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A kind of preparation method of the gap-based elastomer of non-isocyanate curing mode

A non-isocyanate, curing method, applied in the field of preparation of GAP-based elastomers, can solve the problems of material mechanical properties and adverse effects of application effects, and achieve good mechanical properties, easy purification, and simple preparation process

Active Publication Date: 2015-09-30
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 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

Method used

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  • A kind of preparation method of the gap-based elastomer of non-isocyanate curing mode
  • A kind of preparation method of the gap-based elastomer of non-isocyanate curing mode
  • A kind of preparation method of the gap-based elastomer of non-isocyanate curing mode

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Embodiment 1

[0030] A kind of preparation method of the GAP-based elastomer of non-isocyanate curing mode, it comprises the steps:

[0031] 1) Preparation of dimethyl 2,2-propargylmalonate:

[0032] 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 THF solution, obtains the solution of propargyl bromide;

[0033] 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;

[0034] Add (3×50mL) saturated ammonium chloride solution to the reacti...

Embodiment 2

[0042] A kind of preparation method of the GAP-based elastomer of non-isocyanate curing mode, it comprises the steps:

[0043]1) Preparation of dimethyl 2,2-propargyl malonate:

[0044] 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 THF solution, obtains the solution of propargyl bromide;

[0045] 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;

[0046] Add (3×50mL) saturated ammonium chloride solution to the reacti...

Embodiment 3

[0052] A kind of preparation method of the GAP-based elastomer of non-isocyanate curing mode, it comprises the steps:

[0053] 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 THF solution, obtains the solution of propargyl bromide;

[0054] 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;

[0055] Add (3×50mL) saturated ammonium chloride solution to the reaction solution C and extract 3 times, separate the lower inorga...

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Abstract

A method for preparing a non-isocyanate-cured GAP-based elastomer, which comprises the following steps: 1) preparation of 2,2-propargyl dimethyl malonate; 2) stirring under N2 protection conditions, and polycondensation The nitrogen glycidyl ether solution is added to the 2,2-propargyl dimethyl malonate solution to obtain the mixed solution H. Under N2 protection and stirring conditions, cuprous chloride is added to the mixed solution H to keep 0~ React at 25°C in the dark for 8-24 hours to obtain a reaction solution J; 3) Suction filter the reaction solution J, rotary evaporate, and evaporate the solvent to obtain a non-isocyanate-cured GAP-based elastomer. The preparation process of the method of the present invention is simple, the obtained product has better mechanical properties, and the content of GAP in the elastomer is very high, which makes the elastomer have higher energy, and is developed based on azide high-energy clean propellants and PBX explosives. It has great potential application value in this field.

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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Patent Type & Authority Patents(China)
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