Preparation method of diethylene monoisopropanolamine

A technology of monoisopropanolamine and diethanolamine, which is applied in the preparation of organic compounds, chemical instruments and methods, and the preparation of aminohydroxyl compounds, etc. It can solve the problems of reducing the utilization rate of propylene oxide, high vacuum in the distillation process, and complex reaction systems and other problems, to achieve the effect of reducing the probability of side reactions, high material conversion rate, and high product purity

Active Publication Date: 2014-12-24
NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] Patent CN10292403A discloses a method for preparing diethanol monoisopropanolamine using water as a solvent, DEA and propylene oxide as raw materials in the presence of a polymerization inhibitor. The defect of this method is that the vacuum degree of the distillation process is high , the requirements for production equipment are higher; at the same time, the addition of polymerization inhibitors makes the reaction system more complicated, and there will be residual bottoms after distillation, which is difficult to handle
[0006] Patent CN103224453A uses water as a solvent, and uses propylene oxide and diethanolamine as raw materials to prepare diethanol monoisopropanolamine. The defect of this method is that the alk

Method used

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Examples

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Effect test

Embodiment 1

[0026] The high-pressure reactor is pre-replaced with nitrogen to replace the air in the reactor, and 2.1 tons of diethanolamine and 1.14 tons of propylene oxide are sent into the high-pressure reactor through a pre-mixer, and the reactor is boosted to 0.4MPa, and the stirring device is turned on, and the condensation is turned on. Control the temperature in the kettle with water at 10-20°C, stir and mix for 1 hour, stop condensing water, heat the material to 30°C, stop heating, use the heat of reaction to raise the temperature, control the reaction temperature to 80°C, stir and react for 6 hours, and obtain two The ethanol monoisopropanolamine product has a product purity of 96.51% through gas chromatography analysis.

Embodiment 2

[0028] The high-pressure reactor is pre-replaced with nitrogen to replace the air in the reactor, and 2.1 tons of diethanolamine and 1.16 tons of propylene oxide are sent into the high-pressure reactor through a pre-mixer, and the reactor is boosted to 0.4MPa, and the stirring device is turned on, and the condensation is turned on. Control the temperature in the kettle with water at 10-20°C, stir and mix for 0.8 hours, stop condensing water, heat the material to 35°C, stop heating, use the heat of reaction to raise the temperature, control the reaction temperature to 90°C, stir and react for 6 hours, and obtain two The ethanol monoisopropanolamine product has a product purity of 95.63% through gas chromatography analysis.

Embodiment 3

[0030] The high-pressure reactor is pre-replaced with nitrogen to replace the air in the reactor, and 2.1 tons of diethanolamine and 0.464 tons of propylene oxide are sent into the high-pressure reactor through a pre-mixer, and the reactor is boosted to 0.2MPa, and the stirring device is turned on, and the condensation is turned on. Control the temperature in the kettle with water at 10-20°C, stir and mix for 0.5 hours, stop condensing water, heat the material to 40°C, stop heating, use the heat of reaction to raise the temperature, control the reaction temperature to 100°C, stir and react for 4 hours, and obtain two For the crude product of ethanol monoisopropanolamine, heat the crude product and pass it into a continuous rectification device. Under the vacuum condition of -0.099MPa, the raw material of diethanolamine in the crude product is separated, and the material in the tower tank is the required diethanol The monoisopropanolamine product has a product purity of 98.31% t...

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Abstract

The invention relates to a preparation method of diethylene monoisopropanolamine. The preparation method comprises the following steps of (1) introducing an inert gas to replace air inside a reaction kettle into the reaction kettle; (2) premixing epoxy propane and diethanolamine, then adding to the reaction kettle, introducing the inert gas to keep the pressure inside the reaction kettle to 0.1-0.5 Mpa, stirring and mixing materials, then raising temperature, keeping the temperature, and reacting to obtain a diethylene monoisopropanolamine product. According to the preparation method disclosed by the invention, diethanolamine and epoxy propane are utilized as raw materials and the conventional way of taking water as a solvent is abandoned, and the materials are premixed, so that the viscosity and solidification point of the reacted materials are reduced; the fast progress of reaction is facilitated due to the uniform dispersion of the two materials in a reactor; in addition, under the condition of low alkane-amine ratio, the improvement of the utilization ratio of epoxy propane and the reduction of generation probability of side reaction are facilitated. The whole process has the advantages of low energy consumption, high material transformation rate, high product purity, stable quality and no wastes.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of high-purity diethanol monoisopropanolamine. Background technique [0002] Diethanolamine monoisopropanolamine is a low-toxic, environmentally friendly alcohol amine fine chemical product, mainly used in surfactants, widely used in chemical raw materials, pigments, medicine, building materials and other fields, in cement additives , Skin care products and fabric softener are widely used. [0003] At present, in the field of cement grinding aids, most of its formulas are single or compound products of chemical raw materials such as alcohols, alcohol amines, and acetates. It has a strengthening effect on cement, so the development and application of cement grinding aids with high grinding aid and high strength enhancement performance have been paid more and more attention. Compared with other similar cement additive products, diethanol monoisopropanolamine (...

Claims

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Application Information

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IPC IPC(8): C07C215/12C07C213/04
CPCY02P20/582
Inventor 汪少平张书杭建荣李国华
Owner NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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