CN101265196B - Method of synthesizing monoisopropanolamine - Google Patents
Method of synthesizing monoisopropanolamine Download PDFInfo
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- CN101265196B CN101265196B CN2008100240531A CN200810024053A CN101265196B CN 101265196 B CN101265196 B CN 101265196B CN 2008100240531 A CN2008100240531 A CN 2008100240531A CN 200810024053 A CN200810024053 A CN 200810024053A CN 101265196 B CN101265196 B CN 101265196B
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Abstract
The invention relates to a synthesis method of isopropanolamine. The synthesis method comprises the following steps: (1) liquid ammonia and water are mixed to form ammonia water which is mixed with propylene oxide; mixed solution is preheated until the temperature reaches 120 to 125 DEG C, and the inputting molar ratio of the ammonia and the propylene oxide is controlled within 10 to 15; (2) the materiel after preheating is delivered into a reactor, the reaction temperature ranges from 128 to 138 DEG C, the pressure ranges from 12.6 to 13.8MPa, and the reaction time ranges from 1.5 to 3 hours; (3) the surplus unreacted ammonia is separated from the obtained mixture after the reaction by using a flash distillation column, the pressure in the flash distillation column ranges from 0.6 to 1.6MPa, and the temperature of a column kettle ranges from 140 to 160 DEG C; (4) the mixture which is separated through the flash distillation column is delivered into a leading tower for rectification dehydration, the pressure in the leading tower ranges from minus 0.080 to minus 0.085MPa, the temperature at the top of the leading tower is 45 to 55 DEG C, and the temperature at the bottom in a tower kettle ranges from 110 to 130 DEG C; (5) the mixture after dehydration is delivered into a rectification column for rectification, the pressure in the rectification column ranges from minus 0.095 to minus 0.099MPa, the temperature in the column kettle ranges from 135 to 160 DEG C, the temperature at the top of the rectification column ranges from 60 to 70 DEG C, isopropanolamine products are obtained at the top of the rectification column, and the mixture composed of diisopropanolamine and triisopropanolamine is obtained in the column kettle. The synthesis method has simple production procedure, little equipment investment, and high product quality.
Description
Technical field
The present invention relates to a kind of synthetic method of a Yi Bingchunan.
Technical background
One Yi Bingchunan is 1-amino-2-propyl alcohol (chemical formula: CH
3CH (OH) CH
2NH
2) be commonly called as, claim monoisopropanolamine again.One Yi Bingchunan has purposes widely: can be used for household chemicalss such as washing agent, liquid washing agent, shampoo; Can be used for fabric, wool spinning, leather agent; Can be used for metal electron liquid crystal, semi-conductive clean-out system; Can be used for synthesizing of medicine, agricultural chemicals and essence and flavoring agent intermediate etc.
The method of present industrial production one Yi Bingchunan is to be raw material petrohol amine series mixture with ammoniacal liquor or liquefied ammonia and propylene oxide mostly, isolates a Yi Bingchunan, diisopropanolamine (DIPA), three kinds of products of tri-isopropanolamine more step by step.A Yi Bingchunan that adopts this method to produce contains the above isomers 2-amino-1-propyl alcohol of 3% (quality percentage composition, butt) usually, and (chemical formula is: CH
3CH (NH2) CH
2OH), this isomer can generate the chemical substance of no drug effect when synthetic medicine or pesticide intermediate, sometimes even the chemical substance of generation toxic side effect.Therefore, the Yi Bingchunan that existing method is produced can not be directly used in synthetic medicine or pesticide intermediate, two kinds of isomers 1-amino-2-propyl alcohol in the one Yi Bingchunan product need be separated with 2-amino-1-propyl alcohol again, obtain high purity (〉=99%, mass ratio) 1-amino-2-propyl alcohol just can be used for synthetic medicine or pesticide intermediate.But, these two kinds the isolating difficulty of isomers is big, energy consumption is high with its isomers 2-amino-1-propyl alcohol for 1-amino-2-propyl alcohol, and complex technical process, processing condition harshness, then bigger in the industrial difficulty that they are separated, not only need to increase new installation, and process cost is also very big.
Summary of the invention
The technical problem to be solved in the present invention is exactly existing method synthetic 1-amino-2-propyl alcohol isometry body burden higher (more than 3%), can not be directly used in the problem of synthetic medicine and pesticide intermediate, a kind of synthetic method of new 1-amino-2-propyl alcohol is provided, directly isomers is controlled in 1% at synthesis phase, thereby makes product one Yi Bingchunan (1-amino-2-propyl alcohol) can satisfy the high-end needs of products such as synthetic medicine, agricultural chemicals, essence, spices.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
1) liquefied ammonia and water are made into ammoniacal liquor, mix with propylene oxide (being called for short PO), be preheated to 120-125 ℃ then, the molar ratio of ammonia and propylene oxide is controlled at 10-15;
2) material after the preheating is sent into reactor and react, temperature is controlled at 128-138 ℃ during reaction, and pressure-controlling was reacted 1.5-3 hour at 12.6-13.8Mpa;
3) mixture that obtains after will reacting is isolated unnecessary unreacted ammonia with flashing tower, and the flashing tower pressure-controlling is at 0.6-1.6Mpa, and tower still temperature is controlled at 140-160 ℃;
4) will send into dehydration tower through the mixture that flashing tower separated and carry out rectifying and dewatering, the dehydration tower pressure-controlling-0.080～-0.085Mpa, tower top temperature is controlled at 45～55 ℃, tower still temperature is controlled at 110-130 ℃, behind the rectifying tower stable operation, cat head is sloughed moisture content, and the dehydration tower still obtains the Yi Bingchunan mixture;
5) mixture after will dewatering is sent into fractionate and is carried out rectifying, the fractionate pressure-controlling-0.095～-0.099Mpa, tower still temperature is controlled at 135-160 ℃, tower top temperature is controlled at 60～70 ℃, cat head promptly gets a Yi Bingchunan product, the tower still obtain two, the mixture of tri-isopropanolamine.
Above-mentioned ammoniacal liquor is formulated by liquefied ammonia and deionized water, and wherein the mass content of water is 6-8%.
The present invention is on the basis of existing installation, adjustment and control by technological parameter, 1-amino in the Yi Bingchunan product that makes-2-propyl alcohol composition accounts for more than 99% (mass percent), and its isomers 2-amino-1-propyl alcohol can satisfy the high-end needs of products such as synthetic medicine, agricultural chemicals, essence, spices below 1%.And production process of the present invention is simple relatively, the equipment less investment, and the production operation expense is few, and production cost is low, the product quality height.
Embodiment
Embodiment 1
With 4650kg liquefied ammonia and 350kg deionized water thorough mixing, form ammoniacal liquor (water accounts for 7%) and use the high pressure measurement pump delivery, again with behind another high pressure measurement pump delivery 1322kg ring third and the ammoniacal liquor thorough mixing, enter preheater, be preheated to 120 ℃, enter temperature of reactor then and be controlled at 130-132 ℃, pressure-controlling is at 12.9-13.0Mpa, react after 2.5 hours, the mix product that reaction obtains is introduced into flashing tower, pressure-controlling is at 1.0Mpa, tower still temperature is controlled at 155-158 ℃, the recovered overhead excess of ammonia, flashing tower still material, enter the dehydration tower dehydration, the dehydration tower pressure-controlling is at-0.082Mpa, tower top temperature is controlled at 53～54 ℃, tower still temperature is controlled at 118-120 ℃, the Yi Bingchunan mixture that the dehydration tower still obtains enters a Yi Bingchunan rectifying tower (be called for short down a different tower) pressure-controlling at-0.097Mpa, tower still temperature is controlled at 154～155 ℃, tower top temperature is controlled at 69～70 ℃, and cat head gained one Yi Bingchunan product 1-amino-2-propyl alcohol composition after testing accounts for 99.33%, and 2-amino-1-propyl alcohol composition accounts for 0.67%.
Embodiment 2
With 4300kg liquefied ammonia and 280kg deionized water thorough mixing, form ammoniacal liquor (water accounts for 6.5%) and use the high pressure measurement pump delivery, again with behind another high pressure measurement pump delivery 1145kg ring third and the ammoniacal liquor thorough mixing, enter preheater, be preheated to 122 ℃, enter temperature of reactor then and be controlled at 134-137 ℃, pressure-controlling is reacted after 2 hours at 13.5-13.6Mpa, and the mix product that reaction obtains is introduced into flashing tower, pressure-controlling is at 1.2Mpa, tower still temperature is controlled at 156-158 ℃, reclaims excess of ammonia, flashing tower still material, enter the dehydration tower dehydration, the dehydration tower pressure-controlling is at-0.085Mpa, and tower top temperature is controlled at 46～47 ℃, and tower still temperature is controlled at 115-118 ℃, the Yi Bingchunan mixture that the dehydration tower still obtains enters a different tower, one different pressure tower is controlled at-0.098Mpa, and tower still temperature is controlled at 148-150 ℃, and tower top temperature is controlled at 66～67 ℃, cat head gained one Yi Bingchunan product 1-amino-2-propyl alcohol composition after testing accounts for 99.55%, and 2-amino-1-propyl alcohol composition accounts for 0.45%.
Embodiment 3
With 4610kg liquefied ammonia and 410kg deionized water thorough mixing, form ammoniacal liquor (water accounts for 8%) and use the high pressure measurement pump delivery, again with behind another high pressure measurement pump delivery 1426kg ring third and the ammoniacal liquor thorough mixing, enter preheater, be preheated to 123 ℃, enter temperature of reactor then and be controlled at 130 ℃, pressure, reacts after 1.8 hours at 12.9Mpa with only, and the mix product that reaction obtains is introduced into flashing tower, pressure-controlling is at 0.9Mpa, tower still temperature is controlled at 153-155 ℃, reclaims excess of ammonia, flashing tower still material, enter the dehydration tower dehydration, pressure-controlling is at-0.085Mpa, and tower top temperature is controlled at 46～47 ℃, and tower still temperature is controlled at 116-118 ℃, the Yi Bingchunan mixture that the dehydration tower still obtains enters a different tower, one different pressure tower is controlled at-0.099Mpa, and tower still temperature is controlled at 147-150 ℃, and tower top temperature is controlled at 65～66 ℃, cat head gained one Yi Bingchunan product 1-amino-2-propyl alcohol composition after testing accounts for 99.11%, and 2-amino-1-propyl alcohol composition accounts for 0.89%.
Claims (3)
1. the synthetic method of a Yi Bingchunan is characterized in that comprising the steps:
1) liquefied ammonia and water are made into ammoniacal liquor, mix with propylene oxide, be preheated to 120-125 ℃ then, the molar ratio of ammonia and propylene oxide is controlled at 10-15;
2) material after the preheating is sent into reactor and react, temperature is controlled at 128-138 ℃ during reaction, and pressure-controlling was reacted 1.5-3 hour at 12.6-13.8Mpa;
3) mixture that obtains after will reacting is isolated unnecessary unreacted ammonia with flashing tower, and the flashing tower pressure-controlling is at 0.6-1.6Mpa, and tower still temperature is controlled at 140-160 ℃;
4) will send into dehydration tower through the mixture that flashing tower separated and carry out rectifying and dewatering, the dehydration tower pressure-controlling-0.080～-0.085Mpa, tower top temperature is controlled at 45～55 ℃, tower still temperature is controlled at 110-130 ℃, cat head is sloughed moisture content, and the dehydration tower still obtains the Yi Bingchunan mixture;
5) mixture after will dewatering is sent into fractionate and is carried out rectifying, the fractionate pressure-controlling-0.095～-0.099Mpa, tower still temperature is controlled at 135-160 ℃, tower top temperature is controlled at 60～70 ℃, cat head promptly gets a Yi Bingchunan product, the tower still obtain two, the mixture of tri-isopropanolamine.
2. the synthetic method of a Yi Bingchunan according to claim 1, the mass content that it is characterized in that water in the ammoniacal liquor is 6-8%.
3. the synthetic method of a described as claimed in claim 1 or 2 Yi Bingchunan is characterized in that described water is deionized water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100240531A CN101265196B (en) | 2008-04-23 | 2008-04-23 | Method of synthesizing monoisopropanolamine |
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|---|---|---|---|
| CN2008100240531A CN101265196B (en) | 2008-04-23 | 2008-04-23 | Method of synthesizing monoisopropanolamine |
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| CN101265196A CN101265196A (en) | 2008-09-17 |
| CN101265196B true CN101265196B (en) | 2011-05-04 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102702000A (en) * | 2012-06-27 | 2012-10-03 | 淄博德信联邦化学工业有限公司 | Preparation method of triisopropanolamine |
| CN104961641B (en) * | 2015-07-15 | 2016-11-16 | 河北工业大学 | A kind of reactive distillation produces the method for monoisopropanolamine |
| CN108947852A (en) * | 2018-07-16 | 2018-12-07 | 南京红宝丽聚氨酯有限公司 | A kind of preparation method of 1- amino -2- propyl alcohol |
| CN109646426B (en) * | 2019-01-09 | 2022-01-25 | 成都倍特药业股份有限公司 | Composition and method for detecting purity and related substances of 1-amino-2-propanol |
| CN112812026A (en) * | 2020-12-30 | 2021-05-18 | 茂名云龙工业发展有限公司 | Method for producing N, N-diethylamino isopropanol |
| CN116082172B (en) * | 2023-04-11 | 2023-07-14 | 山东友泉新材料有限公司 | Method for producing isopropanolamine |
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Address after: 210047 1-C18-1, Nanjing chemical industry park, Jiangsu, Nanjing Patentee after: NANJING HONGBAOLI ALKYLOL AMINE CHEMICAL CO., LTD. Address before: 210047 1-C18-1, Nanjing chemical industry park, Jiangsu, Nanjing Patentee before: Nanjing Baochun Chemical Co., Ltd. |