CN102320906B - Amide-type aid and preparation method thereof - Google Patents
Amide-type aid and preparation method thereof Download PDFInfo
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- CN102320906B CN102320906B CN 201110234550 CN201110234550A CN102320906B CN 102320906 B CN102320906 B CN 102320906B CN 201110234550 CN201110234550 CN 201110234550 CN 201110234550 A CN201110234550 A CN 201110234550A CN 102320906 B CN102320906 B CN 102320906B
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Abstract
The invention relates to an amide-type aid and a preparation method thereof, which belong to the field of the manufacture of a compound solid propellant. The amide-type aid is produced through the reaction of triethylene tetramine and linoleic acid dimer, and the wetting states of the solid particles of the solid propellant and an adhesive system can be markedly improved, so that the solid particles are easily dispersed, the structural strength for blocking the flow at the inner part of a medicine slurry is reduced, the yield value and the viscidity of the medicine slurry are decreased, and meanwhile, the mechanical performance of the propellant is not influenced.
Description
Technical field
The invention belongs to composite solidpropellant and make the field, be specifically related to a kind of amide-type aid and preparation method thereof.
Background technology
The highly filled solid energetic material that the composite solidpropellant material is comprised of bonder system, softening agent, metal fine powder (such as aluminium powder, magnesium powder etc.), oxygenant micro mist (such as ammoniumper chlorate, potassium perchlorate etc.), catalyzer and relevant auxiliary agent.Its manufacturing processed mainly comprises the weighing of each component of material prescription, mixing, cast and curing molding.Cast is the technological process of carrying out under composite solidpropellant medicine slurry flow state, and the quality of medicine sizing process performance is directly connected to pourability, the levelling property of composite solidpropellant, finally affects the quality of product.From the sixties in last century, the composite solidpropellant industry successively by choosing suitable process auxiliaries, reduces the viscosity of medicine slurry both at home and abroad, reduces yield value, improve the flowability of medicine slurry, levelling property prolongs the working life that medicine is starched, and used process auxiliaries mainly contains fatty acid methyl esters, Yelkin TTS and Great Britain's washing composition, P contained compound, these process auxiliaries applicable poor, or usage quantity is more, influential to mechanical property and the aging resistance of prescription.At present, general amides can speed adhesive to the wetting speed of solid packing, improve the suspensoid rheological property, can effectively improve the processing performance of propelling agent, consumption is few, falls low viscous effect remarkable, but can affect the mechanical property of propelling agent.
Summary of the invention
The invention provides a kind of amide-type aid and preparation method thereof, reach its volume low and reduce the viscosity successful, improve simultaneously the purpose of mechanical property.
A kind of amide-type aid of the present invention is mixture, a kind of amide-type aid, comprise substance A: N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl)-10-(2-(8-(2-(2-(2-ammonia ethylamino) ethylamino) ethylamino)-8-oxo octyl group)-5,6-dihexyl-3-cyclohexenyl) 9-decene acid amides; Substance B: 10-2-(1, two (8-(2-(2-(2-ammonia ethylamino) ethylamino) ethylamino)-8-oxo octyl group)-3 of 5-, 4,8-, three hexyls-1,2,3,4,4a, 5,8,8a-octalin base)-N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl) 9-decene acid amides; Substance C: N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl) 18 carbon-9, the 11-diene amide.
The quality percentage composition of described three kinds of compounds is respectively: substance A: 0 ~ 4.8%, and substance B: 83.4% ~ 95.5%, substance C: 0 ~ 11.8%.
The preparation method is: the linolic acid dimeracid is added in the reactor, pass into nitrogen, when temperature in the kettle rises to 95-105 ℃; triethylene tetramine is added wherein, continue to be warming up to 155-160 ℃, begin to carry out acylation reaction in the still; keep temperature in the kettle at 160 ℃ ~ 180 ℃ lower reaction 2h; continue to be warming up to 238 ℃, keep this thermotonus 1.5h, when reacting without water generates; reaction is finished; begin cooling, change vacuum distillation apparatus and steam excessive triethylene tetramine, namely get amide-type aid.
The content of described triethylene tetramine is greater than 99.5%.
The content of described linolic acid dimeracid is controlled at 85% ~ 92%.
The mole proportioning of described triethylene tetramine and linolic acid dimeracid is 2.5:1.
Amide-type aid provided by the invention, in the composite solidpropellant prescription, add 0.05%, can significantly improve the wetting regime of solids and the adhesive composition of solid propellant, so that solids are easy to disperse, reduce the structural strength that medicine slurry internal constraint flows, reduced yield value and the viscosity of medicine slurry.Medicine slurry initial viscosity reduces by 30%, and medicine slurry levelling property is good, and reach more than the 4h working life of medicine slurry.Mechanical properties of propellant is not affected simultaneously.
Embodiment
Embodiment 1: be that 85% linolic acid dimeracid adds in the reactor with content; pass into nitrogen; when temperature in the kettle rises to 95 ℃; content is added wherein greater than 99.5% triethylene tetramine; the mole proportioning of triethylene tetramine and linolic acid dimeracid is 2.5:1; continue to be warming up to 155 ℃; begin in the still to carry out acylation reaction, keep temperature in the kettle at 160 ℃ ~ 180 ℃ lower reaction 2h, continue to be warming up to 238 ℃; keep this thermotonus 1.5h; when reacting without water generates, reaction is finished, and begins cooling; change vacuum distillation apparatus and steam excessive triethylene tetramine, namely get amide-type aid.
Embodiment 2: be that 90% linolic acid dimeracid adds in the reactor with content; pass into nitrogen; when temperature in the kettle rises to 100 ℃; content is added wherein greater than 99.5% triethylene tetramine; the mole proportioning of triethylene tetramine and linolic acid dimeracid is 2.5:1; continue to be warming up to 157 ℃; begin in the still to carry out acylation reaction, keep temperature in the kettle at 160 ℃ ~ 180 ℃ lower reaction 2h, continue to be warming up to 238 ℃; keep this thermotonus 1.5h; when reacting without water generates, reaction is finished, and begins cooling; change vacuum distillation apparatus and steam excessive triethylene tetramine, namely get amide-type aid.
Embodiment 3: be that 92% linolic acid dimeracid adds in the reactor with content; pass into nitrogen; when temperature in the kettle rises to 105 ℃; content is added wherein greater than 99.5% triethylene tetramine; the mole proportioning of triethylene tetramine and linolic acid dimeracid is 2.5:1; continue to be warming up to 160 ℃; begin in the still to carry out acylation reaction, keep temperature in the kettle at 160 ℃ ~ 180 ℃ lower reaction 2h, continue to be warming up to 238 ℃; keep this thermotonus 1.5h; when reacting without water generates, reaction is finished, and begins cooling; change vacuum distillation apparatus and steam excessive triethylene tetramine, namely get amide-type aid.
The amide-type aid that obtains contains substance A: N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl)-10-(2-(8-(2-(2-(2-ammonia ethylamino) ethylamino) ethylamino)-8-oxo octyl group)-5,6-dihexyl-3-cyclohexenyl) 9-decene acid amides; Substance B: 10-2-(1, two (8-(2-(2-(2-ammonia ethylamino) ethylamino) ethylamino)-8-oxo octyl group)-3 of 5-, 4,8-, three hexyls-1,2,3,4,4a, 5,8,8a-octalin base)-N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl) 9-decene acid amides; Substance C: N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl) 18 carbon-9, the 11-diene amide.
The quality percentage composition of described three kinds of compounds is respectively: substance A: 0 ~ 4.8%, and substance B: 83.4% ~ 95.5%, substance C: 0 ~ 11.8%.
Substance A: N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl) 18 carbon-9, the 11-diene amide.
N-(2-(2-(2-aminoethylamino)ethylamino)ethyl)octadeca-9,11-dienamide
The molecular formula of substance B: N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl)-10-(2-(8-(2-(2-(2-ammonia ethylamino) ethylamino) ethylamino)-8-oxo octyl group)-5,6-dihexyl-3-cyclohexenyl) 9-decene acid amides is as follows:
N-(2-(2-(2-aminoethylamino)ethylamino)ethyl)-10-(2-(8-(2-(2-(2-aminoethylamino)ethylamino)ethylamino)-8-oxooctyl)-5,6-dihexylcyclohex-3-enyl)dec-9-enamide
Substance C: 10-2-(1, two (8-(2-(2-(2-ammonia ethylamino) ethylamino) ethylamino)-8-oxo octyl group)-3 of 5-, 4,8-, three hexyls-1,2,3,4,4a, 5,8,8a-octalin base)-molecular structural formula of N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl) 9-decene acid amides is as follows:
10-(1,5-bis(8-(2-(2-(2-aminoethylamino)ethylamino)ethylamino)-8-oxooctyl)-3,4,8-trihexyl-1,2,3,4,4a,5,8,8a-octahydronaphthalen-2-yl)-N-(2-(2-(2-aminoethylamino)ethylamino)ethyl)dec-9-enamide。
Claims (5)
1. amide-type aid, comprise substance A: N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl)-10-(2-(8-(2-(2-(2-ammonia ethylamino) ethylamino) ethylamino)-8-oxo octyl group)-5,6-dihexyl-3-cyclohexenyl) 9-decene acid amides; Substance B: 10-2-(1, two (8-(2-(2-(2-ammonia ethylamino) ethylamino) ethylamino)-8-oxo octyl group)-3 of 5-, 4,8-, three hexyls-1,2,3,4,4a, 5,8,8a-octalin base)-N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl) 9-decene acid amides; Substance C: N-(2-(2-(2-ammonia ethylamino) ethylamino) ethyl) 18 carbon-9, the 11-diene amide, the quality percentage composition of described three kinds of materials is respectively: substance A: 0 ~ 2.8%, and substance B: 86.0% ~ 94.4%, substance C: 5.6% ~ 11.2%.
2. the preparation method of a kind of amide-type aid claimed in claim 1; it is characterized in that: the linolic acid dimeracid is added in the reactor; pass into nitrogen; when temperature in the kettle rises to 95 ℃ ~ 105 ℃; triethylene tetramine is added wherein; continue to be warming up to 155-160 ℃; begin in the still to carry out acylation reaction, keep temperature in the kettle at 160 ℃ ~ 180 ℃ lower reaction 2h, continue to be warming up to 238 ℃; keep this thermotonus 1.5h; when reacting without water generates, reaction is finished, and begins cooling; steam excessive triethylene tetramine with vacuum distillation apparatus, namely get amide-type aid.
3. the preparation method of a kind of amide-type aid according to claim 2, it is characterized in that: the content of described triethylene tetramine is greater than 99.5%.
4. the preparation method of a kind of amide-type aid according to claim 2, it is characterized in that: the content of described linolic acid dimeracid is controlled at 85% ~ 92%.
5. the preparation method of a kind of amide-type aid according to claim 2, it is characterized in that: the mole proportioning of described triethylene tetramine and linolic acid dimeracid is 2.5:1.
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| CN102320906B true CN102320906B (en) | 2013-03-06 |
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| CN103113556B (en) * | 2013-03-10 | 2014-12-10 | 齐鲁工业大学 | Preparation method of curing agent suitable for epoxy resin base microporous ceramic molding die |
| CN107628969B (en) * | 2017-10-21 | 2020-05-01 | 湖北三江航天江河化工科技有限公司 | Amide auxiliary agent for composite solid propellant and synthetic method thereof |
| CN112986055B (en) * | 2021-03-19 | 2023-06-09 | 西安近代化学研究所 | Propellant slurry leveling property detection and analysis system |
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Inventor after: Zhang Hao Inventor after: Duan Junhong Inventor after: Niu Caoping Inventor after: Song Huaibing Inventor after: He Yifeng Inventor after: Cui Ruixi Inventor after: Zheng Hua Inventor after: Huang Zhanghua Inventor after: Li Fangshuo Inventor after: Yang Xiangping Inventor after: Yin Yihua Inventor after: Nie Jiaorong Inventor before: He Yifeng Inventor before: Cui Ruixi Inventor before: Zheng Hua Inventor before: Yang Xiangping Inventor before: Yin Yihua Inventor before: Nie Jiaorong Inventor before: Duan Junhong Inventor before: Niu Caoping Inventor before: Song Huaibing |
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Free format text: CORRECT: INVENTOR; FROM: HE YIFENG CUI RUIXI ZHENG HUA YANG XIANGPING YIN YIHUA NIE JIAORONG DUAN JUNHONG NIU CAOPING SONG HUAIBING TO: ZHANG HAO HE YIFENG CUI RUIXI ZHENG HUA HUANG ZHANGHUA LI FANGSHUO YANG XIANGPING YIN YIHUA NIE JIAORONG DUAN JUNHONG NIU CAOPING SONG HUAIBING |
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