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Method for preparing diisopropanolamine

A technology of diisopropanolamine and temperature control, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problems of high isomer content, inability to synthesize intermediates and the like, Achieve the effect of high product quality, low production cost and low production operation cost

Active Publication Date: 2011-04-20
NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is the problem that the isomer content in the 1,1'-azonylidene dipropan-2-ol synthesized by the existing method is relatively high and cannot be used in the synthesis intermediate of medicine or pesticide , to provide a new synthesis of 1,1'-azinoalkyldipropan-2-ol, which can directly control the isomers within 1% in the synthesis stage, so that the product 1,1'- Azadipropan-2-ol can meet the high-end needs of synthetic medicine, pesticide and other products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Mix 4950kg of liquid ammonia and 50kg of deionized water to form ammonia (water 1%), transport it with a high-pressure metering pump, and then use another high-pressure metering pump to deliver 2815kg (ammonia to cyclopropyl molar ratio is 6), cyclopropyl and ammonia After fully mixing, enter the preheater, preheat to 140°C, and then enter the reactor temperature control at 151-154°C, pressure control at 16.8-17.0Mpa, after full reaction for 3 hours, the mixture product obtained by the reaction first enters the flash evaporation The pressure of the tower is controlled at 1.5Mpa, the temperature of the tower bottom is controlled at 155-158℃, the excess ammonia is recovered, and the material in the tower bottom is flashed, and enters the dehydration tower for rectification and dehydration. The pressure of the dehydration tower is controlled at -0.085Mpa, and the temperature at the top of the tower is controlled At 46~47℃, the temperature of the tower bottom is controlled at...

Embodiment 2

[0017] Mix 4925kg of liquid ammonia and 75kg of deionized water to form ammonia water (water 1.5%), use a high-pressure metering pump to deliver, and then use another high-pressure metering pump to deliver 2400kg (ammonia to cyclopropyl molar ratio is 7), cyclopropyl and ammonia water After fully mixing, enter the preheater, preheat to 142°C, and then enter the reactor. The temperature is controlled at 152-155°C and the pressure is controlled at 17.0-17.3Mpa. After full reaction for 2.5 hours, the mixture product obtained by the reaction first enters the flash evaporation The pressure of the tower is controlled at 1.0Mpa, the temperature of the tower bottom is controlled at 155-158℃, the excess ammonia is recovered, the material in the tower bottom is flashed, and then enters the dehydration tower for rectification and dehydration, the pressure is controlled at -0.082Mpa, and the tower top temperature is controlled at 53 ~54℃, the temperature of the tower bottom is controlled at...

Embodiment 3

[0019] Mix 4875kg of liquid ammonia and 125kg of deionized water to form ammonia water (2.5% water), transport it with a high-pressure metering pump, and then use another high-pressure metering pump to deliver 2079kg (the molar ratio of ammonia to cyclopropyl is 8), cyclopropyl and ammonia After fully mixing, enter the preheater, preheat to 143°C, and then enter the reactor. The temperature is controlled at 149-152°C and the pressure is controlled at 17.2-17.5Mpa. After fully reacting for 2.0 hours, the mixture product obtained by the reaction first enters the flash evaporation Tower, the pressure is controlled at 0.8Mpa, the temperature of the tower bottom is controlled at 145-148℃, the excess ammonia is recovered, and the material in the tower bottom is flashed, and then enters the dehydration tower for rectification and dehydration. The pressure is controlled at -0.085Mpa, and the temperature at the top of the tower is controlled at 46. ~47℃, the temperature of the tower bott...

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PUM

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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 thediisopropanolamine 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 [0001] The invention relates to a method for preparing diisopropanolamine. Background technique [0002] Diisopropanolamine is 1,1’-nitronedipropan-2-ol (chemical formula: [CH 3 CH(OH)CH 2 〕 2 The common name of NH) is a derivative of isopropanolamine and propylene oxide. Diisopropanolamine has a wide range of uses as follows: it can be used as a foam stabilizer for detergents and a pesticide neutralizer; it can be used as a wax, fiber additives, insecticide, emulsifier, and dispersant; it can be used as a high-efficiency desulfurizer ; Used as synthetic gas CO in the synthetic ammonia industry 2 Remover, etc. [0003] Nowadays, most of the industrial production of diisopropanolamine uses ammonia water or liquid ammonia and propylene oxide as raw materials to synthesize isopropanolamine series mixtures, and then gradually separate monoisopropanolamine, diisopropanolamine, and triisopropylamine. Propanolamine method, the diisopropanolamine produced by this method u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C215/12C07C213/04
Inventor 张书芮益民韦华
Owner NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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