WO2000044691A1 - METHOD FOR REDUCING NO¿x? - Google Patents
METHOD FOR REDUCING NO¿x? Download PDFInfo
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- WO2000044691A1 WO2000044691A1 PCT/JP2000/000419 JP0000419W WO0044691A1 WO 2000044691 A1 WO2000044691 A1 WO 2000044691A1 JP 0000419 W JP0000419 W JP 0000419W WO 0044691 A1 WO0044691 A1 WO 0044691A1
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- gas generating
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- derivative
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
- C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
- C06D5/06—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids
Definitions
- the present invention relates to a NOX reduction method for reducing the amount of NOX generated by combustion of a gas generating agent for an airbag during an inflation of an airbag system provided for protecting a human body mounted on an automobile, an aircraft, or the like.
- sodium azide is well known as a fuel component of a gas generating agent used in an airbag system.
- a gas generator using sodium azide has a decomposition temperature of at least 400 and is excellent in heat resistance, and has no particular problem with its combustion characteristics, and is widely used in practice.
- sodium azide generates explosive compounds by reacting with heavy metals, etc., and has a low oral toxicity LD50 of 27 mg / kg for mouse rats. It is known that there is a concern about environmental pollution.
- Japanese Patent Publication No. 6-57669 discloses a gas generating agent containing a transition metal complex of tetrazole and triazol
- Japanese Patent Application Laid-Open No. 5-254977 discloses A gas generating agent containing triaminoguanidine nitrate is disclosed
- Japanese Patent Application Laid-Open No. Hei 6-23963 discloses a gas generating agent containing carbohydrazide
- Japanese Patent Application Laid-Open No. 7-61885 The gazette contains cellulose acetate and perchloric acid lime and nitrogen-containing nonmetallic compounds.
- 5,125,684 discloses a gas generating agent containing 15 to 30% of a cellulosic binder such as nitrocellulose and an energy substance;
- No. 292 discloses a gas generating composition comprising a combination of a tetrazole and triazole derivative, an oxidizing agent and a slag forming agent.
- a gas generating composition comprising a nitrogen-containing organic compound emits a chemical equivalent in combustion, that is, an amount of oxygen necessary for burning carbon, hydrogen, and other oxidizable elements in the nitrogen-containing organic compound molecule.
- a chemical equivalent in combustion that is, an amount of oxygen necessary for burning carbon, hydrogen, and other oxidizable elements in the nitrogen-containing organic compound molecule.
- NOX reduction method As a method generally known as a NOX reduction method, there is a large-scale denitration technology using a boiler or a burner that burns heavy oil, light oil, coal, propane gas, and the like.
- a selective reduction method using NH 3 to remove NO x by the following reaction There is a selective reduction method using NH 3 to remove NO x by the following reaction.
- the present invention provides a method for reducing NOx that can reduce the amount of NOx generated by the combustion of a gas generating agent for an airbag and improve safety further from the viewpoint of user protection during the inflation of an airbag system.
- the purpose is to provide.
- the inventors of the present invention have repeated studies focusing on the fact that the selective reduction method shows a certain effect as a method for reducing the amount of NOx. As a result, they found that the selective reduction method reduces the amount of N ⁇ X due to the effective reaction between the gas generated by the combustion of the gas generating agent and the gas generated from the reducing substance. Was. By further developing this principle, they have found that an effective reaction between an oxidizing gas and a reducing gas can achieve the above object, and have completed the present invention. That is, the present invention provides a NOX reduction method characterized by reducing the amount of NOX generated by simultaneously burning two or more types of gas generating agents having different oxygen balances.
- the present invention also provides an inflation system that employs the above-mentioned N ⁇ X reduction method.
- the present invention is a method for generating a gas in which the amount of generated NO X is reduced by simultaneously burning two or more types of gas generating agents having different oxygen balances in an air bag gas generator including the gas generating agent.
- the NO X reduction method of the present invention By applying the NO X reduction method of the present invention, the amount of NO X generated by combustion of the gas generating agent for an air bag can be reduced. As a result, the possibility of adversely affecting the user's health can be reduced, and the reliability and safety of the infra-system can be improved.
- this does not control combustion in the solid phase by means of a combustion catalyst or the like, but daringly generates oxidizing gas and reducing gas from two or more types of gas generating agents with different oxygen balances, and makes these effective reactions.
- the temperature is high and the pressure is high, which is favorable conditions for these gas reactions.
- the oxygen balance of the two or more gas generating agents used may be any as long as it has an effect, but is preferably -0.2 to +0.2 g / g. It is particularly preferred that it is -0.1 to +0.1 lg / g.
- the balance is preferably -0.2 to 0.2 Og / g and 0.0 to +0.2 g / g, -0.1 to 0.Og / g and 0.0 to + 0.lg / g. g is particularly preferred.
- the gas generating agent may be placed anywhere in the inflation bath if the combustion gas generated from two or more types of gas generating agents effectively reacts. Preferably, it is located in the gas generant combustion chamber.
- Two or more types of gas generating agents may be mixed well by a mixer, etc., and handled as if they were a single type of gas generating agent, or they may be completely separated and charged during inflation. .
- the gas generating agent is easy to handle and a more reliable gas reaction can be expected.
- the gas generating agent is handled separately, there is an advantage that the amount of each gas generating agent can be measured more accurately.
- the non-azide gas generating composition used in the present invention is preferably composed of a nitrogen-containing compound, an oxidizing agent, if necessary, a slag forming agent and a binder.
- the nitrogen-containing compound used in the present invention is selected from the group consisting of a guanidine derivative, a tetrazole derivative, a bititrazole derivative, a triazole derivative, a hydrazine derivative, a triazine derivative, an azodicarbonamide derivative and a disocyanamide derivative. Species or a mixture of two or more species.
- nitroguanidine examples include nitroguanidine, guanidine nitrate, 5-aminotetrazole, bittrazol diammonium salt, 5-year-old xo 1,2,4-triazolyl, cyanoguanidine, triaminoguanidine nitrate, Examples thereof include trihydrazinotriazine, biuret, azodicarbonamide, piurea, carbohydrazide, carbohydrazide nitrate complex, oxalic acid dihydrazide, hydrazine nitrate complex, and sodium disocyanamide.
- nitrogen-containing compounds one or more members selected from the group consisting of a tetrazole derivative and a guanidine derivative are preferable, and nitroguanidine, cyanoguanidine and 5-aminotetrazole are particularly preferable.
- the mixing ratio of the nitrogen-containing compound in the gas generating composition according to the present invention varies depending on the number of carbon elements, hydrogen elements and other oxidized elements in the molecular formula, but is usually in the range of 20 to 70% by weight. Is preferred, and a range of 25 to 60% by weight is particularly preferred.
- oxidizing agents can be used as the oxidizing agent used in the gas generating composition according to the present invention, and nitrates, nitrites, and perchloric acids containing cations selected from the group consisting of alkali metal and alkaline earth metal are used. At least salt and chlorate
- An oxidizing agent selected from one type is preferred.
- the nitrate containing a cation selected from an alkali metal or an alkaline earth metal include sodium nitrate, potassium nitrate, magnesium nitrate, strontium nitrate, and the like.
- the mixing ratio of the oxidizing agent in the gas generating composition according to the present invention varies in absolute value depending on the type and amount of the gas generating compound used, but is preferably in the range of 30 to 80% by weight, particularly 40 to 75% by weight. A range is preferred.
- the function of the slag forming agent in the gas generating composition according to the present invention is as follows.
- slag forming agents include acid clay, silica, bentonite-based, kaolin-based, and other naturally-occurring clays mainly composed of aluminosilicates; synthetic myc, synthetic olinite, synthetic smectite Slag forming agents selected from at least one of alumina, aluminum hydroxide, and the like.
- acid clay, Alumina or silica is preferred.
- the slag forming agent is not essential, but adding an appropriate amount to the gas generating composition is very effective.
- the mixing ratio can be varied in the range of 1 to 20% by weight, but is preferably in the range of 3 to 10% by weight. If the amount is too large, the linear burning speed and the gas generation efficiency decrease, and if the amount is too small, the slag forming ability can be sufficiently exhibited. Absent.
- any binder can be used as long as it does not significantly affect the burning behavior of the composition.
- the binder used in the present invention include metal salts of carboxymethyl cellulose, hydroxyxethyl cellulose, cellulose acetate, cellulose propionate, cellulose acetate butyrate, nitrocellulose, microcrystalline cellulose, and polyvinyl alcohol.
- Polysaccharide derivatives such as guar gum and starch; organic binders such as calcium stearate; or inorganic binders such as molybdenum disulfide, acid clay, talc, bentonite, diatomaceous earth, kaolin, silica, and alumina.
- the binder is not essential, but adding an appropriate amount to the gas generating composition is very effective.
- the compounding ratio is preferably in the range of 0 to 15% by weight. The larger the amount, the stronger the fracture strength of the molded body, but as the amount increases, the number of carbon elements and hydrogen elements in the composition increases, and a small amount of CO gas, which is an incomplete combustion product of carbon elements It is not preferable because the concentration of methane increases or the linear burning rate decreases.
- the gas generating composition of the present invention can be produced by a dry method in which a fuel for a gas generating agent, an oxidizing agent, and the like are mixed in a powder form, or a wet method in which the fuel and the oxidizing agent are mixed in the presence of water or an organic solvent.
- the gas generating composition of the present invention can be molded into a desired shape.
- compression molding using a tableting machine to produce pellets compression molding using a disk molding machine to produce discs, grinding pellets to discs, or granulation using nahiure
- it can be extruded using a drawing machine (extrusion molding machine) to make a drawn medicine (non-porous, single-hole, porous).
- drawing machine extruded using a drawing machine (extrusion molding machine) to make a drawn medicine (non-porous, single-hole, porous).
- it can be rolled and formed into a film or plate shape.
- the binder does not need to be molded or only a small amount is required, so that there is a tendency that the flammability does not decrease.
- the extrusion molding method is applied, it is easier to mold a thin web than the compression molding method, so that a molded product can be obtained even with a composition having a slow burning rate.
- the extrusion molding method is suitable for mass production because molding can be performed in a relatively short time. In the case of a composition having a high burning rate, the size of the molded product can be increased, so that the production efficiency can be further increased.
- a molded article having a complicated shape such as non-porous, single-pored, or porous can be manufactured, so that various combustion characteristics can be imparted.
- the NOX reduction method according to the present invention provides an inflation system provided with a module case containing an inflation circuit and an airbag, a judgment circuit, a sensor, and the like, which are provided for protecting a human body mounted on an automobile, an aircraft, or the like. It can be applied to the overnight system.
- a module case containing an inflation circuit and an airbag, a judgment circuit, a sensor, and the like, which are provided for protecting a human body mounted on an automobile, an aircraft, or the like. It can be applied to the overnight system.
- Nitoroguanijin a (NQ) and strontium nitrate (S r (N0 3) 2 ) were mixed so that the compositions shown in Table 1. Then, about 2 g of the mixed powder was compression-molded with a hand brace machine. A strand having a diameter of 9.6 mm and a length of about 14 mm was obtained. table 1
- Example 1 The strands of Example 1 were burned in the combinations shown in Table 2, and the gas after combustion was analyzed to confirm the NOX reduction effect of the present invention.
- the strand was burned in a 1 liter combustion vessel by energizing the nichrome wire. The inside of the container was replaced with nitrogen, and the pressure was 5 O kgi / cm 2 .
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Abstract
A method for reducing the amount of NOx generating on the burning of a gas-generating agent for an air bag which comprises burning simultaneously two or more types of gas-generating agents having different oxygen balances. The amount of NOx is reduced through the reaction of an oxidizing gas and a reducing gas. The employment of the method according to the invention reduces the amount of NOx generating on the burning of a gas-generating agent for an air bag, which results in the reduction of the probability for the use of an air bag to affect adversely the health of an occupant, and thus in improvement of the safety and reliability of an inflator system.
Description
明細書 Specification
N O x低減方法 技術分野 NOx reduction method Technical field
本発明は、 自動車、 航空機等に搭載される人体保護のために供せられ るエアバッグシステムのインフレ一夕において、 エアバッグ用ガス発生 剤の燃焼により発生する N O X量を減少させる N O X低減方法に関する The present invention relates to a NOX reduction method for reducing the amount of NOX generated by combustion of a gas generating agent for an airbag during an inflation of an airbag system provided for protecting a human body mounted on an automobile, an aircraft, or the like.
従来の技術 Conventional technology
現在、 エアバッグシステムに用いられているガス発生剤の燃料成分と しては、 アジ化ナトリウムが周知である。 アジ化ナトリウムを用いたガ ス発生剤は、 分解温度が 4 0 0で以上と高く耐熱性が優れているし、 ま たその燃焼特性に関して特に問題が無く、 広く実用に供せられている。 しかし、 アジ化ナトリウムは、 例えば、 重金属との反応により爆発性化 合物を生成するほか、 マウスゃラッ 卜の経口毒性 L D 50が 2 7 mg/kgで あること等のために、 大量廃棄時に心配される環境汚染問題があること が知られている。 At present, sodium azide is well known as a fuel component of a gas generating agent used in an airbag system. A gas generator using sodium azide has a decomposition temperature of at least 400 and is excellent in heat resistance, and has no particular problem with its combustion characteristics, and is widely used in practice. However, sodium azide generates explosive compounds by reacting with heavy metals, etc., and has a low oral toxicity LD50 of 27 mg / kg for mouse rats. It is known that there is a concern about environmental pollution.
これらの問題を解決する手段として、 アジ化ナ卜リゥムに替わる化合 物が検討されている。 例えば、 特公平 6 — 5 7 6 2 9号公報には、 テト ラゾール、 トリアゾ一ルの遷移金属錯体を含むガス発生剤が開示され ； 特開平 5— 2 5 4 9 7 7号公報には、 トリアミノグァ二ジン硝酸塩を含 むガス発生剤が開示され； 特開平 6— 2 3 9 6 8 3号公報には、 カルボ ヒドラジドを含むガス発生剤が開示され ； 特開平 7 - 6 1 8 8 5号公報 には酢酸セルロースと過塩素酸力リゥム及び窒素含有非金属化合物を含
むガス発生剤が開示され ； USP5, 125, 684には、 15〜 30 %のニトロセル口 ース等のセルロース系バインダーとエネルギー物質を含有するガス発生 剤が開示され ； 特開平 4 一 2 6 5 2 9 2号公報には、 テトラゾ一ル及び トリアゾール誘導体と、 酸化剤及びスラグ形成剤とを組み合わせたガス 発生剤組成物が開示されている。 As a means to solve these problems, compounds that replace sodium azide are being studied. For example, Japanese Patent Publication No. 6-57669 discloses a gas generating agent containing a transition metal complex of tetrazole and triazol; Japanese Patent Application Laid-Open No. 5-254977 discloses A gas generating agent containing triaminoguanidine nitrate is disclosed; Japanese Patent Application Laid-Open No. Hei 6-23963 discloses a gas generating agent containing carbohydrazide; Japanese Patent Application Laid-Open No. 7-61885 The gazette contains cellulose acetate and perchloric acid lime and nitrogen-containing nonmetallic compounds. US Pat. No. 5,125,684 discloses a gas generating agent containing 15 to 30% of a cellulosic binder such as nitrocellulose and an energy substance; No. 292 discloses a gas generating composition comprising a combination of a tetrazole and triazole derivative, an oxidizing agent and a slag forming agent.
含窒素有機化合物からなるガス発生剤組成物は、 一般的に燃焼におい て、 化学当量分、 即ち含窒素有機化合物分子中の炭素、 水素、 その他の 被酸化元素の燃焼に必要な量の酸素を発生させるだけの酸化剤を用いる 際、 無機アジド系化合物を用いたガス発生剤組成物に比べて発熱量が大 きく、 燃焼温度が高く、 線燃焼速度が小さく、 更に微量の毒性ガスが発 生するという欠点を有している。 In general, a gas generating composition comprising a nitrogen-containing organic compound emits a chemical equivalent in combustion, that is, an amount of oxygen necessary for burning carbon, hydrogen, and other oxidizable elements in the nitrogen-containing organic compound molecule. When using an oxidizing agent that generates enough, it generates a larger amount of heat, has a higher combustion temperature, has a lower linear burning rate, and generates a smaller amount of toxic gas than a gas generating composition using an inorganic azide compound. Has the disadvantage of doing so.
ガス発生剤の燃焼により発生するガスのうち、 特に問題となるのは C O及び N O xであり、 これらのガスは、 有機化合物の燃焼によりほぼ常 に発生するガスである。 ガス発生剤に用いられる有機化合物と酸化剤の 種類により絶対数値は異なるが、 完全酸化理論量より有機化合物が多い と発生ガス中の微量 C 0濃度が増大し、 有機化合物が完全酸化理論量及 びそれ以下になると発生ガス中の微量 N O X濃度が増大する。 ガス発生 剤の燃焼において両者が完全にゼロになることは無く、 両者の最適バラ ンスが保たれる範囲を探す必要がある。 利用者保護の観点から、 発生す る C〇及び N O X濃度のさらなる低減化が求められているものの、 効果 的な低減化方法は実用化されていないのが現状であり、 特に N〇 X濃度 は有機化合物と酸化剤の混合比を変化させてもあまり減少せず、 低減化 することは非常に困難である。 Of the gases generated by the combustion of the gas generating agent, CO 2 and NO x are particularly problematic, and these gases are almost always generated by the combustion of organic compounds. Although the absolute value differs depending on the type of organic compound and oxidizing agent used in the gas generating agent, if the amount of organic compound is larger than the stoichiometric total amount, the concentration of trace C0 in the generated gas will increase, and the oxidizing amount of the organic compound will increase. If it is lower than that, the concentration of trace NOX in the generated gas will increase. During combustion of the gas generant, the two do not become completely zero, and it is necessary to find a range in which the optimum balance between them is maintained. From the viewpoint of user protection, it is required to further reduce the concentration of C〇 and NOX generated, but at present, no effective reduction method has been put into practical use. Even if the mixing ratio of the organic compound and the oxidizing agent is changed, it does not decrease so much, and it is very difficult to reduce it.
一般に N O Xの低減法として知られているものとしては、 重油、 軽油 、 石炭、 プロパンガス等を燃焼させるボイラーやバーナーを使用する大 型プロセスの脱硝技術がある。 この脱硝技術の代表的なものの一つとし
て、 下記反応によって NO xを除去する NH3 による選択還元法があ る。 As a method generally known as a NOX reduction method, there is a large-scale denitration technology using a boiler or a burner that burns heavy oil, light oil, coal, propane gas, and the like. One of the typical denitration technologies There is a selective reduction method using NH 3 to remove NO x by the following reaction.
NO + NH3 + 1/4 〇 2 → N 2 + 3/2 H20 この選択還元法をィンフレー夕においても利用することが考えられる が、 ガスである NH3 (沸点一 3 3. 4で） をそのまま還元剤として 採用することはできない。 NO + NH 3 + 1/4 〇 2 → N 2 + 3/2 H 2 0 it is conceivable to use also in this selective reduction method Infure evening and at NH 3 (boiling point one 3 3.4 a gas ) Cannot be directly used as a reducing agent.
しかし、 この選択還元法をインフレ一夕に利用する方法が W0 However, this selective reduction method is used in inflation overnight.
98/06682 に示されている。 確かに NO X低減の効果は見られるが、 こ こに示されている尿素、 炭酸アンモニゥム、 力ルバミ ド酸アンモニゥム は耐熱性が悪く、 ィンフレー夕に要求される高温試験では分解や昇華が おこり、 実用化できない。 また、 塩化アンモニゥム、 硫酸アンモニゥム 、 フッ化アンモニゥムは分解後に塩素、 フッ素、 硫黄を含んだガスが発 生し、 好ましくない。 このようにこの技術も問題を抱えており、 充分な ものではない。 本発明の開示 98/06682. Certainly, NOx reduction effects can be seen, but the urea, ammonium carbonate and ammonium carbamide shown here have poor heat resistance, and will decompose and sublime in the high-temperature test required for infra-free. Cannot be put to practical use. In addition, ammonium chloride, ammonium sulfate, and ammonium fluoride are not preferable because a gas containing chlorine, fluorine, and sulfur is generated after decomposition. Thus, this technology also has problems and is not enough. Disclosure of the present invention
本発明は、 エアバッグシステムのインフレ一夕において、 利用者保護 の見地から、 エアバッグ用ガス発生剤の燃焼により発生する NO x量を 低減させ、 より安全性を高めることができる NO X低減方法を提供する ことを目的とする。 The present invention provides a method for reducing NOx that can reduce the amount of NOx generated by the combustion of a gas generating agent for an airbag and improve safety further from the viewpoint of user protection during the inflation of an airbag system. The purpose is to provide.
また、 本発明は、 前記 NO x低減方法を採用するインフレ一夕システ ムを提供することを他の目的とする。 It is another object of the present invention to provide an inflation system that employs the NOx reduction method.
本発明者は、 NO x量を低減する方法として、 選択還元法がある程度 の効果を示すことに着目して研究を重ねた。 その結果、 選択還元法が N 〇 X量を低減化するのは、 ガス発生剤の燃焼により発生するガスと還元 性物質から発生するガスの効果的な反応によるものであることを見出し
た。 そして、 この原理をさらに発展させ、 酸化性ガスと還元性ガスの効 果的な反応が上記目的を達成できることを見出し、 本発明を完成した。 即ち本発明は、 酸素バランスの違う 2種類以上のガス発生剤を同時に 燃焼させることにより、 発生する N O X量を低減化することを特徴とす る N O X低減方法を提供する。 The inventors of the present invention have repeated studies focusing on the fact that the selective reduction method shows a certain effect as a method for reducing the amount of NOx. As a result, they found that the selective reduction method reduces the amount of N〇X due to the effective reaction between the gas generated by the combustion of the gas generating agent and the gas generated from the reducing substance. Was. By further developing this principle, they have found that an effective reaction between an oxidizing gas and a reducing gas can achieve the above object, and have completed the present invention. That is, the present invention provides a NOX reduction method characterized by reducing the amount of NOX generated by simultaneously burning two or more types of gas generating agents having different oxygen balances.
また本発明は、 前記の N〇 X低減方法を採用したインフレ一夕システ ムを提供する。 The present invention also provides an inflation system that employs the above-mentioned N〇X reduction method.
本発明はガス発生剤を含むエアバッグ用ガス発生器において、 酸素バ ランスの違う 2種類以上のガス発生剤を同時に燃焼して、 N O Xの発生 量を低減したガスを発生する方法である。 The present invention is a method for generating a gas in which the amount of generated NO X is reduced by simultaneously burning two or more types of gas generating agents having different oxygen balances in an air bag gas generator including the gas generating agent.
本発明の N O X低減方法を適用することにより、 エアバッグ用ガス発 生剤の燃焼により発生する N O Xの量を、 低減することができる。 その 結果、 利用者の健康に悪影響を及ぼす可能性を低下させることができ、 ィンフレー夕システムの信頼性及び安全性を高めることができる。 発明の実施の形態 By applying the NO X reduction method of the present invention, the amount of NO X generated by combustion of the gas generating agent for an air bag can be reduced. As a result, the possibility of adversely affecting the user's health can be reduced, and the reliability and safety of the infra-system can be improved. Embodiment of the Invention
普通、 インフレ一夕に入れられるガス発生剤は一種類である。 ガス発 生剤として求められる特性を満足するように、 燃料、 酸化剤、 バインダ 一、 スラグ形成剤、 その他の添加物の種類及び量を調整したものが用い られる。 この時、 燃焼後ガス中に発生する微量の毒性ガスである C O量 及び N O X量の最適バランスが保たれる範囲を探すことは非常に重要で ある。 実際には、 これらのガス成分を調整するためには、 ガス発生剤の 酸素バランスを調整することになる。 酸素バランスとは、 火薬中の可燃 成分が完全燃焼するための酸素の過不足量のことである。 酸素バランス は火薬 1 g当りの酸素の過不足量 （ g ) で表される。 しかし、 これ以上 の毒性ガスの効果的な低減化方法は実用化されていないのが現状である
そこで、 研究の結果、 本発明のように、 酸素バランスの違う 2種類以 上のガス発生剤を同時に燃焼させることにより、 発生する N O X量を低 減化することができることを見出した。 Normally, only one gas generant is put into inflation overnight. Fuels, oxidizing agents, binders, slag forming agents, and other additives whose types and amounts are adjusted to satisfy the characteristics required for gas generating agents are used. At this time, it is very important to find a range in which the optimal balance between the amounts of CO and NOX, which are trace amounts of toxic gases generated in the post-combustion gas, is maintained. In practice, adjusting these gas components involves adjusting the oxygen balance of the gas generating agent. Oxygen balance is the excess or deficiency of oxygen for the complete combustion of combustible components in explosives. Oxygen balance is expressed as excess or deficiency of oxygen (g) per gram of explosive. However, no further effective method of reducing toxic gases has been put to practical use. Therefore, as a result of research, it has been found that the amount of NOX generated can be reduced by simultaneously burning two or more gas generating agents having different oxygen balances as in the present invention.
つまり これは燃焼触媒などにより固相での燃焼をコントロールするの ではなく、 酸素バランスの違う 2種類以上のガス発生剤からあえて酸化 性ガスと還元性ガスを発生させ、 これらの効果的な反応をコントロール することで、 N〇 x量を低減しょうとするものである。 ガス発生剤が燃 焼中のインフレ一夕内は、 高温、 高圧になっており、 これらのガス反応 にとつては好適な条件となっている。 In other words, this does not control combustion in the solid phase by means of a combustion catalyst or the like, but daringly generates oxidizing gas and reducing gas from two or more types of gas generating agents with different oxygen balances, and makes these effective reactions. By controlling it, we try to reduce the amount of N〇 x. During the period of inflation during which the gas generating agent is burning, the temperature is high and the pressure is high, which is favorable conditions for these gas reactions.
この時、 使用する 2種類以上のガス発生剤の酸素バランスは、 効果が あればいかなるものであってもよいが、 -0. 2〜+0. 2 g/gであることが好 ましく、 -0. 1〜+0. l g/gであることが特に好ましい。 At this time, the oxygen balance of the two or more gas generating agents used may be any as long as it has an effect, but is preferably -0.2 to +0.2 g / g. It is particularly preferred that it is -0.1 to +0.1 lg / g.
また、 普通は、 酸素バランスがマイナスであるガス発生剤とプラスで あるガス発生剤の 2種類を使用して、 この N〇 x低減法を行うことが好 ましく、使用するガス発生剤の酸素バランスは、 - 0. 2〜0. Og/gと 0. 0〜 +0. 2g/gであることが好ましく、 - 0. 1〜0. Og/gと 0. 0〜+0. l g/gであること が特に好ましい。 Usually, it is preferable to perform this N〇 x reduction method using two types of gas generators, one having a negative oxygen balance and the other having a positive oxygen balance. The balance is preferably -0.2 to 0.2 Og / g and 0.0 to +0.2 g / g, -0.1 to 0.Og / g and 0.0 to + 0.lg / g. g is particularly preferred.
本発明の N O X低減法においては、 2種類以上のガス発生剤から発生 した燃焼ガスが効果的に反応する構造になっていれば、 ガス発生剤はィ ンフレー夕内のどこに置いてもよいが、 ガス発生剤燃焼室に配置するの が好ましい。 In the NOX reduction method of the present invention, the gas generating agent may be placed anywhere in the inflation bath if the combustion gas generated from two or more types of gas generating agents effectively reacts. Preferably, it is located in the gas generant combustion chamber.
次にインフレ一夕内における 2種類以上のガス発生剤の分離又は混合 状態であるが、 これも特に制限を受けない。 2種類以上のガス発生剤を 混同機等でよく混ぜて、 見かけ 1種類のガス発生剤のようにして取り扱 つてもよいし、 完全に分離した状態でインフレ一夕内に充填してもよい
。混同した場合はガス発生剤を取り扱いやすいし、 より確実なガス反応 が期待できる。 又、 分離して取り扱う場合は、 それぞれのガス発生剤量 をより正確に秤量できるという利点がある。 Next is the separation or mixing of two or more gas generants during inflation, but this is not particularly limited. Two or more types of gas generating agents may be mixed well by a mixer, etc., and handled as if they were a single type of gas generating agent, or they may be completely separated and charged during inflation. . When confused, the gas generating agent is easy to handle and a more reliable gas reaction can be expected. In addition, when the gas generating agent is handled separately, there is an advantage that the amount of each gas generating agent can be measured more accurately.
次に、 本発明で使用される非アジド系ガス発生剤組成物について説明 する。 Next, the non-azide gas generating composition used in the present invention will be described.
本発明で使用される非アジド系ガス発生剤組成物は、 含窒素化合物、 酸化剤、 必要によりスラグ形成剤及びバインダ一から成るものが好まし い。 The non-azide gas generating composition used in the present invention is preferably composed of a nitrogen-containing compound, an oxidizing agent, if necessary, a slag forming agent and a binder.
本発明で用いられる含窒素化合物としては、 グァニジン誘導体、 テト ラゾール誘導体、 ビチトラゾール誘導体、 トリァゾール誘導体、 ヒ ドラ ジン誘導体、 トリアジン誘導体、 ァゾジカルボンアミ ド誘導体、 ジシァ ナミ ド誘導体から成る群から選ばれる 1種又は 2種以上の混合物が挙げ られる。 これらの具体例としては、 ニトログァニジン、 硝酸グァニジン 、 5—アミノテ卜ラゾール、 ビテ卜ラゾールジアンモニゥム塩、 5—才 キソー 1， 2 , 4— 卜リアゾ一ル、 シァノグァニジン、 トリアミノグァ 二ジン硝酸塩、 トリヒ ドラジノ 卜リアジン、 ビウレッ ト、 ァゾジカルボ ンアミ ド、 ピウレア、 カルボヒ ドラジド、 カルボヒ ドラジド硝酸塩錯体 、 蓚酸ジヒ ドラジド、 ヒ ドラジン硝酸塩錯体、 ナトリウムジシァナミ ド 等を挙げることができる。 The nitrogen-containing compound used in the present invention is selected from the group consisting of a guanidine derivative, a tetrazole derivative, a bititrazole derivative, a triazole derivative, a hydrazine derivative, a triazine derivative, an azodicarbonamide derivative and a disocyanamide derivative. Species or a mixture of two or more species. Specific examples of these include nitroguanidine, guanidine nitrate, 5-aminotetrazole, bittrazol diammonium salt, 5-year-old xo 1,2,4-triazolyl, cyanoguanidine, triaminoguanidine nitrate, Examples thereof include trihydrazinotriazine, biuret, azodicarbonamide, piurea, carbohydrazide, carbohydrazide nitrate complex, oxalic acid dihydrazide, hydrazine nitrate complex, and sodium disocyanamide.
これらの含窒素化合物の中ではテトラゾール誘導体及びグァニジン誘 導体から成る群から選ばれる 1種又は 2種以上が好ましく、 特にニトロ グァニジン、 シァノグァニジン、 5—アミノテトラゾ一ルが好ましい。 本発明に係わるガス発生剤組成物中の含窒素化合物の配合割合は、 分 子式中の炭素元素、 水素元素及びその他の酸化される元素の数によって 異なるが、 通常 20〜70重量％の範囲が好ましく、 25〜60重量％の範囲が 特に好ましい。
本発明に係わるガス発生剤組成物に用いられる酸化剤としては種々の ものが使用できるが、 アル力リ金属又はアル力リ土類金属から選ばれた カチオンを含む硝酸塩、 亜硝酸塩、 過塩素酸塩、 塩素酸塩の少なく ともAmong these nitrogen-containing compounds, one or more members selected from the group consisting of a tetrazole derivative and a guanidine derivative are preferable, and nitroguanidine, cyanoguanidine and 5-aminotetrazole are particularly preferable. The mixing ratio of the nitrogen-containing compound in the gas generating composition according to the present invention varies depending on the number of carbon elements, hydrogen elements and other oxidized elements in the molecular formula, but is usually in the range of 20 to 70% by weight. Is preferred, and a range of 25 to 60% by weight is particularly preferred. Various oxidizing agents can be used as the oxidizing agent used in the gas generating composition according to the present invention, and nitrates, nitrites, and perchloric acids containing cations selected from the group consisting of alkali metal and alkaline earth metal are used. At least salt and chlorate
1種から選ばれた酸化剤が好ましい。 アルカリ金属又はアル力リ土類金 属から選ばれたカチオンを含む硝酸塩としては、 硝酸ナトリウム、 硝酸 カリウム、 硝酸マグネシウム、 硝酸ス トロンチウム等が挙げられる。 本発明に係わるガス発生剤組成物中の酸化剤の配合割合は用いられる ガス発生化合物の種類と量により絶対数値は異なるが 30〜80重量％の範 囲が好ましく、 特に 40〜75重量％の範囲が好ましい。 An oxidizing agent selected from one type is preferred. Examples of the nitrate containing a cation selected from an alkali metal or an alkaline earth metal include sodium nitrate, potassium nitrate, magnesium nitrate, strontium nitrate, and the like. The mixing ratio of the oxidizing agent in the gas generating composition according to the present invention varies in absolute value depending on the type and amount of the gas generating compound used, but is preferably in the range of 30 to 80% by weight, particularly 40 to 75% by weight. A range is preferred.
本発明に係わるガス発生剤組成物中のスラグ形成剤の機能は、 ガス発 生剤組成物中の特に酸化剤成分の分解によって生成するアル力リ金属又 はアル力リ土類金属の酸化物をミス トとしてインフレー夕外へ放出する ことを避けるため液状から固体状に変えて燃焼室内に止める機能であり 、 金属成分の違いによって最適化されたスラグ形成剤を選ぶことができ る。 The function of the slag forming agent in the gas generating composition according to the present invention is as follows. The oxide of a metal or an alkaline earth metal formed by the decomposition of the oxidizer component in the gas generating composition. It is a function to change from a liquid to a solid to stop it in the combustion chamber in order to avoid releasing mist as an inflation outside the evening. It is possible to select a slag forming agent optimized by the difference in metal components.
スラグ形成剤の具体例としては、 酸性白土、 シリカ、 ベントナイ 卜系 、 カオリン系等のアルミノケィ酸塩を主成分とする天然に産する粘土 ； 合成マイ力、 合成力オリナイ ト、 合成スメク夕イ ト等の人工的粘土 ； 含 水マグネシウムケィ酸塩鉱物の 1種であるタルク等 ； アルミナ、 水酸化 アルミニウム等の少なく とも 1種から選ばれたスラグ形成剤が挙げられ 、 これらの中では酸性白土、 アルミナ又はシリカが好ましい。 Specific examples of slag forming agents include acid clay, silica, bentonite-based, kaolin-based, and other naturally-occurring clays mainly composed of aluminosilicates; synthetic myc, synthetic olinite, synthetic smectite Slag forming agents selected from at least one of alumina, aluminum hydroxide, and the like. Among them, acid clay, Alumina or silica is preferred.
本発明においてスラグ形成剤は必須ではないがガス発生剤組成物中に 適量加えることは非常に効果がある。 スラグ形成剤を加える場合の配合 割合は 1〜20重量％の範囲で変えることができるが、 好ましくは 3〜10 重量％の範囲である。 多すぎると線燃焼速度の低下及びガス発生効率の 低下をもたらし、 少なすぎるとスラグ形成能を十分発揮することができ
ない。 In the present invention, the slag forming agent is not essential, but adding an appropriate amount to the gas generating composition is very effective. When the slag forming agent is added, the mixing ratio can be varied in the range of 1 to 20% by weight, but is preferably in the range of 3 to 10% by weight. If the amount is too large, the linear burning speed and the gas generation efficiency decrease, and if the amount is too small, the slag forming ability can be sufficiently exhibited. Absent.
本発明に係わるガス発生剤組成物中のバインダ一は、 組成物の燃焼挙 動に大幅な悪影響を与えないものであれば何れでも使用可能である。 本 発明に用いられるバインダ一の具体例としては、 カルボキシメチルセル ロースの金属塩、 ヒ ドロキシェチルセルロース、 酢酸セルロース、 プロ ピオン酸セルロース、 酢酸酪酸セルロース、 ニトロセルロース、 微結晶 性セルロース、 ポリ ビエルアルコール、 グァガム、 澱粉等の多糖誘導体 、 ステアリン酸カルシウム等の有機バインダーまたは二硫化モリブデン 、 酸性白土、 タルク、 ベントナイ ト、 ケイソゥ土、 カオリン、 シリカ、 アルミナ等の無機バインダ一が挙げられる。 As the binder in the gas generating composition according to the present invention, any binder can be used as long as it does not significantly affect the burning behavior of the composition. Specific examples of the binder used in the present invention include metal salts of carboxymethyl cellulose, hydroxyxethyl cellulose, cellulose acetate, cellulose propionate, cellulose acetate butyrate, nitrocellulose, microcrystalline cellulose, and polyvinyl alcohol. Polysaccharide derivatives such as guar gum and starch; organic binders such as calcium stearate; or inorganic binders such as molybdenum disulfide, acid clay, talc, bentonite, diatomaceous earth, kaolin, silica, and alumina.
本発明においてバインダ一は必須ではないがガス発生剤組成物中に適 量加えることは非常に効果がある。 バインダーを加える場合の配合割合 は 0〜 1 5重量％の範囲が好ましい。 量的には多い側でより成型体の破壊 強度が強くなるが、 量が多いほど組成物中の炭素元素及び水素元素の数 が増大し、 炭素元素の不完全燃焼生成物である微量 C Oガスの濃度が増 大したり、 線燃焼速度を低下させるため好ましくない。 In the present invention, the binder is not essential, but adding an appropriate amount to the gas generating composition is very effective. When the binder is added, the compounding ratio is preferably in the range of 0 to 15% by weight. The larger the amount, the stronger the fracture strength of the molded body, but as the amount increases, the number of carbon elements and hydrogen elements in the composition increases, and a small amount of CO gas, which is an incomplete combustion product of carbon elements It is not preferable because the concentration of methane increases or the linear burning rate decreases.
本発明のガス発生剤組成物は、 ガス発生剤用燃料、 酸化剤等を粉末状 で混合する乾式法又は水や有機溶剤等の存在下で混合する湿式法により 製造することができる。 The gas generating composition of the present invention can be produced by a dry method in which a fuel for a gas generating agent, an oxidizing agent, and the like are mixed in a powder form, or a wet method in which the fuel and the oxidizing agent are mixed in the presence of water or an organic solvent.
また、 本発明のガス発生剤組成物は、 所望の形状に成型することもでき る。 例えば、 打錠機を用いて圧縮成型してペレッ トにしたり、 ディスク 成型機を用いて圧縮成型してディスクにしたり、 ペレツ トゃディスクを 粉碎するか又はダラ二ユレ一夕を用いて顆粒にしたり、 圧伸機 （押出成 形機） を用いて押出成型して圧伸薬 （無孔、 単孔、 多孔） にしたりする ことができる。 さらに、 圧延してフィルム状又は板状に成型することも できる。
これらの成型方法は、 ガス発生剤組成物の成型品に対して付与しょう とする性質等に応じて適宜選択することができる。 例えば、 圧縮成型法 を適用した場合、 成型にバインダーを必要としないか又は少量だけでよ いので、 燃焼性の低下がない傾向がある。 また、 押出成型法を適用した 場合、 ウェブが薄いものを成型することが圧縮成型法よりも容易である ので、 燃焼速度の遅い組成でも成型品を得ることができる。 さらに、 押 出成型法は成型が比較的短時間ですむため大量生産に向いている。 また 、 燃焼速度が速い組成の場合は成型品のサイズを大きくできるために、 より製造効率を上げることができる。 そのほか、 押出成型法を適用した 場合には、 無孔、 単孔、 多孔等の複雑な形状の成型品を製造できるため 、 種々の燃焼特性を付与することができる。 Further, the gas generating composition of the present invention can be molded into a desired shape. For example, compression molding using a tableting machine to produce pellets, compression molding using a disk molding machine to produce discs, grinding pellets to discs, or granulation using daraniure Alternatively, it can be extruded using a drawing machine (extrusion molding machine) to make a drawn medicine (non-porous, single-hole, porous). Furthermore, it can be rolled and formed into a film or plate shape. These molding methods can be appropriately selected according to the properties to be imparted to the molded article of the gas generating composition. For example, when the compression molding method is applied, the binder does not need to be molded or only a small amount is required, so that there is a tendency that the flammability does not decrease. Also, when the extrusion molding method is applied, it is easier to mold a thin web than the compression molding method, so that a molded product can be obtained even with a composition having a slow burning rate. In addition, the extrusion molding method is suitable for mass production because molding can be performed in a relatively short time. In the case of a composition having a high burning rate, the size of the molded product can be increased, so that the production efficiency can be further increased. In addition, when the extrusion molding method is applied, a molded article having a complicated shape such as non-porous, single-pored, or porous can be manufactured, so that various combustion characteristics can be imparted.
本発明の N O X低減方法は、 自動車、 航空機等に搭載される人体保護 のために供せられる、 インフレ一夕とエアバッグが収納されたモジュ一 ルケ一ス、 判断回路、 センサー等を備えたインフレ一夕システムに適用 することができる。 実施例 The NOX reduction method according to the present invention provides an inflation system provided with a module case containing an inflation circuit and an airbag, a judgment circuit, a sensor, and the like, which are provided for protecting a human body mounted on an automobile, an aircraft, or the like. It can be applied to the overnight system. Example
以下、 実施例及び比較例を挙げて本発明を具体的に説明するが、 本発 明はこれらの実施例のみに限定されるものではない。 Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to only these Examples.
実施例 1 Example 1
ニトログァニジン （N Q ) 及び硝酸ストロンチウム （S r (N03) 2) を表 1の組成になるように混合した。 ついでその混合粉約 2 gをハンドブレ ス機で圧縮成型した。 径 9 . 6 m m、 長さ約 1 4 m mのストランドを得 た。
表 1 Nitoroguanijin a (NQ) and strontium nitrate (S r (N0 3) 2 ) were mixed so that the compositions shown in Table 1. Then, about 2 g of the mixed powder was compression-molded with a hand brace machine. A strand having a diameter of 9.6 mm and a length of about 14 mm was obtained. table 1
実施例 1のス トランドを表 2 に示した組み合わせで燃焼し、 その燃焼 後ガスを分析することで、 本発明の N O X低減効果を確認した。 ス トラ ンドはニクロム線に通電することにより、 1 リ ッ トルの燃焼容器内で燃 やされた。 容器内は窒素置換され、 圧力は 5 O kgi/cm2であった。 The strands of Example 1 were burned in the combinations shown in Table 2, and the gas after combustion was analyzed to confirm the NOX reduction effect of the present invention. The strand was burned in a 1 liter combustion vessel by energizing the nichrome wire. The inside of the container was replaced with nitrogen, and the pressure was 5 O kgi / cm 2 .
C O及び N 0 Xの分析は、 着火後直ちに検知管を用いて行った。 Analysis of C O and N 0 X was performed using a detector tube immediately after ignition.
この結果より、 比較例 1のように酸素バランスが 0. 00g/gのガス発生 剤を燃焼させた場合よりも、 実施例 2や 3のように酸素バランスがブラ スとマイナスのガス発生剤を混合して燃焼させた場合の方が N 0 X及び C Oを低減できることが証明された。 From these results, it was found that the gas generating agent having the oxygen balance of the brass and the gas generating agent having the negative oxygen balance of Examples 2 and 3 was smaller than the case of burning the gas generating agent having the oxygen balance of 0.000 g / g as in Comparative Example 1. It has been proved that NOx and CO can be reduced when mixed and burned.
また、 比較例 2や 3のように酸素バランスがマイナスやプラスのガス 発生剤を単独で燃焼させた場合には N O Xや C〇が著しく増加しており 、 これらを単純混合しても実施例 3のガス組成にはならないことが分か つた。 つまり、 実施例 3では 2種類のガス発生剤から発生したガスの反 応により N O X及び C 0が低減されていることが分かった。
表 2 In addition, when the gas generating agent having a negative or positive oxygen balance was burned alone as in Comparative Examples 2 and 3, NOX and C〇 increased remarkably. It was found that the gas composition did not become the same. That is, in Example 3, it was found that NOX and C 0 were reduced by the reaction of the gases generated from the two types of gas generating agents. Table 2
Claims
1 . 酸素バランスの違う 2種類以上のガス発生剤を同時に燃焼させる ことにより、 発生する N O X量を低減化することを特徴とする N O X低 減方法。 1. A NOx reduction method characterized by reducing the amount of NOx generated by simultaneously burning two or more gas generating agents with different oxygen balances.
2 . 使用するガス発生剤の酸素バランスがマイナスであるものと、 プ ラスであるものの 2種類であることを特徴とする請求項 1記載の N O X 低減方法。 2. The NOx reduction method according to claim 1, wherein the gas generating agent used is of two types: one having a negative oxygen balance and one having a positive oxygen balance.
3 . ガス発生剤が非アジド系ガス発生剤であり、 含窒素化合物と酸化 剤を含有することを特徴とする請求項 1〜 2記載の N O X低減方法。 3. The NOx reduction method according to claim 1, wherein the gas generating agent is a non-azide-based gas generating agent and contains a nitrogen-containing compound and an oxidizing agent.
4 . 含窒素化合物がグァニジン誘導体、 テ卜ラゾール誘導体、 ビテト ラゾール誘導体、 卜リアゾール誘導体、 ヒ ドラジン誘導体、 トリアジン 誘導体、 ァゾジカルボンアミ ド誘導体、 ジシアナミ ド誘導体から選ばれ る 1種以上である請求項 3記載の N O X低減方法。 4. The nitrogen-containing compound is one or more selected from a guanidine derivative, a tetrazole derivative, a bitetrazole derivative, a triazole derivative, a hydrazine derivative, a triazine derivative, an azodicarbonamide derivative, and a dicyanamide derivative. NOX reduction method described in 3.
5 . 請求項 1〜4のいずれか 1記載の N O X低減方法を採用したィン フレー夕システム。 5. An inkjet system employing the NOx reduction method according to any one of claims 1 to 4.
6 . ガス発生剤を含むエアバッグ用ガス発生器において、 酸素バラ ンスの違う 2種類以上のガス発生剤を同時に燃焼して、 N O Xの発生量 を低減したガスを発生する方法。
6. In a gas generator for an airbag containing a gas generating agent, a method of simultaneously burning two or more types of gas generating agents with different oxygen balances to generate a gas with reduced NO X emissions.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11017965A JP2000211987A (en) | 1999-01-27 | 1999-01-27 | Reduction in nox |
| JP11/17965 | 1999-01-27 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2000044691A1 true WO2000044691A1 (en) | 2000-08-03 |
Family
ID=11958464
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/JP2000/000419 WO2000044691A1 (en) | 1999-01-27 | 2000-01-27 | METHOD FOR REDUCING NO¿x? |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP2000211987A (en) |
| WO (1) | WO2000044691A1 (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3814694A (en) * | 1971-08-09 | 1974-06-04 | Aerojet General Co | Non-toxic gas generation |
| JPS63176387A (en) * | 1987-01-16 | 1988-07-20 | ダイセル化学工業株式会社 | Gas generator |
| US5386775A (en) * | 1993-06-22 | 1995-02-07 | Automotive Systems Laboratory, Inc. | Azide-free gas generant compositions and processes |
| EP0763511A2 (en) * | 1995-09-15 | 1997-03-19 | Morton International, Inc. | Igniter compositions for non-azide gas generants |
| JPH09100191A (en) * | 1995-10-06 | 1997-04-15 | Daicel Chem Ind Ltd | Gas producer composition |
-
1999
- 1999-01-27 JP JP11017965A patent/JP2000211987A/en active Pending
-
2000
- 2000-01-27 WO PCT/JP2000/000419 patent/WO2000044691A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3814694A (en) * | 1971-08-09 | 1974-06-04 | Aerojet General Co | Non-toxic gas generation |
| JPS63176387A (en) * | 1987-01-16 | 1988-07-20 | ダイセル化学工業株式会社 | Gas generator |
| US5386775A (en) * | 1993-06-22 | 1995-02-07 | Automotive Systems Laboratory, Inc. | Azide-free gas generant compositions and processes |
| EP0763511A2 (en) * | 1995-09-15 | 1997-03-19 | Morton International, Inc. | Igniter compositions for non-azide gas generants |
| JPH09100191A (en) * | 1995-10-06 | 1997-04-15 | Daicel Chem Ind Ltd | Gas producer composition |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2000211987A (en) | 2000-08-02 |
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