CN101265197B - Method for preparing diisopropanolamine - Google Patents
Method for preparing diisopropanolamine Download PDFInfo
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- CN101265197B CN101265197B CN2008100240546A CN200810024054A CN101265197B CN 101265197 B CN101265197 B CN 101265197B CN 2008100240546 A CN2008100240546 A CN 2008100240546A CN 200810024054 A CN200810024054 A CN 200810024054A CN 101265197 B CN101265197 B CN 101265197B
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Abstract
The invention relates to a method of manufacturing diisopropanolamine. Liquid ammonia and water are mixed to form ammonia water which is fully mixed with propylene oxide; the mixed solution is preheated until the temperature reach 140 to 145 DEG C and then is delivered into a reactor for reacting, the temperature is controlled within 148 to 155 DEG C when in reacting, the pressure is controlled within 16.0 to 18.0MPa, the inputting molar ratio of the ammonia and the propylene oxide is controlled within 5 to 8, and the reaction is fully performed for 1.5 to 3 hours; the mixture products obtained in the reaction are separated to obtain isopropanolamine products, diisopropanolamine products and triisopropanolamine products through flash evaporation and rectification in a stepwise way. In the diisopropanolamine products which are manufactured by adopting the method, the component of 1, 1<1>-nitrousalkyl-dipropyl-2-alcohol accounts for more than 99 percent (hereinafter referred to as mass percent), and the isomeride thereof is less than 1 percent. In addition, the cost of the production operation in the method is less, the production cost is low, the product quality is high, and the high-end requirement of products such as synthetic medicine, farm insecticide, etc. is satisfied.
Description
Technical field
The present invention relates to a kind of method of producing diisopropanolamine (DIPA).
Background technology
Diisopropanolamine (DIPA) is 1, and (chemical formula is 1 '-Ya azanyl, two propan-2-ols: (CH
3CH (OH) CH
2)
2Being commonly called as NH) is the derivative that a Yi Bingchunan and propylene oxide reaction generate.Diisopropanolamine (DIPA) has following extensive use: can be used for suds-stabilizing agent, agricultural chemicals neutralizing agent as detergent use; Can be used as wax, textile auxiliary agent, sterilant, emulsifying agent, dispersion agent; Can be used as efficient desulfurizing agent; Be used as the synthetic gas CO that uses in the ammonia synthesizing industry
2Remover etc.
Present industrial production diisopropanolamine (DIPA) mostly is that adopting with ammoniacal liquor or liquefied ammonia and propylene oxide is raw material petrohol amine series mixture, isolate the method for a Yi Bingchunan, diisopropanolamine (DIPA), tri-isopropanolamine more step by step, the diisopropanolamine (DIPA) that this method is produced contains the above isomers of 4-10% (quality percentage composition, butt) usually.Because the isomer that wherein contains can generate the chemical substance of no drug effect when synthetic medicine or pesticide intermediate, sometimes even generate the chemical substance of toxic side effect, therefore, the Yi Bingchunan that existing method is produced can not be directly used in synthetic medicine or pesticide intermediate, need be with 1 in the diisopropanol amine product, the pure and mild isomer of 1 '-Ya azanyl dipropyl-2-separates again, to obtain high purity (〉=99%, mass ratio) 1,1 '-Ya azanyl, two propan-2-ols just can be used for synthetic medicine or pesticide intermediate.But, 1, the separating difficulty of pure and mild these the two kinds of isomerss of its isomers of 1 '-Ya azanyl dipropyl-2-is big, energy consumption is high, and production process complexity, processing condition harshness, and bigger in the industrial difficulty that they will be separated, need to increase new installation, 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, the isometry body burden is higher in 1 '-Ya azanyl, two propan-2-ols, the problem that can not in medicine or agricultural chemicals synthetic intermediate, use, provide a kind of new synthetic 1,1 '-Ya azanyl, two propan-2-ols, can directly isomers be controlled in 1% at synthesis phase, thereby make product 1,1 '-Ya azanyl, two propan-2-ols can satisfy the high-end needs of products such as synthetic medicine, agricultural chemicals.
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, again with the propylene oxide thorough mixing after, be preheated to 140～145 ℃ then, the molar ratio of ammonia and propylene oxide is controlled at 5～8;
2) material after the preheating is sent into reactor and react, temperature is controlled at 148～155 ℃ during reaction, and pressure-controlling was reacted 1～3 hour at 16.0～18.0Mpa;
3) mixture that reaction is obtained 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) the Yi Bingchunan mixture after will dewatering is sent into a Yi Bingchunan fractionate and is carried out rectifying, the fractionate pressure-controlling-0.095～-0.099Mpa, tower still temperature is controlled at 140-160 ℃, tower top temperature is controlled at 55～70 ℃;
6) the Yi Bingchunan mixture that a Yi Bingchunan fractionate tower still is obtained enters the diisopropanolamine (DIPA) rectifying tower and carries out smart gold-plating, the rectifying tower pressure-controlling-0.097～-0.1Mpa, tower still temperature is controlled at 170-200 ℃, and tower top temperature is controlled at 130～150 ℃, cat head extraction diisopropanol amine product.
Above-mentioned ammoniacal liquor adopts the deionized water preparation, and wherein the mass percent of water is 0.5～2.5%.
Adopt diisopropanol amine product that the present invention makes wherein 1,1 '-Ya azanyl-two propan-2-ol composition accounts for 99% more than (mass percent, down with), and its isometry body burden is below 1%.In addition, production operation expense of the present invention is few, and production cost is low, and the product quality height has satisfied the high-end needs of products such as synthetic medicine, agricultural chemicals.
Embodiment
Embodiment 1
4950kg liquefied ammonia and 50kg deionized water thorough mixing are formed ammoniacal liquor (water 1%), use the high pressure measurement pump delivery, use another high pressure measurement pump delivery 2815kg (ammonia is 6 with ring third mol ratio) again, behind ring third and the ammoniacal liquor thorough mixing, enter preheater, be preheated to 140 ℃, enter temperature of reactor then and be controlled at 151-154 ℃, pressure-controlling is at 16.8-17.0Mpa, fully reaction is after 3 hours, the mix product that reaction obtains is introduced into flashing tower, pressure-controlling is at 1.5Mpa, tower still temperature is controlled at 155-158 ℃, reclaim excess of ammonia, flashing tower still material, enter dehydration tower and carry out rectifying and dewatering, 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 113-115 ℃, the Yi Bingchunan mixture that the dehydration tower still obtains enters a different pressure tower and is controlled at-0.098Mpa, tower still temperature is controlled at 148-151 ℃, and tower top temperature is controlled at 59～61 ℃, and the Yi Bingchunan mixture that a different tower still obtains enters two different towers, pressure-controlling is at-0.098Mpa, tower still temperature is controlled at 185-190 ℃, and tower top temperature is controlled at 138～140 ℃, cat head extraction diisopropanol amine product.Gained diisopropanol amine product after testing 1,1 '-Ya azanyl, two propan-2-ol compositions account for 99.22%.
Embodiment 2
4925kg liquefied ammonia and 75kg deionized water thorough mixing are formed ammoniacal liquor (water 1.5%), use the high pressure measurement pump delivery, use another high pressure measurement pump delivery 2400kg (ammonia is 7 with ring third mol ratio) again, behind ring third and the ammoniacal liquor thorough mixing, enter preheater, be preheated to 142 ℃, enter temperature of reactor then and be controlled at 152-155 ℃, pressure-controlling is at 17.0-17.3Mpa, fully reaction is 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 ℃, reclaim excess of ammonia, flashing tower still material, enter dehydration tower and carry out rectifying and dewatering, pressure-controlling is at-0.082Mpa, and tower top temperature is controlled at 53～54 ℃, and tower still temperature is controlled at 123-125 ℃, the Yi Bingchunan mixture that the dehydration tower still obtains enters a different pressure tower and is controlled at-0.098Mpa, tower still temperature is controlled at 149-152 ℃, and tower top temperature is controlled at 60～61 ℃, and the Yi Bingchunan mixture that a different tower still obtains enters two different towers, pressure-controlling is at-0.099Mpa, tower still temperature is controlled at 190-193 ℃, and tower top temperature is controlled at 137～139 ℃, cat head extraction diisopropanol amine product.Gained diisopropanol amine product after testing 1,1 '-Ya azanyl, two propan-2-ol compositions account for 99.45%.
Embodiment 3
4875kg liquefied ammonia and 125kg deionized water thorough mixing are formed ammoniacal liquor (water 2.5%), use the high pressure measurement pump delivery, use another high pressure measurement pump delivery 2079kg (ammonia is 8 with ring third mol ratio) again, behind ring third and the ammoniacal liquor thorough mixing, enter preheater, be preheated to 143 ℃, enter temperature of reactor then and be controlled at 149-152 ℃, pressure-controlling is at 17.2-17.5Mpa, fully reaction is after 2.0 hours, the mix product that reaction obtains is introduced into flashing tower, pressure-controlling is at 0.8Mpa, tower still temperature is controlled at 145-148 ℃, reclaim excess of ammonia, flashing tower still material, enter dehydration tower and carry out rectifying and dewatering, pressure-controlling is at-0.085Mpa, and tower top temperature is controlled at 46～47 ℃, and tower still temperature is controlled at 114-115 ℃, the Yi Bingchunan mixture that the dehydration tower still obtains enters a different pressure tower and is controlled at-0.098Mpa, tower still temperature is controlled at 148-152 ℃, and tower top temperature is controlled at 60～62 ℃, and the Yi Bingchunan mixture that a different tower still obtains enters two different towers, pressure-controlling is at-0.0995Mpa, tower still temperature is controlled at 178-185 ℃, and tower top temperature is controlled at 133～135 ℃, cat head extraction diisopropanol amine product.Gained diisopropanol amine product after testing 1,1 '-Ya azanyl, two propan-2-ol compositions account for 99.18%.
Claims (2)
1. a method of producing diisopropanolamine (DIPA) is characterized in that comprising the steps:
1) liquefied ammonia and water are made into ammoniacal liquor, again with the propylene oxide thorough mixing after, be preheated to 140～145 ℃ then, the molar ratio of ammonia and propylene oxide is controlled at 5～8;
2) material after the preheating is sent into reactor and react, temperature is controlled at 148～155 ℃ during reaction, and pressure-controlling was reacted 1～3 hour at 16.0～18.0Mpa;
3) mixture that reaction is obtained 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) the Yi Bingchunan mixture after will dewatering is sent into a Yi Bingchunan fractionate and is carried out rectifying, the fractionate pressure-controlling-0.095～-0.099Mpa, tower still temperature is controlled at 140-160 ℃, tower top temperature is controlled at 55～70 ℃;
6) the Yi Bingchunan mixture that a Yi Bingchunan fractionate tower still is obtained enters the diisopropanolamine (DIPA) rectifying tower and carries out smart gold-plating, the rectifying tower pressure-controlling-0.097～-0.1Mpa, tower still temperature is controlled at 170-200 ℃, and tower top temperature is controlled at 130～150 ℃, cat head extraction diisopropanol amine product.
2. make the method for diisopropanolamine (DIPA) according to claim 1, it is characterized in that ammoniacal liquor adopts the deionized water preparation, wherein the mass percent of water is 0.5～2.5%.
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|---|---|---|---|
| CN2008100240546A CN101265197B (en) | 2008-04-23 | 2008-04-23 | Method for preparing diisopropanolamine |
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| CN2008100240546A CN101265197B (en) | 2008-04-23 | 2008-04-23 | Method for preparing diisopropanolamine |
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| CN101265197B true CN101265197B (en) | 2011-04-20 |
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| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410416A (en) * | 2002-11-13 | 2003-04-16 | 南京红宝丽股份有限公司 | Production method of isopropanolamine |
| US20040068143A1 (en) * | 2002-10-07 | 2004-04-08 | Diwakar Garg | Process for producing alkanolamines |
| CN1800147A (en) * | 2005-10-13 | 2006-07-12 | 南京红宝丽股份有限公司 | Method for improving isopropanolamine synthetic effect |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040068143A1 (en) * | 2002-10-07 | 2004-04-08 | Diwakar Garg | Process for producing alkanolamines |
| CN1410416A (en) * | 2002-11-13 | 2003-04-16 | 南京红宝丽股份有限公司 | Production method of isopropanolamine |
| CN1800147A (en) * | 2005-10-13 | 2006-07-12 | 南京红宝丽股份有限公司 | Method for improving isopropanolamine synthetic effect |
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Address after: 210047 Nanjing chemical industry park, Jiangsu, Nanjing, 1-C18-1 Patentee after: NANJING HONGBAOLI ALKYLOL AMINE CHEMICAL CO., LTD. Address before: 210047 Nanjing chemical industry park, Jiangsu, Nanjing, 1-C18-1 Patentee before: Nanjing Baochun Chemical Co., Ltd. |