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Preparation method for cyanoethyl graft amide

A method of determination, the technology of dimethyl sulfoxide, applied in the field of cyanoethyl grafted amide and its preparation, can solve the problems of too fast increase of the viscosity of the syrup, high reactivity, and less dosage, and achieve the flow flow of the syrup Good flatness, stable reaction process and high purity

Active Publication Date: 2014-07-23
HUBEI SANJIANG AEROSPACE JIANGHE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, amide compounds are introduced into the high burning rate formula of butylated hydroxy as process additives, and the dosage is small and the effect is remarkable; it can improve the physical infiltration of the interface between the filler and the binder, and effectively improve the process performance of the propellant in the early stage of mixing. The active hydrogen on the active group reacts too high with the curing agent toluene diisocyanate, which causes the viscosity of the syrup to increase too fast, and the pot life of the syrup is only about 4 hours

Method used

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  • Preparation method for cyanoethyl graft amide
  • Preparation method for cyanoethyl graft amide
  • Preparation method for cyanoethyl graft amide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve the amide in 4.5 times the volume of dimethyl sulfoxide solvent, add dropwise acrylonitrile with a molar ratio of 2.8 times under mechanical stirring, and use an ice-water bath to cool the dropwise addition of acrylonitrile so that the liquid phase temperature is maintained at 30 ℃. Under the condition of reflux and stirring, react at 78°C for 6h; stop the reaction, evaporate excess acrylonitrile and inert solvent to obtain cyanoethyl grafted amide.

Embodiment 2

[0020] The amide was dissolved in 4.5 times the volume of dimethyl sulfoxide and acetone 1:1 mixed solution solvent, and under mechanical stirring, 2.5 times the molar ratio of acrylonitrile was added dropwise. The liquidus temperature was maintained at 30°C. Under the condition of reflux and stirring, react at 50°C for 12h; stop the reaction, evaporate excess acrylonitrile and inert solvent to obtain cyanoethyl grafted amide.

Embodiment 3

[0022] Dissolve the amide in 3 times the volume of dimethyl sulfoxide solution solvent, add dropwise acrylonitrile with a molar ratio of 2.2 times under mechanical stirring, and use an ice-water bath to cool the dropwise addition of acrylonitrile so that the liquid phase temperature is maintained at 27°C. React at 100°C for 3 hours under reflux and stirring; stop the reaction, distill off excess acrylonitrile and inert solvent to obtain cyanoethyl grafted amide.

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Abstract

The invention relates to a preparation method for cyanoethyl graft amide and a product, which belong to the field of manufacturing for composite solid propellants. The preparation method for cyanoethyl graft amide comprises the following steps of: dissolving amide in 3-6 times of volume of inert solvent, dripping a certain amount of acrylonitrile at a room temperature while mechanically stirring, and reacting for 3-12 hours at 50-100 DEG C in a reflux stirring condition; and stopping the reaction, and steaming out excessive acrylonitrile and inert solvent to obtain the cyanoethyl graft amide. The preparation method has the characteristics of being safe, convenient to operate, high in product purity and high in yield.

Description

technical field [0001] The invention belongs to the field of composite solid propellant manufacture, and in particular relates to a cyanoethyl grafted amide and a preparation method thereof. Background technique [0002] Composite solid propellant materials are high solids composed of binder system, plasticizer, metal micropowder such as aluminum powder, magnesium aluminum alloy, etc., oxidant micropowder such as ammonium perchlorate, potassium perchlorate, etc., burning rate regulator and functional additives content of solid energetic material. The manufacturing process mainly includes three main processes of slurry mixing, pouring and curing. The mixing and pouring of the propellant is carried out under the flowing state of the slurry. The rheological properties of the slurry are directly related to the reliability of the propellant. Pourability, leveling, structural integrity, stability of internal ballistic performance, etc. Since the 1960s, the solid propellant indus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/25C07C253/30G01N5/04C06B23/00
Inventor 舒凯凯易会岩段军鸿罗桂莲牛草坪韩清杨香萍郑化殷以华李方朔
Owner HUBEI SANJIANG AEROSPACE JIANGHE CHEM TECH
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