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Preparation method of HX-878

A technology of HX-878 and solvent, applied in the field of HX-878 preparation, can solve the problems of low purity and yield of HX-878, and achieve the effects of high purity and yield, short reaction time and low product viscosity

Pending Publication Date: 2022-03-22
天元航材(营口)科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The embodiment of the present invention provides a preparation method of HX-878, which aims to solve the problems of low purity and yield of HX-878 obtained by the existing preparation method of HX-878

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 150g of toluene, 41.5g of tetraethylenepentamine, and 14.5g of glycerin into a 500ml flask, stir evenly, raise the temperature to 40°C, start to slowly add 25.2g of acrylonitrile dropwise, control the dropping temperature between 40-60°C, drop After finishing, continue to insulate for 0.5 hour, desolvent toluene (toluene) after reaction finishes

[0018] After recovery by distillation, it can be recycled), followed by high vacuum dehydration for 2 hours, sampling and testing the water content (water content≤0.1%, deemed dehydration qualified), to obtain 75g of product (HX-878).

Embodiment 2

[0020] Add 150g of cycloethane, 50.5g of tetraethylenepentamine, and 14.5g of glycerin into a 500ml flask, stir evenly, raise the temperature to 60°C, and slowly add 25.2g of acrylonitrile dropwise, and the dropping temperature is controlled between 60-80°C. After the dropwise addition, continue to insulate for 1 hour. After the reaction, desolventize cyclohexane (recovered by cyclohexane distillation, which can be recycled), then high-vacuum dehydration for 2 hours, and take a sample to test the water content (water content≤0.1%, regarded as dehydration qualified), to obtain product (HX-878) 85g.

Embodiment 3

[0022] Add 150g of dichloroethane, 41.5g of tetraethylenepentamine, and 41.5g of glycerin into a 500ml flask, stir evenly, raise the temperature to 50°C, start to slowly add 25.2g of acrylonitrile dropwise, and control the dropping temperature between 50-70°C , continue to keep warm for 2 hours after the dropwise addition is completed, desolventize dichloroethane after the end of the reaction (dichloroethane can be recycled after distillation and recovery), then high-vacuum dehydration for 2 hours, take a sample to test the water content (water content≤0.1%) , regarded as qualified for dehydration), the product (HX-878) 110g was obtained.

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PUM

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Abstract

The embodiment of the invention provides a preparation method of HX-878, which comprises the following steps: S1, dissolving tetraethylenepentamine and glycerol in a specific solvent, fully stirring at normal temperature to uniformly mix, slowly dropwise adding acrylonitrile, controlling the reaction temperature within a certain range, and continuously keeping the temperature for a certain reaction time after dropwise adding; and S2, under a reduced pressure condition, firstly distilling to recover the solvent, then carrying out reduced pressure distillation to remove a trace amount of water to obtain HX-878, and when the water content of HX-878 is less than or equal to 0.1%, determining that HX-878 is qualified. The HX-878 prepared by the method disclosed by the invention is high in purity and yield.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of HX-878. Background technique [0002] Special bonding agent for nitramine, the hydroxyl group in the molecular structure of the multi-nitrile hydroxylamine polymer can chemically bond with the butyl rubber to enter the crosslinked network, and the multiple nitrile groups in the molecular structure can form a strong bond with the surface of the nitramine oxidant particle physical adsorption. Used as nitramine or nitramine-modified butylated hydroxyl solid propellant bonding agent can significantly improve the mechanical properties of the propellant, and can also be used in combination with other bonding agents for bonding of butylated hydroxyl rubber and ammonium perchlorate composite solid propellant . However, the HX-878 obtained by the traditional HX-878 preparation method has the problems of low purity and low yield. Contents of the invention...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08G73/02
CPCC08G83/00C08G73/02
Inventor 史哲周莹董长春王浩杨录新何通蔡东祝凯乾
Owner 天元航材(营口)科技股份有限公司
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