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Photocurable adhesive for additive manufacturing and synthesis method thereof

A technology of additive manufacturing and light curing, which is applied in additive processing, compressed gas generation, explosives, etc., and can solve problems such as solvent volatilization, side reactions, and incomplete curing

Inactive Publication Date: 2021-05-18
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention provides a light-cured energetic adhesive capable of additively manufacturing energetic materials such as explosives and solid propellants and a synthesis method thereof, aiming to solve the problem that traditional adhesives are difficult to realize light-cured forming. Solve the problems of incomplete curing, high temperature, easy to cause solvent volatilization and side reactions, and the inability to manufacture complex models in traditional thermal curing

Method used

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  • Photocurable adhesive for additive manufacturing and synthesis method thereof
  • Photocurable adhesive for additive manufacturing and synthesis method thereof
  • Photocurable adhesive for additive manufacturing and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] A method for synthesizing an azide polyether type urethane acrylate photocurable energetic adhesive, the specific steps are as follows:

[0039] Step 1) In a four-necked round-bottomed flask equipped with a magnetic heating stirrer, a condensing reflux tube, a constant pressure dropping funnel, and a thermocouple, feed N 2Remove moisture from the atmosphere. Toluene diisocyanate (1.04g, about 6mmol) was added to the system, heated to 50°C, and then GAP (5g, about 3mmol) and catalyst dibutyltin dilaurate (0.012g, about 0.02%) were mixed and dropped at constant pressure Start dropping in the liquid funnel, keep the system temperature at 50°C and react for 2h.

[0040] Step 2) Use di-n-butylamine titration method to measure the content of -NCO group in the system. When the conversion rate reaches 50%, stop heating, and after cooling to 40°C, add hydroxyethyl acrylate (0.73g, about 6.3mmol) and polymerization inhibitor hydroquinone (0.02g, about 0.03%), after the system i...

Embodiment 2

[0042] A method for synthesizing an azide polyether type urethane acrylate photocurable energetic adhesive, the specific steps are as follows:

[0043] Step 1) In a four-necked round-bottomed flask equipped with a magnetic heating stirrer, a condensing reflux tube, a constant pressure dropping funnel, and a thermocouple, feed N 2 Remove moisture from the atmosphere. Add isophorone diisocyanate (1.33g, about 6mmol) to the system, heat to 50°C, then mix GAP (5g, about 3mmol) and catalyst dibutyltin dilaurate (0.018g, about 0.03%) in Start dropping in the constant-pressure dropping funnel, and keep the system temperature at 50°C for 3 hours.

[0044] Step 2) Use di-n-butylamine titration to measure the content of -NCO groups in the system. When the conversion rate reaches 50%, stop heating, and after cooling to 40° C., add hydroxyethyl acrylate (0.73 g, About 6.3mmol) and polymerization inhibitor hydroquinone (0.021g, about 0.03%), after the system is stable, the temperature is...

Embodiment 3

[0046] A method for synthesizing an azide polyether type urethane acrylate photocurable energetic adhesive, the specific steps are as follows:

[0047] Step 1) In a four-necked round-bottomed flask equipped with a magnetic heating stirrer, a condensing reflux tube, a constant pressure dropping funnel, and a thermocouple, feed N 2 Remove moisture from the atmosphere. Add hexamethylene diisocyanate (1.01g, about 6mmol) to the system, heat to 80°C, then mix GAP (5g, about 3mmol) and catalyst dibutyltin dilaurate (0.018g, about 0.03%) in Start dropping in the constant-pressure dropping funnel, and keep the system temperature at 80°C for 5 hours.

[0048] Step 2) Use di-n-butylamine titration method to measure the content of -NCO group in the system. When the conversion rate reaches 50%, stop heating, cool to 60 ° C, then add hydroxyethyl acrylate (0.73g, about 6.3mmol) and polymerization inhibitor hydroquinone (0.035g, about 0.05%), after the system is stable, the temperature is...

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Abstract

The invention discloses a photocurable energetic adhesive for additive manufacturing and a synthesis method thereof, and belongs to the field of energetic materials. The preparation method comprises the following steps of: taking an aliphatic polyether intermediate containing an azide group (-N3) as an initial raw material, and then carrying out end capping by using diisocyanate and hydroxyl acrylate to obtain the bifunctional azide polyether urethane acrylate. The azide polyether urethane acrylate has the photocuring characteristic and lower viscosity, can be molded and manufactured by applying a 3D printing technology when being matched with a proper reactive diluent, in addition, the azide polyether urethane acrylate is endowed with certain flexibility and good low-temperature mechanical property by virtue of the structure of a polyether main chain and terminal urethane, the glass transition temperature is between -20DEG C and -60DEG C, and the basic requirements of a propellant adhesive are met.

Description

technical field [0001] The invention relates to a light-curing energetic adhesive and a synthesis method thereof, belonging to the field of energetic materials. Background technique [0002] The binder is the core component of the solid propellant. In addition to being able to burn to provide energy for the solid propellant, it is liquid before solidification and can be used as a dispersed phase for other solid fillers to mix them uniformly to ensure stable combustion. After curing, it has a certain toughness as an elastomer, which can provide good impact resistance for solid propellants. [0003] The traditional adhesive curing method is thermal curing, that is, using long-chain diols such as HTPB and GAP as prepolymers, adding diisocyanate to crosslink and cure under heating conditions. Although the traditional thermal curing method is widely used, it has the disadvantages of long curing time, volatile solvents, and high temperature that easily cause many side reactions. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/50C08G18/67C06B45/10C06B21/00B33Y70/00C06D5/00
CPCC08G18/5021C08G18/672C06B45/10C06B21/0033B33Y70/00C06D5/00
Inventor 蔺向阳彭洋郑文芳刘征哲张西亚郭本月史少芳张弼凤李恒檀成袁璟
Owner NANJING UNIV OF SCI & TECH