Preparation method for GAP base elastomer with non-isocyanate curing manner

A non-isocyanate, curing technology, applied in the field of preparation of GAP-based elastomers, can solve the problems of mechanical properties of materials and adverse effects of application effects, and achieve the effects of good mechanical properties, less interference, and mild reaction conditions.

Active Publication Date: 2013-12-11
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the isocyanate curing agent mainly has the following disadvantages: the isocyanate group can react with water, and the produced by-product primary amine has a higher reactivity with N

Method used

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  • Preparation method for GAP base elastomer with non-isocyanate curing manner
  • Preparation method for GAP base elastomer with non-isocyanate curing manner
  • Preparation method for GAP base elastomer with non-isocyanate curing manner

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A kind of preparation method of the GAP-based elastomer of non-isocyanate curing mode, it comprises the steps:

[0032] 1) Preparation of dimethyl 2,2-propargylmalonate:

[0033] a. Weigh 3.36g of 70wt% NaH and dissolve in 40mL of anhydrous THF to obtain a THF solution containing NaH; another 4.86ml of dimethyl malonate is dissolved in 40mL of anhydrous THF to obtain a dimethyl malonate solution ; 10.1ml propargyl bromide is added dropwise in the 80ml anhydrous tetrahydrofuran solution, obtains the solution of propargyl bromide;

[0034] b. Slowly add the dimethyl malonate solution into the THF solution of NaH at room temperature, and continue stirring for 1 h to obtain the reaction solution A; slowly transfer the propargyl bromide solution to the reaction solution A [Dimethyl malonate : Sodium hydride: the mol ratio of propargyl bromide=1:2.3:2.5], at 110 ℃, reflux reaction 3h, obtain reaction solution C;

[0035] Add (3×50mL) saturated ammonium chloride solution t...

Embodiment 2

[0043]A kind of preparation method of the GAP-based elastomer of non-isocyanate curing mode, it comprises the steps:

[0044] 1) Preparation of dimethyl 2,2-propargylmalonate:

[0045] a. Weigh 3.36g of 70wt% NaH and dissolve in 40mL of anhydrous THF to obtain a THF solution containing NaH; another 4.86ml of dimethyl malonate is dissolved in 40mL of anhydrous THF to obtain a dimethyl malonate solution ; 10.1ml propargyl bromide is added dropwise in the 80ml anhydrous tetrahydrofuran solution, obtains the solution of propargyl bromide;

[0046] b. Slowly add the dimethyl malonate solution into the THF solution of NaH at room temperature, and continue stirring for 1 h to obtain the reaction solution A; slowly transfer the propargyl bromide solution to the reaction solution A [Dimethyl malonate : Sodium hydride: the mol ratio of propargyl bromide=1:2.3:2.5], at 110 ℃, reflux reaction 3h, obtain reaction solution C;

[0047] Add (3×50mL) saturated ammonium chloride solution to...

Embodiment 3

[0053] A kind of preparation method of the GAP-based elastomer of non-isocyanate curing mode, it comprises the steps:

[0054] a. Weigh 3.36g of 70wt% NaH and dissolve in 40mL of anhydrous THF to obtain a THF solution containing NaH; another 4.86ml of dimethyl malonate is dissolved in 40mL of anhydrous THF to obtain a dimethyl malonate solution ; 10.1ml propargyl bromide is added dropwise in the 80ml anhydrous tetrahydrofuran solution, obtains the solution of propargyl bromide;

[0055] b. Slowly add the dimethyl malonate solution into the THF solution of NaH at room temperature, and continue stirring for 1 h to obtain the reaction solution A; slowly transfer the propargyl bromide solution to the reaction solution A [Dimethyl malonate : Sodium hydride: the mol ratio of propargyl bromide=1:2.3:2.5], at 110 ℃, reflux reaction 3h, obtain reaction solution C;

[0056] Add (3×50mL) saturated ammonium chloride solution to the reaction solution C and extract 3 times, separate the ...

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Abstract

The invention relates to a preparation method for a GAP base elastomer with a non-isocyanate curing manner. The preparation method comprises: 1) preparing 2,2-propargyl dimethyl malonate; 2) stirring under a N2 protection condition, adding a glycidyl azide polymer solution to the 2,2-propargyl dimethyl malonate solution to obtain a mixing solution H, adding cuprous chloride to the mixing solution H under N2 protection and stirring, maintaining a temperature of 0-25 DEG C, and carrying out a reaction under a light avoiding condition for 8-24 h to obtain a reaction solution J; and 3) carrying out suction filtration and rotary evaporation on the reaction solution J, and evaporating the solvent to obtain the GAP base elastomer with the non-isocyanate curing manner. According to the present invention, the preparation process is simple, the obtained product has good mechanical property, and the GAP content in the elastomer is high, such that the elastomer has high energy and has great potential application values in the development fields of high energy cleaning propellants based on azide, PBX explosives and the like.

Description

technical field [0001] The invention relates to a preparation method of a non-isocyanate-cured GAP-based elastomer, belonging to the technical field of new materials. Background technique [0002] Since the polyurethane curing system has the advantages of mild chemical reaction during the curing process, no small molecules are produced, and the formed propellant has good mechanical properties, it is widely used in the field of materials. However, the isocyanate curing agent mainly has the following disadvantages: the isocyanate group can react with water, and the produced by-product primary amine has a higher reactivity with NCO, and the generated CO 2 It will remain in the matrix to form air bubbles, which will directly have an adverse effect on the mechanical properties of the material and the application effect. Therefore, the development of a non-isocyanate curing system with excellent mechanical properties and insensitivity to ambient humidity and filler moisture conte...

Claims

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Application Information

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IPC IPC(8): C08G73/06C07C67/343C07C69/606
Inventor 黄进胡冲郭翔车圆圆丁有朝
Owner WUHAN UNIV OF TECH
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