CN101407485A - Method for preparing ethylene polyamine by ammonolyzing dichloroethane with alcohol as medium - Google Patents
Method for preparing ethylene polyamine by ammonolyzing dichloroethane with alcohol as medium Download PDFInfo
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- CN101407485A CN101407485A CNA2008101774803A CN200810177480A CN101407485A CN 101407485 A CN101407485 A CN 101407485A CN A2008101774803 A CNA2008101774803 A CN A2008101774803A CN 200810177480 A CN200810177480 A CN 200810177480A CN 101407485 A CN101407485 A CN 101407485A
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- Prior art keywords
- dichloroethane
- ethylene polyamine
- aminolysis
- ammonia
- medium
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Abstract
The invention relates to the method field of manufacturing ethylene polyamine genera chemicla by aminolysis dichloroethane in alcohol medium. With current disclosed method for manufacturing ethylene polyamine by aminolysis dichloroethane, aminolysis dichloroethane is carried out with ammonia or ammonia water (namely, water is aminolysis medium) to directly obtain a mixture of ethylene polyamine hydrochloride and ammonium chloride; ethylene polyamine solution can be obtained only after the mixture is neutralized by sodium hydroxide; and azeotropic mixture is formed by water and ethylene dimine component in ethylene polyamine, thus bringing troubles for separation. Effective utilization of side product sodium chloride is difficult. The technical characteristics for manufacturing ethylene polyamine by aminolysis dichloroethane in alcohol medium are: aminolysis dichloroethane media is ethanol or normal propyl alcohol, thus directly obtaining ethylene polyamine without sodium hydroxide. The manufacturing process is simple, with little equipment, low investment and energy consumption, and side product sodium chloride can be effectively utilized.
Description
Ammonia is separated ethylene dichloride system ethyleneamines and is belonged to the chemical production field in the patent of the present invention alcohol medium.
Ammonia is separated the own disclosed manufacture method of ethylene dichloride system ethyleneamines all with the ammonia or its aqueous solution (being that water is that ammonia is separated medium).Because what this manufacture method obtained is the mixture of ethyleneamines hydrochloride and ammonium chloride, the mixture of ethyleneamines hydrochloride and ammonium chloride need with in the sodium hydroxide and after could get the aqueous solution of ethyleneamines, consume a large amount of sodium hydroxide, also can produce a large amount of sodium-chlor in the N-process, effectively utilize very difficult.Quadrol component and water in the ethyleneamines can form the azeotropic component, give and separate Tapes Come difficulty, cause the big energy consumption height of facility investment.
The purpose that ammonia is separated ethylene dichloride system ethyleneamines in the patent of the present invention alcohol medium is directly to obtain ethyleneamines.The sample separates easily, reduced investment, energy consumption are low, reduce material cost, and the side product sodium chloride purposes is wide.
Ammonia is separated the mechanism of ethylene dichloride system ethyleneamines and is in the patent of the present invention alcohol medium: the raw material ethylene dichloride of ammonolysis reaction, ammonia and product ethyleneamines all are dissolved in ethanol or n-propyl alcohol and product ammonium chloride is slightly soluble in ethanol, is insoluble in n-propyl alcohol, product ammonium chloride is constantly separated out the disengaging reaction system under the excessive condition of ammonia, so not only helps improving speed of response but also has realized separating of ethyleneamines and ammonium chloride.Quadrol component in the ethyleneamines does not have and ethanol or n-propyl alcohol form the possibility of azeotrope, and the ethanol of ethyleneamines or n-propyl alcohol solution can be told each component in ethanol or n-propyl alcohol and the ethyleneamines with the distillation technique of routine.The alcoholic acid latent heat of vaporization is that the latent heat of vaporization of 204.3cal/g, n-propyl alcohol is that the latent heat of vaporization of 163cal/g, water is 639cal/g, under the situation of identical ammonia mass concentration and identical ammonia and ethylene dichloride mol ratio, ammonia is separated ethylene dichloride system ethyleneamines and is Yaoed the method heat energy consumption that ammonia that the own disclosed water of Jiao Now is medium separates ethylene dichloride system ethyleneamines and reduce by 70% at least in the patent alcohol medium of the present invention.
Ammonia is separated the technical characterictic of ethylene dichloride system ethyleneamines and is in the patent of the present invention alcohol medium: the medium that ammonia is separated ethylene dichloride is ethanol or n-propyl alcohol.
Ammonia is separated the embodiment of ethylene dichloride system ethyleneamines and is in the patent of the present invention alcohol medium: ethanol or n-propyl alcohol, ethylene dichloride, ammonia are mixed into solution, ammonia mass concentration in the control ammonia alcoholic solution is that the mol ratio of 15-60%, ammonia and ethylene dichloride is 4-40, and the mass concentration height of ammonia helps reducing the generation that heat energy consumption, ammonia and ethylene dichloride mol ratio height help primary amine component in the ethyleneamines.Flow of Goods and Materials state when the time that ammonia is separated separates with ammonia, temperature, pressure are relevant, and the effective collision when promptly separating with ammonia between reactant is relevant.With deciding the ammonium chloride that chlorine method chemical examination ammonia parses, when the purity of ammonium chloride surpasses 99%, the chloride total amount of ammonium chloride separated out surpasses chloride total amount 95% Time of ethylene dichloride in the raw material, assert that ammonia is separated to finish.Divide the ammonium chloride of leaving away excess of ammonia and separating out after ammonia is separated and finished, ammonium chloride washs three times with 1/4 ethanol of measuring or the n-propyl alcohol of ammonium chloride amount at every turn.Merging filtrate and washings are lower than 116 ℃ of Xia Fen Evaporated in gas phase temperature and remove ethanol or n-propyl alcohol, by boiling point the each component Fen Evaporated in the ethyleneamines are come out then.Fen Evaporated residue washs the back burning disposal with the ethanol or the n-propyl alcohol of equivalent.Washings makes ethanol or n-propyl alcohol and isolated ammonia Ji ethanol that Fen Evaporated goes out or n-propyl alcohol are all made down the raw material usefulness that batch ammonia is separated.Ammonium chloride dealcoholysis oven dry back packing.
Claims (1)
1. ammonia is separated the technical characterictic of ethylene dichloride system ethyleneamines and is in the patent of the present invention alcohol medium: the medium that ammonia is separated ethylene dichloride is: ethanol or n-propyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101774803A CN101407485A (en) | 2008-11-26 | 2008-11-26 | Method for preparing ethylene polyamine by ammonolyzing dichloroethane with alcohol as medium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101774803A CN101407485A (en) | 2008-11-26 | 2008-11-26 | Method for preparing ethylene polyamine by ammonolyzing dichloroethane with alcohol as medium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101407485A true CN101407485A (en) | 2009-04-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101774803A Pending CN101407485A (en) | 2008-11-26 | 2008-11-26 | Method for preparing ethylene polyamine by ammonolyzing dichloroethane with alcohol as medium |
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| CN (1) | CN101407485A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2458913C1 (en) * | 2010-12-29 | 2012-08-20 | Открытое акционерное общество "Каустик" (ОАО "Каустик") | Method for ammonolysis of chlorohydrocarbons and method of purifying ammonium chloride separated from amine synthesis products |
| CN103130653A (en) * | 2011-11-22 | 2013-06-05 | 上海氯碱化工股份有限公司 | Method for continuous production of vinylamine by tubular reactor and device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101287701A (en) * | 2005-10-11 | 2008-10-15 | 巴斯夫欧洲公司 | Method for producing ethylene amines |
-
2008
- 2008-11-26 CN CNA2008101774803A patent/CN101407485A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101287701A (en) * | 2005-10-11 | 2008-10-15 | 巴斯夫欧洲公司 | Method for producing ethylene amines |
Non-Patent Citations (1)
| Title |
|---|
| 宗弘元: "乙二胺的生产技术与市场状况", 《精细石油化工进展》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2458913C1 (en) * | 2010-12-29 | 2012-08-20 | Открытое акционерное общество "Каустик" (ОАО "Каустик") | Method for ammonolysis of chlorohydrocarbons and method of purifying ammonium chloride separated from amine synthesis products |
| CN103130653A (en) * | 2011-11-22 | 2013-06-05 | 上海氯碱化工股份有限公司 | Method for continuous production of vinylamine by tubular reactor and device |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20090415 |