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Energetic room-temperature curing agent based on hydroxyl-terminated polybutadiene bonding system and solidified body thereof and preparation method thereof

A technology of hydroxyl-terminated polybutadiene and room temperature curing agent, which is applied in chemical instruments and methods, preparation of organic compounds, adhesives, etc., can solve problems such as high curing molding temperature and unsatisfactory properties of cured products, and achieve the goal of curing products containing Performance improvement, suitable for large-scale industrial production, and wide environmental adaptability

Inactive Publication Date: 2018-12-28
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems and deficiencies such as high curing molding temperature and unsatisfactory performance of the cured product in the prior art of HTPB type cast composite propellant, and provide a kind of energy-containing room-temperature curing based on hydroxyl-terminated polybutadiene bonding system Agent and its curing body and preparation method

Method used

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  • Energetic room-temperature curing agent based on hydroxyl-terminated polybutadiene bonding system and solidified body thereof and preparation method thereof
  • Energetic room-temperature curing agent based on hydroxyl-terminated polybutadiene bonding system and solidified body thereof and preparation method thereof
  • Energetic room-temperature curing agent based on hydroxyl-terminated polybutadiene bonding system and solidified body thereof and preparation method thereof

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Embodiment 1

[0045] A method for preparing an energetic room-temperature curing agent based on a hydroxyl-terminated polybutadiene bonding system, that is, a method for preparing 5-nitrobenzene-1,3-dinitrile oxide, comprising the following steps:

[0046] a. Nitration: Add 13.4g of 1,3-phthalaldehyde and 12.2g of acetyl nitrate into a 250ml three-neck flask under ice bath temperature, mix well and carry out nitration reaction at 40°C for 100 minutes; wait for the reaction to complete Finally, the reaction product is poured into ice water while it is hot (the volume consumption of ice water can be 1 to 4 times the volume of the material after the reaction, and the ice water is a mixture of ice and water with a temperature of 0 to 4 ° C, the same below), and the yellow color is immediately precipitated. Suction filter the solid, wash the solid with ice water, and dry to obtain a pale yellow 5-nitrobenzene-1,3-dicarbaldehyde solid for use;

[0047] b. Oximation: Add 17.9g of 5-nitrobenzene-1,...

Embodiment 2

[0055] A method for preparing an energetic room-temperature curing agent based on a hydroxyl-terminated polybutadiene bonding system, that is, a method for preparing 5-nitrobenzene-1,3-dinitrile oxide, comprising the following steps:

[0056] a. Nitration: Add 13.4g of 1,3-benzenedicarbaldehyde to a 250ml three-necked flask, dissolve it in 44mL of concentrated sulfuric acid, and add the mixed acid dropwise (the mixed acid is 13mL of concentrated sulfuric acid and 27mL of concentrated nitric acid) mixed acid) mixed uniformly and then carried out nitration reaction at 50°C for 80 minutes; after the reaction was completed, pour the reaction product into ice water while hot (the volume of ice water can be 1 to 4 times the volume of the material after the reaction, and the ice water can be A yellow solid was precipitated immediately in a mixture of ice and water at a temperature of 0-4°C, the same below), and was filtered with suction, washed with ice water, and dried to obtain a li...

Embodiment 3

[0065] A method for preparing an energetic room-temperature curing agent based on a hydroxyl-terminated polybutadiene bonding system, that is, a method for preparing 5-nitrobenzene-1,3-dinitrile oxide, comprising the following steps:

[0066] a. Nitration: Add 13.4g of 1,3-benzenedicarbaldehyde to a 250ml three-necked flask, dissolve it in 44mL of concentrated sulfuric acid, and add the mixed acid dropwise (the mixed acid is 13mL of concentrated sulfuric acid and 27mL of concentrated nitric acid) mixed acid) mixed uniformly and then carried out nitration reaction at 50°C for 80 minutes; after the reaction was completed, pour the reaction product into ice water while hot (the volume of ice water can be 1 to 4 times the volume of the material after the reaction, and the ice water can be A yellow solid was precipitated immediately in a mixture of ice and water at a temperature of 0-4°C, the same below), and was filtered with suction, washed with ice water, and dried to obtain a li...

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Abstract

The invention discloses an energetic room-temperature curing agent based on a hydroxyl-terminated polybutadiene bonding system, namely, 5-nitrobenzene-1, 3-dinitrile oxide. According to a preparationmethod of the energetic room-temperature curing agent based on the hydroxyl-terminated polybutadiene bonding system, with 1, 3-phthalic aldehyde as an initial raw material, the 5-nitrobenzene-1, 3-dinitrile oxide is synthesized through four steps of reactions of nitrification, oximation, halogenation and dehydrohalogenation. The invention further discloses a solidified body, which is formed by mixing hydroxyl-terminated polybutadiene and the 5-nitrobenzene-1, 3-dinitrile oxide, of the energetic room-temperature curing agent based on the hydroxyl-terminated polybutadiene bonding system. The prepared energetic room-temperature curing agent based on the hydroxyl-terminated polybutadiene bonding system, disclosed by the invention, has the advantages of good product quality, high yield and simple separation, is suitable for large-scale industrial production, is suitable for room temperature curing and forming of hydroxyl-terminated polybutadiene type cast composite propellent in a solid rocket engine and room temperature curing and forming of a HTPB type explosive mixture and can also be used for room temperature curing of other HTPB type adhesives, sealing materials and coatings.

Description

technical field [0001] The invention belongs to organic compounds and their preparation, and relates to an energetic room-temperature curing agent based on a hydroxyl-terminated polybutadiene bonding system, its cured body and a preparation method. The energetic room-temperature curing agent based on the hydroxyl-terminated polybutadiene bonding system of the present invention is suitable for the room-temperature curing molding of the hydroxyl-terminated polybutadiene (HTPB) type pouring composite propellant and the room-temperature curing molding of the HTPB mixed explosive in solid rocket motors , It can also be used for room temperature curing of other HTPB adhesives, sealing materials, coatings, etc. Background technique [0002] Composite propellant is a kind of composite gunpowder composed of fuel and explosive particles as the dispersed phase, and binder and plasticizer as the continuous phase. Tough polymer binders firmly bond the explosive components together, allo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/51C07C253/00C09J147/00C09J11/06C06B23/00C06D5/00
CPCC06B45/10C06D5/00C07C253/00C07C255/51C09J11/06C09J147/00C08K5/32
Inventor 雷永林樊亚琴
Owner SOUTHWEAT UNIV OF SCI & TECH
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