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A kind of preparation method of polyol amine

A polyolamine and alcoholamine technology, which is applied in the preparation of organic compounds, chemical instruments and methods, preparation of aminohydroxy compounds, etc., can solve the problems of low product yield, high risk, and high pressure of ammoniation reaction, and achieve product The effect of high yield and green reaction process

Active Publication Date: 2020-11-20
NANJING POLYTECHNIC INSITUTE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dichloropropane undergoes ammoniation reaction, and the product propylenediamine is obtained through neutralization, concentration, desalination, rectification and other processes; the ammoniation reaction has high pressure and high risk, and a large amount of waste water is generated in the post-treatment process to pollute the environment
Dichloropropane is hydrolyzed to produce propylene glycol. The product yield of this process is low, a large amount of industrial salt is produced as a by-product, and a large amount of industrial wastewater is produced at the same time.
At present, domestic propylene oxide manufacturers have not yet found an effective way to utilize dichloropropane as a by-product. In order to further improve the comprehensive benefits of producing propylene oxide by the chlorohydrin method and reduce the raw material consumption of propylene oxide products, Rational treatment and utilization of by-product dichloropropane is an urgent technical research subject to be developed

Method used

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  • A kind of preparation method of polyol amine
  • A kind of preparation method of polyol amine
  • A kind of preparation method of polyol amine

Examples

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Effect test

preparation example Construction

[0026] A kind of preparation method of polyol amine, comprises the steps:

[0027] Step 1: Catalyst Preparation

[0028] Roast coconut shell charcoal in a nitrogen atmosphere at 250-350°C for 3-6 hours, after cooling, soak it in 1-10mol / L sodium hydroxide or potassium hydroxide aqueous solution for 1-10 hours, filter and wash with distilled water for 2-6 times, 110- After drying at 150°C for 3-12 hours, soak in 1-10mol / L nitric acid aqueous solution for 1-12 hours, then wash the filtered coconut shell charcoal with distilled water for 2-6 times, and dry at 110-150°C for 3-12 hours for later use.

[0029] Mix the pretreated granular coconut shell charcoal with sodium hydroxide or potassium hydroxide and lanthanum nitrate or cesium nitrate evenly, place in a horse boiling furnace, and roast at 250-550°C for 6-12 hours in a nitrogen atmosphere, so that sodium hydroxide, hydroxide Potassium, lanthanum nitrate, and cesium nitrate melt and infiltrate into the gap between the activa...

Embodiment 1

[0034] Coconut shell charcoal was roasted at 300°C in a nitrogen atmosphere for 6h, cooled and soaked in 7mol / L sodium hydroxide aqueous solution for 6h, filtered and washed with distilled water for 4 times, dried at 120°C for 6h, then soaked in 7mol / L nitric acid aqueous solution for 8h, The coconut shell charcoal was washed with distilled water for 3 times, dried at 120°C for 6 hours after filtration, and roasted at 300°C for 6 hours for later use.

[0035] The processed granular coconut shell charcoal, sodium hydroxide and lanthanum nitrate are mixed according to the mass ratio of 100:5:1, and sodium hydroxide and lanthanum nitrate are prepared into a mixed solution. The coconut shell charcoal is excessively impregnated and adsorbed for 10 hours under stirring, and dried at 120°C for 8 hours. Then put it in a horse boiling furnace and roast at 350°C for 8 hours in a nitrogen atmosphere, so that sodium hydroxide and lanthanum nitrate melt and penetrate into the gap between th...

Embodiment 2

[0037] at 1 # In the head tank, alcohol amine and dichloropropane are mixed in a molar ratio of 1:1 to form a homogeneous solution, and under the action of gravity, the flow rate is adjusted to 1000mL / min, from 1 # The bottom of the catalytic column enters 1 # Catalytic column, control the column temperature at 60°C for reaction; the reaction system leaves the top of the catalytic column for 1 # column entry 2 # high slot; in 2 # high slot, from 1 # The material of the column is fully mixed with the alcohol amine metered in (alcohol amine and the original dichloropropane molar ratio is 1:2), and under the action of gravity, the mixed solution changes from 2 # The bottom of the catalytic column enters 2 # The catalytic column completes the catalytic reaction at 70°C, and the reaction material leaves the reaction column from the top of the catalytic column and enters the 3 # High slot. in 3 # The alcohol amine (alcohol amine and original dichloropropane mol ratio is 1:2)...

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Abstract

The invention relates to a preparation method of multielement alcohol amine and belongs to the technical field of organic chemicals. The preparation method comprises the following step: continuously-flowing propylene dichloride and alcohol amine added stepwise react on a solid catalyst on design equipment to synthesize the multielement alcohol amine. The invention provides a deep processing methodof the propylene dichloride, and the problem that other application ways of the propylene dichloride pollute the environment is solved, the used catalyst can be regenerated and repeatedly used, therefore, the deep processing method belongs to a pollution-free chemical process; the preparation method of the multielement alcohol amine provided by the invention has the advantages of mild condition,low operation cost, high production efficiency and flexible functionality adjustment of multielement alcohol amine, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of polyol amine, which belongs to the technical field of organic chemical industry. Background technique [0002] A large amount of dichloropropane is by-produced in the process of producing epichlorohydrin by chlorohydrin method. Dichloropropane undergoes ammoniation reaction, and the product propylenediamine is obtained through neutralization, concentration, desalination, rectification and other processes; the ammoniation reaction has high pressure and high risk, and a large amount of waste water is generated in the post-treatment process to pollute the environment. Under the action of a catalyst, dichloropropane undergoes a chlorination reaction in an air stream at 490°C to generate carbon tetrachloride and tetrachloroethylene; dichloropropane can also be pyrolyzed to produce 3-chloropropene and 1-chloropropene; the chlorination And decomposition reaction conditions are harsh, and equipment requirements...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/08C07C215/12C07C215/14B01J27/25
CPCB01J27/25C07C213/08C07C215/12C07C215/14Y02P20/584
Inventor 于清跃朱新宝黎松于荟孙飞
Owner NANJING POLYTECHNIC INSITUTE
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