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A kind of preparation method of bis (fatty alcohol polyoxyalkylene ether) secondary amine

A technology of alcohol polyoxyalkylene alkenyl ether and alcohol polyoxyalkylene, which is applied in the field of preparation of bis-secondary amines, can solve the problems of inability to prepare secondary amine content and lack, etc., achieve less side reactions, convenient feeding, and reduce costs Effect

Active Publication Date: 2015-12-30
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the existing amine ether preparation method at present, can not prepare two (fatty alcohol polyoxyalkylene ether) secondary amines with high secondary amine content and stable product quality, so lack of bis (fatty alcohol polyoxyalkylene ether) in the current product series enyl ether) secondary amine

Method used

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  • A kind of preparation method of bis (fatty alcohol polyoxyalkylene ether) secondary amine
  • A kind of preparation method of bis (fatty alcohol polyoxyalkylene ether) secondary amine
  • A kind of preparation method of bis (fatty alcohol polyoxyalkylene ether) secondary amine

Examples

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Effect test

example 1

[0047] 500g terminal primary amino C 12～14 Alcohol polyoxyethylene ether, 15g of catalyst Raney nickel are added to a 1000ml four-necked flask with a stirrer, a thermometer, a gas conduit, and a straight condenser tube, and the terminal primary amino group C 12～14 The molecular weight of alcohol polyoxyethylene ether is 390, and the amination rate is 46%. Pass hydrogen gas at a flow rate of 100ml / min, raise the temperature to 200°C at a stirring speed of 300r / min, and react for 5h.

[0048] After the reaction is over, lower the temperature to below 100°C, stop the hydrogen flow, and remove the catalyst, that is, bis(C 12～14 Alcohol polyoxyethylene) secondary amine, the secondary amine content (S%) is 92%.

example 2

[0050] 200g terminal primary amino C 12～14 Alcohol polyoxyethylene ether, 10g of catalyst Raney nickel are added to a 500ml four-necked flask with a stirrer, a thermometer, a gas conduit, and a straight condenser tube, and the terminal primary amino group C 12～14 The molecular weight of the alcohol polyoxyethylene ether is 390, and the amination rate is 63%. Pass hydrogen gas at a flow rate of 100ml / min, raise the temperature to 200°C at a stirring speed of 300r / min, and react for 5h.

[0051] After the reaction is over, lower the temperature to below 100°C, stop the hydrogen flow, and remove the catalyst, that is, bis(C 12～14 Alcohol polyoxyethylene) secondary amine, the secondary amine content (S%) is 89%.

example 3

[0053] 400g terminal primary amino C 12～14 Alcohol polyoxypropylene ether, 20g catalyst Raney nickel joins in the 1000ml four-necked flask that has stirrer, thermometer, gas conduit, straight condenser tube, terminal primary amino group C 12～14 The molecular weight of the alcohol polyoxypropylene ether is 476, and the amination rate is 61%. Pass hydrogen gas at a flow rate of 200ml / min, raise the temperature to 200°C at a stirring speed of 300r / min, and react for 5h.

[0054] After the reaction is over, lower the temperature to below 100°C, stop the hydrogen flow, and remove the catalyst, that is, bis(C 12～14 Alcohol polyoxypropylene) secondary amine, the secondary amine content (S%) is 43%.

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Abstract

The invention discloses a preparation method of bis(fatty alcohol polyoxyalkene ether) secondary amine, belonging to the technical field of organic chemical industry. The method comprises the following step of: preparing the bis(fatty alcohol polyoxyalkene ether) secondary amine through condensation-deamination coupling reaction of two-molecule primary amine under normal-pressure condition by taking primary amine-terminated fatty alcohol polyoxyalkene ether as a raw material and taking raney nickel as a catalyst. Ammoniation rate of the primary amine-terminated fatty alcohol polyoxyalkene ether is 40%-100%; dosage of the catalyst is 0-20% of the mass of the primary amine-terminated fatty alcohol polyoxyalkene ether; hydrogen gas flow velocity is 0 ml / minute-1000ml / minute for every 100g of the primary amine-terminated fatty alcohol polyoxyalkene ether; reaction temperature is 150 DEG C-250 DEG C; reaction time is 2 hours-20 hours. According to the preparation method disclosed by the invention, on the condition of improving content of secondary amine, process flow is simplified, and cost is lowered, so that the preparation method can be used for large-scale production in the industrial field.

Description

technical field [0001] The invention relates to a preparation method of bis(fatty alcohol polyoxyalkylene ether) secondary amine, which belongs to the technical field of organic chemical industry. Background technique [0002] Amine ether compounds (etheramine) is a class of compounds with both amine groups and ether bonds in the molecule, and its special structure determines its unique properties. Therefore, as a class of functional chemicals, amino ether compounds play an important role in many fields such as chemical industry and medicine. In the past 30 years, amino ether compounds have made great contributions to the development of the global chemical industry, especially this type Polyetheramine in the compound is widely used in many fields such as epoxy materials, concrete additives, organic pigments, fuels, lubricating oil additives, plastics, medical materials, composite materials, herbicides and insecticides. [0003] Based on the current reports on the synthesis ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/08
Inventor 朱新宝吴飞飞吴帅
Owner NANJING FORESTRY UNIV
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