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Three-degree-of-functionality terminal alkenyl energetic adhesive and synthesis method thereof

A technology with three functionalities and synthetic methods, which is applied in the direction of adhesive types, polyether adhesives, adhesives, etc., and can solve the problems of elastomers without energy

Active Publication Date: 2018-09-21
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the elastomer formed after curing has no energy and the tensile strength is only 0.45MPa

Method used

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  • Three-degree-of-functionality terminal alkenyl energetic adhesive and synthesis method thereof
  • Three-degree-of-functionality terminal alkenyl energetic adhesive and synthesis method thereof
  • Three-degree-of-functionality terminal alkenyl energetic adhesive and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 22g (10mmol) trifunctional poly 3-nitrate methyl-3-methyloxetane in a four-necked round bottom flask equipped with mechanical stirring, reflux condenser, thermometer, dropping funnel, at temperature At 50°C, add 2.49g (30mmol) 3-propene isocyanate dropwise for 10 minutes. After the dropwise addition, raise the temperature to 77°C to continue the reaction for 12 hours, and remove unreacted 3-propene isocyanate under reduced pressure. 24.4 g of a pale yellow viscous liquid were obtained.

[0024] Structure Identification:

[0025] IR, ν max (cm -1 ): 3443 (-NH), 1727 (-C=O), 1518 (amide II peak C-N-H), 1112 (fatty ether C-O-C), 1632, 1281, 869 (-ONO 2 ).

[0026] 1 H NMR (CDCl 3 ,500MHz): δ5.70~5.80(m,1H),5.20~5.30(m,2H),4.31~4.49(m,12H),4.39~4.41(m,2H),3.25~3.37(m,24H) ,0.96~1.00(m,18H);

[0027] 13 C NMR (CDCl 3 ,125MHz): δ155.97, 134.37, 116.31, 75.84, 74.93, 73.77, 71.51, 66.55, 43.51, 40.40, 23.32, 17.33, 16.93, 7.51.

[0028] The number average molecu...

Embodiment 2

[0031] Add 22g (10mmol) trifunctional poly 3-nitrate methyl-3-methyloxetane in a four-necked round bottom flask equipped with mechanical stirring, reflux condenser, thermometer, dropping funnel, at temperature At 50°C, add 2.66g (32mmol) 3-propene isocyanate dropwise for 10 minutes. After the dropwise addition, raise the temperature to 77°C to continue the reaction for 18 hours, and remove unreacted 3-propene isocyanate under reduced pressure. 24.6 g of a pale yellow viscous liquid were obtained.

Embodiment 3

[0033] Add 22g (10mmol) trifunctional poly 3-nitrate methyl-3-methyloxetane in a four-necked round bottom flask equipped with mechanical stirring, reflux condenser, thermometer, dropping funnel, at temperature At 50°C, add 2.82g (34mmol) 3-propene isocyanate dropwise for 10 minutes. After the dropwise addition, raise the temperature to 77°C to continue the reaction for 18 hours, and remove unreacted 3-propene isocyanate under reduced pressure. 24.8 g of a pale yellow viscous liquid were obtained.

[0034] The application properties of the trifunctional alkenyl-terminated energetic adhesive of the present invention:

[0035] 1) Viscosities of trifunctional alkenyl-terminated energetic adhesives at different temperatures

[0036] The viscosities at different temperatures of the trifunctional alkenyl-terminated energetic adhesives prepared by the present invention are tested respectively, and the obtained data are as follows:

[0037] Table 1 Viscosities of trifunctional alkeny...

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Abstract

The invention discloses a three-degree-of-functionality terminal alkenyl energetic adhesive and a synthesis method thereof. The structural formula of the three-degree-of-functionality terminal alkenylenergetic adhesive is shown in a formula (I). The synthesis process comprises the following steps: taking three-degree-of-functionality poly3-methyl nitrate-3-methoxy heteroxane as a raw material, adding 3-propylene isocyanate and performing addition reaction to obtain the three-degree-of-functionality terminal alkenyl energetic adhesive. The synthesis method is convenient to prepare on a large scale, and double bonds give room-temperature curing ability to the adhesive. The three-degree-of-functionality terminal alkenyl energetic adhesive is mainly applied to a composite solid propellant. The formula is as shown in the description, wherein m is an integer of 5 to 10.

Description

technical field [0001] The invention relates to a trifunctional alkenyl-terminated energetic adhesive, which belongs to the field of solid propellants. Background technique [0002] At present, the isocyanate curing system has the problem of high curing temperature. The isocyanate curing system used in the curing of hydroxyl-terminated polybutadiene (HTPB) can be cured to produce polyurethane, and the curing temperature is high and sensitive to moisture. For example, the isocyanate curing agent system composed of toluene diisocyanate (TDI) and HTPB has a curing temperature of 60 ℃. [0003] In order to solve the problem of high curing temperature and sensitivity to moisture in traditional curing methods, room temperature curing technology of nitrile oxide was developed. Due to the high activity of the curing agent nitrile oxide, it is very easy to undergo a curing crosslinking reaction with the double bond-containing adhesive, so the curing temperature of this curing syste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J171/00C08G65/48C08G65/333
CPCC08G65/33351C08G65/48C09J171/00
Inventor 王晓川卢先明莫洪昌舒远杰徐明辉刘宁汪伟朱勇张倩
Owner XIAN MODERN CHEM RES INST
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