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

A technology of alkyl polyoxyalkylene ether and primary amino polyoxyalkylene monoalkyl ether, 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 of secondary amines, achieve less side reactions, The effect of convenient feeding and cost reduction

Active Publication Date: 2016-06-29
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 (alkyl polyoxyalkylene ethers) secondary amines with high secondary amine content and stable product quality, so there is a lack of bis (alkyl polyoxyalkylene ethers) in the current product series. enyl ether) secondary amine

Method used

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

Examples

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Effect test

example 1

[0046] Add 200g of primary amino-terminated polyoxyalkylene mono-n-butyl ether and 10g of catalyst Raney nickel into a 500ml four-necked flask equipped with a stirrer, a thermometer, a gas conduit, and a straight condenser tube. The molecular weight of ethylenic mono-n-butyl ether is 1646, n(EO):n(PO)=3:1, and the amination rate is 70%. Hydrogen gas was passed through at a flow rate of 110 ml / min, and the temperature was raised to 180° C. at a stirring speed of 300 r / min, and reacted for 5 h.

[0047] After the reaction, the temperature was lowered to below 100° C., the hydrogen flow was stopped, and the catalyst, that is, the bis(n-butyl polyoxyalkylene ether) secondary amine was removed by suction filtration, and the secondary amine content (S%) was 52%.

example 2

[0049] Add 200g of primary amino-terminated polyoxyalkylene mono-n-butyl ether and 10g of catalyst Raney nickel into a 500ml four-necked flask equipped with a stirrer, a thermometer, a gas conduit, and a straight condenser tube. The molecular weight of alkenyl n-butyl ether is 1646, n(EO):n(PO)=3:1, and the amination rate is 70%. Hydrogen gas was passed through at a flow rate of 100 ml / min, and the temperature was raised to 180° C. at a stirring speed of 300 r / min, and reacted for 5 h.

[0050] After the reaction, the temperature was lowered to below 100° C., the hydrogen flow was stopped, and the catalyst, that is, the bis(n-butyl polyoxyalkylene ether) secondary amine was removed by suction filtration. The secondary amine content (S%) was 59%.

example 3

[0052] Add 1000g of primary amino-terminated polyoxyalkylene mono-n-butyl ether and 30g of catalyst Raney nickel into a 2000ml four-necked flask equipped with a stirrer, thermometer, gas conduit, and straight condenser tube. The molecular weight of ethylenic mono-n-butyl ether is 1420, n(EO):n(PO)=3:1, and the amination rate is 92%. 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 10h.

[0053] After the reaction, the temperature was lowered to below 100° C., the hydrogen flow was stopped, and the catalyst, that is, the bis(n-butyl polyoxyalkylene ether) secondary amine was removed by suction filtration, and the secondary amine content (S%) was 54%.

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Abstract

A preparation method of bis(alkyl polyoxyalkylene ether) secondary amine is invented, which belongs to the technical field of organic chemical industry. The method uses primary amino-terminated polyoxyalkylene monoalkyl ether (R=C1-C4) as a raw material, and Raney nickel as a catalyst, to obtain bis (Alkyl polyoxyalkylene ether) secondary amine. The amination rate of primary amino-terminated polyoxyalkylene monoalkyl ether is 40-100%, the amount of catalyst is 0-20% of the mass of terminal primary amino-polyoxyalkylene mono-alkyl ether, and the hydrogen flow rate is 100g per 100g terminal primary amino group. Polyoxyalkylene monoalkyl ether 0-1000ml / min, reaction temperature 150-250°C, reaction 2-20h. Under the condition of increasing the secondary amine content, the invention simplifies the process flow and reduces the cost, so that it can be used for large-scale production in the industrial field.

Description

technical field [0001] The invention relates to a preparation method of bis(alkyl 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 methods ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00
Inventor 朱新宝吴飞飞于子洲董晓红房连顺张成宝
Owner NANJING FORESTRY UNIV
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