Method for synthesis and purification of bonding agent N-propargyl diethanol amine

A technology of propargyldiethanolamine and a purification method, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., can solve problems such as non-environmental protection, complicated process, low yield, etc., and achieve an increase in yield , The effect of simple process

Inactive Publication Date: 2016-04-13
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction of the above method is a heterogeneous system, the yield is low, and the column chromatography used for separation and purification has a slow rate, complicated process, and is not environmentally friendly.

Method used

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  • Method for synthesis and purification of bonding agent N-propargyl diethanol amine
  • Method for synthesis and purification of bonding agent N-propargyl diethanol amine
  • Method for synthesis and purification of bonding agent N-propargyl diethanol amine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The three-necked flask is equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel, and is cooled by an ice-salt bath. First add 105 g of diethanolamine, 120 g of triethylamine, and 200 g of tetrahydrofuran. After cooling to 0° C., slowly add 126 g of 3-bromopropyne dropwise. The reaction is exothermic, and the temperature of the dropwise addition is controlled so that the temperature of the reaction solution does not exceed 25°C. After the addition, the reaction is continued with natural stirring for 3 hours.

[0023] After stopping the reaction, the reaction solution was filtered with suction to remove the salt generated by the reaction. The filtrate was transferred to a rotary evaporator, and tetrahydrofuran, unreacted 3-bromopropyne and triethylamine were evaporated under the conditions of a temperature of 50° C. and a vacuum of 10 mmHg. The crude product is then transferred to a vacuum distillation unit, rectifying under the conditi...

Embodiment 2

[0033] The three-necked flask is equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel, and is cooled by an ice-salt bath. First add 105 g of diethanolamine, 101 g of triethylamine, and 200 g of tetrahydrofuran. After cooling to 0° C., slowly add 119 g of 3-bromopropyne dropwise. The reaction is exothermic, and the temperature of the dropwise addition is controlled so that the temperature of the reaction solution does not exceed 25°C. After the addition, the reaction is continued with natural stirring for 3 hours.

[0034] After stopping the reaction, the reaction solution was filtered with suction to remove the salt generated by the reaction. The filtrate was transferred to a rotary evaporator, and tetrahydrofuran, unreacted 3-bromopropyne and triethylamine were evaporated under the conditions of a temperature of 50° C. and a vacuum of 10 mmHg. The crude product is then transferred to a vacuum distillation unit, rectifying under the conditi...

Embodiment 3

[0036] The three-necked flask is equipped with mechanical stirring, a thermometer and a constant pressure dropping funnel, and is cooled by an ice-salt bath. First add 105 g of diethanolamine, 101 g of triethylamine, and 200 g of tetrahydrofuran. After cooling to 0° C., slowly add 119 g of 3-bromopropyne dropwise. The reaction is exothermic, and the temperature of the dropwise addition is controlled so that the temperature of the reaction solution does not exceed 25° C. After the addition, the reaction is continued with natural stirring for 2.5 hours.

[0037] After stopping the reaction, the reaction solution was filtered with suction to remove the salt generated by the reaction. The filtrate was transferred to a rotary evaporator, and tetrahydrofuran, unreacted 3-bromopropyne and triethylamine were evaporated under the conditions of a temperature of 50° C. and a vacuum of 10 mmHg. The crude product is then transferred to a vacuum distillation unit, rectified under the condi...

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Abstract

The invention discloses a method for synthesis and purification of the bonding agent N-propargyl diethanol amine. The structure of the compound is shown in the description. The bonding agent N-propargyl diethanol amine is expected to be applied to energetic binder type propellants. The method comprises the steps of adding 3-propargyl bromide to a diethanol amine tetrahydrofuran solution dropwise with triethylamine as the acid-binding agent under the ice-bath condition, conducting filtration after three hours of reaction, conducting filtrate concentration and reduced pressure distillation in sequence, and collecting the product. The method has the advantages of being high in yield and environmentally friendly.

Description

technical field [0001] The invention relates to a method for synthesizing and purifying a bonding agent N-propargyldiethanolamine, belonging to the field of organic synthesis. Background technique [0002] Composite solid propellant is a kind of composite polymer material with polymer prepolymer as binder and solid particles as filler. There are many factors affecting its mechanical properties, among which, ensuring the effective bonding of the interface between the solid particles and the binder is a necessary condition for the composite solid propellant to obtain excellent mechanical properties. In order to improve the bonding strength between the oxidizer and the binder interface in the solid propellant, a few parts per ten thousand to a few parts per thousand of a bonding agent is often added to the propellant formulation. These bonding agent molecules have the following three basic characteristics: (1) can gather on the surface of the solid particles filled in the prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/12C07C213/02C07C213/10
CPCC07C213/02C07C213/10C07C215/12
Inventor 闫峥峰潘永飞姬月萍陈斌刘卫孝汪营磊莫宏昌卢先明丁峰高福磊陆婷婷刘亚静张丽洁
Owner XIAN MODERN CHEM RES INST
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