde, special catalyst, it is passed through hydrogen, terminates after reaction 1h, i.e. can obviously reduce brothers amine in reactant
Content.
The thick tertiary amine (C12/14) that case study on implementation 1:400g reaction terminates, addition 5g formaldehyde, 1g catalyst,
Being passed through Hydrogen Vapor Pressure scope is at 0-1.0MPa, temperature 120-200 DEG C, and after 1 hour, in thick tertiary amine, brothers amine contains
Amount has 0.6% to be reduced to 0.05%；
The thick tertiary amine (C18/16) that case study on implementation 2:400g reaction terminates, addition 5g formaldehyde, 1g catalyst,
Being passed through Hydrogen Vapor Pressure scope is at 0-1.0MPa, temperature 120-200 DEG C, and after 1 hour, in thick tertiary amine, brothers amine contains
Amount has 0.5% to be reduced to 0.2%；
The thick tertiary amine (C12/14) that the reaction of case study on implementation 3:5 ton terminates, adds 10 formaldehyde, and 1Kg is catalyzed
Agent, being passed through Hydrogen Vapor Pressure scope is at 0-1.0MPa, temperature 120-200 DEG C, brothers in thick tertiary amine after 1 hour
Amine content has 0.6% to be reduced to 0.2%；
The thick tertiary amine (C18/16) that the reaction of case study on implementation 4:15 ton terminates, adds 25g formaldehyde, and 1Kg is catalyzed
Agent, being passed through Hydrogen Vapor Pressure scope is at 0-1.0MPa, temperature 120-200 DEG C, brothers in thick tertiary amine after 1 hour
Amine content has 0.6% to be reduced to 0.2%；
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.The industry
Skilled person will appreciate that, the present invention is not restricted to the described embodiments, in above-described embodiment and description
The principle that the present invention is simply described described, without departing from the spirit and scope of the present invention, the present invention
Also having various changes and modifications, these changes and improvements both fall within scope of the claimed invention.This
The claimed scope of invention is defined by appending claims and equivalent thereof.
Claims (1)
1. reducing fat primary amine and a method for fatty primary secondary amine in fatty alkyl tertiary amine product, its feature exists
In: after the reaction of fatty alcohol one-step method terminates, add paraformaldehyde the most in a kettle., special catalyst,
It is passed through hydrogen, terminates after reaction 1h, i.e. 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105949066A true CN105949066A (en) | 2016-09-21 |
| CN105949066B CN105949066B (en) | 2017-12-15 |
Family
ID=56912446
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| 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)
| Country | Link |
|---|---|
| CN (1) | CN105949066B (en) |
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 (5)
| Title |
|---|
| DIMITRA KOVALA-DEMERTZI ETAL: "RANEY® nickel-catalyzed reductive N-methylation of amines with paraformaldehyde: theoretical and experimental study", 《RSC ADVANCES》 * |
| 冯正诗: "脂肪醇常压一步法制叔胺新工艺的开发", 《精细化工》 * |
| 孙在海: "脂肪胺的生产与应用", 《中氮肥》 * |
| 张建生: "烷基二甲基胺的研制", 《河北化工》 * |
| 朱彬: "《有机合成》", 31 January 2014 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105949066B (en) | 2017-12-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108840789B (en) | Method for synthesizing and producing ethylene glycol mono-tert-butyl ether | |
| CN105330836B (en) | A kind of synthetic method of epoxy terminated allyl alcohol polyethenoxy ether | |
| TWI579266B (en) | Method for preparing glycol ester using reactive distillation | |
| IL262406A (en) | Method for preparing azoxystrobin intermediates | |
| MY145831A (en) | A method for the production of dimethyl ether | |
| CN100586942C (en) | Production method of dioxane | |
| CN107641084B (en) | Method for producing nitroalkane and co-producing ketoxime | |
| CN103333042B (en) | A kind of preparation method of amylene | |
| CN102557905A (en) | Clean production process for pinacoline | |
| CN105949066A (en) | Method for reducing fatty primary amine and fatty secondary amine in fatty alkyl tertiary amine product | |
| CN105967978A (en) | Isomerization synthesis of 3-methyl-2-buten-1-ol using water-containing methyl butenol | |
| CN103804160A (en) | Preparation method of 3-methyl-3-amylene-2-ketone | |
| CN109867587B (en) | Preparation method of 3-chloro-1,2-propanediol | |
| MX2020012884A (en) | Hmf preparation catalysed by anolyte fraction. | |
| JP4827473B2 (en) | Method for producing ammonium lactate | |
| CN110862296B (en) | Method for separating reaction product in chloromethane production process | |
| CN108117479A (en) | A kind of preparation method of 1,10- decanediols | |
| EP2900647B1 (en) | Continuous process for producing epichlorohydrin from dichlorohydrins | |
| CN110818538A (en) | Na-NaOH/gamma-Al2O3Method for catalytic synthesis of anisole | |
| CN107573223B (en) | Method for producing tetraethyl orthocarbonate by efficient rectification | |
| CN104120039A (en) | Method for preparing fatty acid methyl ester through multi-stage ester exchange | |
| CN113943210B (en) | Non-translocated six-carbon alcohol translocation method | |
| JP4463627B2 (en) | Method for producing triethylene glycol divinyl ether | |
| CN100360232C (en) | Highly active solid catalyst for preparing ketal and application thereof | |
| CN104326890B (en) | A kind of Carroll reacts continuous process method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |