JP2981592B2 - Azide and nitrato group-containing solid propellants - Google Patents
Azide and nitrato group-containing solid propellantsInfo
- Publication number
- JP2981592B2 JP2981592B2 JP7057298A JP5729895A JP2981592B2 JP 2981592 B2 JP2981592 B2 JP 2981592B2 JP 7057298 A JP7057298 A JP 7057298A JP 5729895 A JP5729895 A JP 5729895A JP 2981592 B2 JP2981592 B2 JP 2981592B2
- Authority
- JP
- Japan
- Prior art keywords
- group
- propellant
- azide
- combustion
- prepolymer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
- C06B45/06—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component
- C06B45/10—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive the solid solution or matrix containing an organic component the organic component containing a resin
- C06B45/105—The resin being a polymer bearing energetic groups or containing a soluble organic explosive
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Molecular Biology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Air Bags (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、アジド基を含有する高
エネルギ−化されたプレポリマ−を用い、これに触媒を
配合することにより燃焼特性を改良した固体推進薬に関
する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a solid propellant having improved combustion characteristics by using a high energy prepolymer containing an azide group and blending a catalyst with the prepolymer.
【０００２】[0002]
【従来の技術】従来の固体推進薬は、酸化剤と燃料成分
からなるコンポジット推進薬と、ニトログリセリンとニ
トロセルロ−スを主成分とするダブルベ−ス推進薬とに
大別される。2. Description of the Related Art Conventional solid propellants are roughly classified into a composite propellant comprising an oxidizing agent and a fuel component, and a double-base propellant comprising nitroglycerin and nitrocellulose as main components.
【０００３】コンポジット推進薬に使用される酸化剤と
しては、過塩素酸アンモニウムや硝酸アンモニウム等が
使用され、燃料兼結合剤としては、ポリウレタン、ポリ
ブタジエン等が使用され、その他金属燃料としては、ア
ルミ粉末等が用いられる。このコンポジット推進薬は、
ダブルベ−ス推進薬に比べ高い比推力を有することか
ら、広く利用されている。As an oxidizing agent used for the composite propellant, ammonium perchlorate, ammonium nitrate, or the like is used. As a fuel / binder, polyurethane, polybutadiene, or the like is used. As another metal fuel, aluminum powder or the like is used. Is used. This composite propellant
It is widely used because it has higher specific thrust than double base propellants.
【０００４】しかし、この中で最も広く使用されている
過塩素酸アンモニウムを酸化剤とするコンポジット推進
薬は、燃焼時に生成する塩化水素の問題から、酸化剤と
して分子内に塩素を含まないニトラミン化合物を用いた
無煙性コンポジット推進薬の研究が近年盛んに行われて
いる。However, among these, the most widely used composite propellant using ammonium perchlorate as an oxidizing agent is a nitramine compound containing no chlorine in the molecule as an oxidizing agent due to the problem of hydrogen chloride generated during combustion. In recent years, studies on smokeless composite propellants using phenol have been actively conducted.
【０００５】さらに、ニトラミン化合物の酸素不足を補
い燃焼性能を向上させるために、燃料成分いわゆるバイ
ンダ−を高エネルギ−化したものが用いられるようにな
った。そのバインダ−として現在研究されているものと
して、熱分解により窒素分子を生成して多量の反応熱を
放出するアジド基を有するポリマ−や、分子内に酸素を
多量にもち、熱分解によって発生ガス量が多いニトラト
基を有するポリマ−が注目されている。Further, in order to improve the combustion performance by supplementing the oxygen deficiency of the nitramine compound, a fuel component having a high energy, that is, a binder, has been used. As binders that are currently being studied, polymers having azide groups that generate nitrogen molecules by thermal decomposition and release a large amount of reaction heat, and gases that have a large amount of oxygen in the molecules and are generated by thermal decomposition Attention has been directed to polymers having a large amount of nitrato groups.
【０００６】[0006]
【発明が解決しようとする課題】ニトラミンを酸化剤、
バインダ−にアジド基及びニトラト基を有するポリマ−
を用いた推進薬は、燃焼性能のうち圧力指数が極めて高
いという問題があった。一般的に燃焼速度ｒは ｒ＝ａＰn ａ：定数 Ｐ：圧力 ｎ：圧力指数 の関係が成立することが経験的に知られている。この意
味するところは、燃焼圧力を増加することにより燃焼速
度が増大するということであるが、ｎが大きい場合、わ
ずかの圧力上昇で燃焼速度が大きく変わることを意味す
る。SUMMARY OF THE INVENTION Nitramin is used as an oxidizing agent,
Polymer having azide group and nitrato group in binder
The propellant using the compound has a problem that the pressure index is extremely high in the combustion performance. Generally burn rate r is r = aP n a: Constant P: Pressure n: is the relationship of the pressure index is established known empirically. This means that the combustion speed is increased by increasing the combustion pressure. However, when n is large, it means that the combustion speed is greatly changed by a slight pressure increase.
【０００７】従って、燃焼圧力の変動を押さえるため燃
焼面積及びノズルスロ−ト面積を極めて正確に維持しな
ければ、信頼性の高いロケットは得られにくい。これを
避けるため、圧力指数ｎは一般に１．０以下が好まし
く、現状０．５以下が固体推進薬として用いられてい
る。Therefore, unless the combustion area and the nozzle slot area are maintained extremely accurately in order to suppress fluctuations in combustion pressure, it is difficult to obtain a highly reliable rocket. In order to avoid this, the pressure index n is generally preferably 1.0 or less, and currently 0.5 or less is used as a solid propellant.
【０００８】本発明は、こうした実情の下に、比推力及
び燃焼速度が大きく、且つアジド基及びニトラト基含有
ポリマ−を用いた固体推進薬の圧力指数を低下させた固
体推進薬を提供することを目的とするものである。[0008] Under the circumstances, the present invention provides a solid propellant having a high specific impulse and a burning rate, and having a reduced pressure index of a solid propellant using a polymer containing an azide group and a nitrate group. It is intended for.
【０００９】[0009]
【課題を解決するための手段】本発明者らは、前記の問
題点を考慮し鋭意研究した結果、燃料結合剤の主成分が
アジド基及びニトラト基を含有するプレポリマ−、好ま
しくは３，３−ビス（アジドメチル）オキセタンと３−
ニトラトメチル−３−メチルオキセタンである燃料結合
剤に酸化剤としてシクロ−１，３，５−トリメチレン−
２，４，６−トリニトラミン（ＲＤＸ）、シクロ−１，
３，５，７−テトラメチレン−２，４，６，８−テトラ
ニトラミン（ＨＭＸ）の様なニトラミンにクエン酸鉛、
及びカ−ボンを配合することにより無煙性で高エネルギ
−をもち且つ圧力指数を低下できるという特性を見いだ
し、本発明を完成するに至った。The present inventors have made intensive studies in consideration of the above problems, and as a result, have found that the main component of the fuel binder is a prepolymer containing an azide group and a nitrate group, preferably 3,3. -Bis (azidomethyl) oxetane and 3-
Cyclo-1,3,5-trimethylene- is used as an oxidant in a fuel binder which is nitratomethyl-3-methyloxetane.
2,4,6-trinitramine (RDX), cyclo-1,
Lead citrate to a nitramine such as 3,5,7-tetramethylene-2,4,6,8-tetranitramine (HMX),
By blending carbon and carbon, it has been found that it is smokeless, has high energy, and can reduce the pressure index, and has completed the present invention.
【００１０】本発明において使用されるアジド基含有プ
レポリマ−としては、アジド基を含有するポリマ−であ
れば、特に制限はなく例えば、３−アジドメチル−３−
メチルオキセタン（ＡＭＭＯ）、グリシジルアジドポリ
マー（ＧＡＰ）、３，３−ビス（アジドメチル）オキセ
タン（ＢＡＭＯ）等が一般的である。The azide group-containing prepolymer used in the present invention is not particularly limited as long as it is a polymer containing an azide group. For example, 3-azidomethyl-3-
Methyl oxetane (AMMO), glycidyl azide polymer (GAP), 3,3-bis (azidomethyl) oxetane (BAMO) and the like are common.
【００１１】また、ニトラト基含有プレポリマ−として
は、３−ニトラトメチル−３−メチルオキセタン（ＮＭ
ＭＯ）、３，３−ビス（ニトラトメチル）オキセタン
（ＢＮＭＯ）等が一般的である。Further, as the nitrato group-containing prepolymer, 3-nitratomethyl-3-methyloxetane (NM
MO), 3,3-bis (nitratomethyl) oxetane (BNMO) and the like.
【００１２】この中で、ＢＡＭＯはアジド基の含有量が
最も多く、従ってエネルギ−が大きいがこのポリマ−
は、常温で固体である。従って、下記（１）式で表され
る如きニトラト基含有のＮＭＭＯと共重合することによ
り、常温で液状にすることができる（ＵＳＰ ５０９９
０４２）ため推進薬としての燃料結合剤として使用可能
となる。Among them, BAMO has the highest content of azide group, and therefore has a large energy.
Is a solid at room temperature. Therefore, by copolymerizing with a nitrate group-containing NMMO represented by the following formula (1), it can be made liquid at normal temperature (USP 5099).
042), so that it can be used as a fuel binder as a propellant.
【００１３】[0013]
【化１】 Embedded image
【００１４】注：上記は、ブロックコポリマ−及びラン
ダムコポリマ−を含む。Note: The above includes block copolymers and random copolymers.
【００１５】なお、このプレポリマ−共重合体にオキセ
タンやテトラヒドロフラン等の第３成分を加えて共重合
することもでき、この様な第３成分を加えたものでも良
い。これらのプレポリマ−は末端水酸基をもち、これを
主成分とするバインダ−とするため、硬化剤は水酸基と
反応するイソシアネ−ト化合物、例えばトリレンジイソ
シアネ−ト、イソホロンジイソシアネ−ト、ヘキサメチ
レンジイソシアネ−トジフェニルメタンジイソシアネ−
ト、トリフェニルジメチレントリイソシアネ−ト、トリ
フェニルメタントリイソシアネ−ト等を用いる。The prepolymer may be copolymerized by adding a third component such as oxetane or tetrahydrofuran, or the prepolymer may be added with such a third component. Since these prepolymers have a terminal hydroxyl group and serve as a binder mainly containing the terminal hydroxyl group, the curing agent is an isocyanate compound which reacts with the hydroxyl group, for example, tolylene diisocyanate, isophorone diisocyanate, and hexane. Methylene diisocyanate-to-diphenylmethane diisocyanate
, Triphenyldimethylenetriisocyanate, triphenylmethanetriisocyanate and the like.
【００１６】架橋剤は、多官能の水酸基をもつ化合物、
例えばトリメチロ−ルエタン、トリメチロ−ルプロパ
ン、グリセリン、ヘキサントリオ−ル、ジグリセリン等
や、多官能イソシアネ−トが用いられる。The crosslinking agent is a compound having a polyfunctional hydroxyl group,
For example, trimethylolethane, trimethylolpropane, glycerin, hexanetriol, diglycerin and the like, and polyfunctional isocyanates are used.
【００１７】可塑剤は、ジオクチルアジペ−ト、ジエチ
ルフタレ−ト等のエステル系や、ジ（ブチルジグリコ−
ル）アジペ−トのようなエ−テルとエステル結合をもっ
た化合物等、プレポリマ−と相溶性が良好なものを用い
る。The plasticizer may be ester-based such as dioctyl adipate or diethyl phthalate, or di (butyldiglycol-
B) A compound having good compatibility with the prepolymer, such as a compound having an ester bond with an ether such as adipate is used.
【００１８】硬化触媒は、ブチルチントリクロライド、
ジブチルチンジアセテ−ト、ジブチルチンジラウレ−ト
等の有機錫化合物や、フェリックアセチルアセトン、フ
ェリックジフェニルアセチルアセトン等の有機鉄化合物
等を用いる。The curing catalyst is butyltin trichloride,
Organic tin compounds such as dibutyltin diacetate and dibutyltin dilaurate, and organic iron compounds such as ferric acetylacetone and ferric diphenylacetylacetone are used.
【００１９】添加する鉛化合物は、クエン酸鉛が用いら
れる。その際、カ−ボンの添加が必要であり、鉛化合物
だけでは、効果を示さない。As the lead compound to be added, lead citrate is used. At that time, addition of carbon is necessary, and the effect is not exhibited only by the lead compound.
【００２０】その添加量は、固体推進薬に対して外割
で、好ましくは２〜４％であり、この時の圧力指数が最
も低い値を示しこれ以下では効果を現さず、また、それ
以上添加しても効果がなく、エネルギ−も低下する。ま
た、カ−ボンの添加量は、固体推進薬に対して外割で
０．１〜３％、好ましくは０．３〜０．８％とする。ま
た、３％より多いと推進薬の粘度が上昇し製造性が悪
く、０．１％より少ないと効果が現れない。The amount of the additive is preferably 2 to 4%, based on the solid propellant, and the pressure index at this time shows the lowest value. There is no effect even if added, and the energy is reduced. The amount of carbon added is 0.1 to 3%, preferably 0.3 to 0.8%, based on the solid propellant. On the other hand, if it is more than 3%, the viscosity of the propellant increases and the productivity is poor. If it is less than 0.1%, no effect is exhibited.
【００２１】[0021]
【実施例】以下に、本発明を実施例によって具体的に説
明する。The present invention will be specifically described below with reference to examples.
【００２２】表１に示す組成により各種推進薬を製造し
た。アジド基及びニトラト基含有プレポリマ−として
は、ＢＡＭＯ／ＮＭＭＯをモル比で７対３の共重合体を
用いた。まず、プレポリマ−と硬化触媒、架橋剤、可塑
剤及び硬化剤を加温で混合し、その中に燃焼触媒を添加
し、さらにＨＭＸを投入したのち混合・脱泡した。硬化
は、６０℃で約７日間行った。Various propellants were manufactured according to the compositions shown in Table 1. As the azide group and nitrato group-containing prepolymer, a BAMO / NMMO copolymer having a molar ratio of 7: 3 was used. First, a prepolymer, a curing catalyst, a cross-linking agent, a plasticizer, and a curing agent were mixed by heating, a combustion catalyst was added thereto , and HMX was further added, followed by mixing and defoaming. Curing was performed at 60 ° C. for about 7 days.
【００２３】[0023]
【表１】 [Table 1]
【００２４】表１に示す各種推進薬を用いて、以下の方
法により燃焼速度等を調べた。Using various propellants shown in Table 1, the burning rate and the like were examined by the following method.
【００２５】固体推進薬を外径７ｍｍ角、長さ７０ｍｍ
の円柱に切り出し円柱状の側面に、約１ｍｍ厚さの樹脂
層（燃焼制御層）を形成し、試料を作製した。このよう
な試料は、ストランド推進薬と一般に呼ばれる。ストラ
ンド推進薬の一端より約１０ｍｍの所に点火用のニクロ
ム線を通し、また一端から２０ｍｍと６０ｍｍの箇所に
ヒュ−ズ線を通した。ストランド推進薬を圧力容器内に
密閉し加圧下でニクロム線によりニクロム線に通電し着
火燃焼させ、２本のヒュ−ズ線が切断した時間差でヒュ
−ズ線間（ここでは、４０ｍｍ）を除した値として、燃
焼速度とする。この測定は加圧下で行うが、燃焼容器と
ストランド推進薬燃焼中に一定圧に保つために十分な容
量をもつ蓄圧器とが連結されたストランド燃焼器を用
い、燃焼容器中にストランド推進薬をセットし、所定圧
に窒素ガスで加圧したのち着火するものとする。[0025] A solid propellant has an outer diameter of 7 mm square and a length of 70 mm.
A resin layer (combustion control layer) having a thickness of about 1 mm was formed on the cylindrical side surface to prepare a sample. Such a sample is commonly called a strand propellant. A nichrome wire for ignition was passed about 10 mm from one end of the strand propellant, and a fuse wire was passed 20 mm and 60 mm from one end. The strand propellant is sealed in a pressure vessel, and the Nichrome wire is energized with the Nichrome wire under pressure to ignite and burn, and the time difference between the two fuse wires is cut by the time difference between the fuse wires (here, 40 mm). The calculated value is the burning speed. This measurement is performed under pressure, but using a strand combustor in which the combustion vessel and an accumulator with sufficient capacity to maintain a constant pressure during the combustion of the strand propellant are connected, the strand propellant is injected into the combustion vessel. It is assumed that the ignition is carried out after setting and pressurizing to a predetermined pressure with nitrogen gas.
【００２６】この様な方法で、加圧圧力を変えて繰り返
し燃焼速度を、測定した。In this way, the burning rate was measured repeatedly while changing the pressure.
【００２７】得られた各種推進薬の燃焼速度を表２に示
す。Table 2 shows the burning rates of the various propellants obtained.
【００２８】[0028]
【表２】 [Table 2]
【００２９】[0029]
【発明の効果】以上説明したように、燃料結合剤の主成
分がアジド基及びニトラト基を含有するポリマ−である
固体推進薬において、成分として鉛化合物及びカ−ボン
を含むことにより以下の特長を有することが判明した。As described above, the solid propellant in which the main component of the fuel binder is a polymer containing an azide group and a nitrate group includes the following features by including a lead compound and carbon as components. Was found to have.
【００３０】１．圧力指数が、従来の値に比べ極めて低
くロケットモ−タの設計が容易となり、信頼性の高いロ
ケットモ−タのための推進薬を得た。1. The pressure index was extremely low as compared with the conventional value, and the design of the rocket motor became easy, and a propellant for the rocket motor with high reliability was obtained.
【００３１】２．燃焼速度についても、低圧側で約２倍
に増加しており固体推進薬の利用範囲を拡大することが
できた。2. The combustion rate also increased about twice on the low pressure side, and the use range of the solid propellant could be expanded.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 甲斐 竜己 大分県大分市大字里2620番地 旭化成工 業株式会社内 (56)参考文献 特開 昭62−41791（ＪＰ，Ａ) 特開 平２−157177（ＪＰ，Ａ) 特開 平５−117384（ＪＰ，Ａ) 特開 昭62−12689（ＪＰ，Ａ) 特開 昭58−64298（ＪＰ，Ａ) Ｐｒｏｐｅｌｌａｎｔｓ，Ｅｘｐｌｏ ｓｉｖｅｓ，Ｐｙｒｏｔｅｃｈｎｉｃ ｓ，17［１］（1992），38−42 Ｊｏｕｒｎａｌ ｏｆ Ｅｎｅｒｇｅ ｔｉｃ Ｍａｔｅｒｉａｌｓ，13［１＆ ２］（1995），１−14 (58)調査した分野(Int.Cl.6，ＤＢ名) C06D 5/00 C06B 23/00 C06B 29/22 ＣＡ（ＳＴＮ) ＲＥＧＩＳＴＲＹ（ＳＴＮ) ＷＰＩＤＳ（ＳＴＮ)──────────────────────────────────────────────────続 き Continuation of front page (72) Inventor Tatsumi Kai 2620 Ojiri, Oita City, Oita Prefecture Asahi Kasei Corporation (56) References JP-A-62-41791 (JP, A) JP-A-2-2 157177 (JP, A) JP-A-5-117384 (JP, A) JP-A-62-12689 (JP, A) JP-A-58-64298 (JP, A) Propellants, Explosives, Pyrotechnics, 17 [1] ] (1992), 38-42 Journal of Energy Materials, 13 [1 & 2] (1995), 1-14 (58) Fields investigated (Int. Cl. 6 , DB name) C06D 5/00 C06B 23/00 C06B 29/22 CA (STN) REGISTRY (STN) WPIDS (STN)
Claims (2)
トラト基を含有するプレポリマ−であり、酸化剤がニト
ラミンである組成物に、クエン酸鉛及びカーボンを各々
２〜４％及び０．３〜０．８％添加したことを特徴とす
る固体推進薬。1. A composition in which a main component of a fuel binder is a prepolymer containing an azide group and a nitrat group, and lead citrate and carbon are added to a composition in which an oxidizing agent is nitramine.
A solid propellant, wherein 2 to 4% and 0.3 to 0.8% are added .
メチル）オキセタンと３−ニトラトメチル−３−メチル
オキセタンの共重合体であることを特徴とする請求項１
記載の固体推進薬。2. The method according to claim 1, wherein the prepolymer is a copolymer of 3,3-bis (azidomethyl) oxetane and 3-nitratomethyl-3-methyloxetane.
The solid propellant described.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7057298A JP2981592B2 (en) | 1995-03-16 | 1995-03-16 | Azide and nitrato group-containing solid propellants |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7057298A JP2981592B2 (en) | 1995-03-16 | 1995-03-16 | Azide and nitrato group-containing solid propellants |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08259366A JPH08259366A (en) | 1996-10-08 |
| JP2981592B2 true JP2981592B2 (en) | 1999-11-22 |
Family
ID=13051655
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7057298A Expired - Lifetime JP2981592B2 (en) | 1995-03-16 | 1995-03-16 | Azide and nitrato group-containing solid propellants |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2981592B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0421167D0 (en) * | 2004-09-23 | 2004-10-27 | Sec Dep For Defence Awe The | Novel energetic polyphosphazenes |
| CN111454113A (en) * | 2020-05-20 | 2020-07-28 | 湖北三江航天江河化工科技有限公司 | Hydroxyl-terminated aluminum-free propellant and preparation method thereof |
-
1995
- 1995-03-16 JP JP7057298A patent/JP2981592B2/en not_active Expired - Lifetime
Non-Patent Citations (2)
| Title |
|---|
| Ｊｏｕｒｎａｌ ｏｆ Ｅｎｅｒｇｅｔｉｃ Ｍａｔｅｒｉａｌｓ，１３［１＆２］（１９９５），１−１４ |
| Ｐｒｏｐｅｌｌａｎｔｓ，Ｅｘｐｌｏｓｉｖｅｓ，Ｐｙｒｏｔｅｃｈｎｉｃｓ，１７［１］（１９９２），３８−４２ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08259366A (en) | 1996-10-08 |
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