WO1996010000A1 - Gas-generating agent, process for producing the agent, and equipment for producing pelletized gas-generating agent - Google Patents

Abstract

A gas-generating agent that is excellent in formability and combustion stability, has readily regulable properties, and can be produced safely. The agent comprises a gas-generating component and an oxidizing agent, and the gas-generating component comprises at least one of the following reaction products (a) through (d): (a) a reaction product formed between ammonia, its salt or a compound having an NH2 or NH group in its structure and an organic compound that has a CHO group in its structure or that can yield a CHO group; (b) a secondary reaction product formed between the reaction product (a) and a compound having an OH group in its structure; (c) a reaction product formed between a compound having an NH2 or NH group in its structure and an N-methylol compound; and (d) a reaction product formed between a compound having an NH2 or NH group in its structure and an N-alkoxy compound.

Description

 Field of the Invention Gas generating agent, method for producing the same, and apparatus for producing gas generating agent pellets

 The present invention relates to a gas generating agent used in an inflator for an air bag of a vehicle, or a gas generating agent for projectile propulsion, and a method for producing the same. Particularly, the present invention relates to the formability and combustion stability, and also to the adjustment of the combustion characteristics. The present invention relates to a gas generating agent which can be easily and safely carried out, a method for producing the gas generating agent, and a method for manufacturing and concealing a gas generating agent pellet. Background art

 First, as a gas generator for inflators, those based on sodium azide * are also typical. This sodium azide is currently used all over the world because of its moderate impact ignitability, combustion speed κ and gas generation amount, but on the other hand, it is a highly toxic and dangerous substance κ. There is a question that an explosion accident occurred during the manufacturing process. Therefore, as a gas generating agent in place of sodium azide, a solid pellet composed of a gold salt of a hydrogen-free bitetrazole compound and a specific oxidizing agent (Japanese Patent Publication No. 616-15656). JP-B-64-61557) and a solid composition containing a transition protein of aminoinoazole and an oxidizing agent

In addition to those using tetrazoles as in the case of No. 2 13 6 87, a solid composition comprising azodicarbonamide, an oxohalogenate and, if necessary, a combustible catalyst (JP-A-6-32) 6 8 9

A method using azodicarbonamide has been proposed as disclosed in Japanese Patent Application Publication No. 32690/1990. In addition, as a gas generating agent for propelling a projectile, polyptadiene is used as a propellant such that it comprises a binder having a hydroxyl group-terminated polybutadiene prepolymer as a main component, an oxidizing agent and a specific binder in the binder. Used as a binder

In addition to (Japanese Patent Publication No. 6-333215), a specific terminal hydroxyl-aliphatic polyester is used as a propellant and a binder (Japanese Patent Publication No. 47-175878). Etc. have been proposed.

 Since all gas generators for inflators in which a compound having a high nitrogen content, such as the above-mentioned tetrazole diazodicarbonamide, and an oxidizing agent are mixed, they are all in a solid state. However, in the manufacturing process, it is necessary to make tablets by tableting. Since this tableting process is a process of applying pressure to the explosive composition and applying pressure, it is an operation involving the greatest risk of explosion. From the viewpoint of safety, the tableting diameter and oxidizing agent that can be selected are selected. There is a limitation on the type of the fuel, and it is difficult to adjust the burning rate and the ignitability, and the obtained velvet is fragile and the burning rate is easily changed.

On the other hand, in a projectile propellant gas generator using a material having caking properties, such as the above-mentioned polyptadene or aliphatic polyester, there is an upper limit and a lower limit to the content in order to obtain an appropriate viscosity. There is a problem that the adjustment range of the gas composition is restricted and the polymerization concept is easily changed. The present invention has been made in view of the above-mentioned problems of the prior art, and has as its object to provide a gas generating agent which is excellent in moldability, and whose characteristics can be easily and safely adjusted. And to provide a method for fabricating the same. In addition, another object of the present invention is to provide an apparatus for producing a gas generant pellet which can more safely form a gas generant produced by the gas generant production method into a pellet or the like. Disclosure of the invention

The gas generating agent of the present invention which solves the above KRjH is ammonia or a compound having ammonia or a compound having Γ-NH _a group j or Γ-NH- in the structural formula

(Hereinafter, in the present invention, these are referred to as “amines j” for convenience) and an organic compound having “one CHO group” or an organic compound capable of forming “one CHO group” in the formula (hereinafter, referred to as “j”). In the present invention, both of these are referred to simply as

The reaction product obtained by reacting with aldehydes has not only the property K as a gas generating component, but also the oxidizing agent and other components added to the gas generating agent. It is based on the new discovery that even binders that bind to agents are extremely useful.

In addition, a secondary reaction product obtained by reacting a reaction product obtained by reacting the amides with the aldehydes and a compound having a 1 OH group in the formula is provided. , a compound having an NH _a group or one NH- in the structural formula and N- methylcarbamoyl ₀ - the reaction product obtained by reacting a Le compound, one in the structural formula NH _a group or one NH- A reaction product obtained by reacting a compound having the formula (I) with an N-alkoxy compound has characteristics similar to those of a reaction product obtained by reacting the amines and the aldehydes. It was made with a focus on

 Accordingly, the present invention provides a gas generating agent comprising a gas generating component and an oxidizing agent, wherein the gas generating component comprises at least one of the following reaction products: is there.

(a) Anmoyua or reaction with a compound having an NH _a group or single NH- in its salt or構迪formula, an organic compound is also an organic compound having an CH0 group in the structural formulas, which may occur an CHO group Reaction product obtained

(b) The reaction product obtained in (a) above and a compound having a 10H group in the structural formula Secondary reaction product obtained by reacting the compound with the compound.

(C) a compound having an NH _a group or one NH- in the structural formula and the reaction product obtained by reacting a N- methylcarbamoyl n- Le compounds.

(d) compounds in the structural formula with an NH _a group or one NH- and the reaction product obtained by reacting N- alkoxy compound.

 Such a gas generating agent can be suitable for being used as a gas generating agent for an inflator for an airbag or a gas generating agent for projectile propulsion for the following reasons.

Here, Amin's mentioned above are those having the meaning of combustion Motozai, an essential one NH _a group j or "an NH-J gamma reacts with" one CHO group j having the aldehyde compound, Any compound can be used as long as it has these functional groups. However, as a gas generating agent for an inflator for an airbag, a large amount of oxygen gas is generated and a small amount of carbon dioxide gas and water vapor is generated. The compound is selected, and the reaction product obtained by the reaction with the aldehydes described below produces a slurry with an appropriate viscosity due to the efficiency of the oxidizing agent described later, and the gas generating agent pellets It is preferable to use a material S which can be easily formed into a shape.

Then, aldehyde such for use in the present invention, that have the Amin such aforementioned "one: H ₂ group" or react with "one NH- j, equipped with a result and caking property and combustion agent This is for generating a reaction product, and can own an aldehyde group (one CHO group) as a functional group or generate a “one CHO group”.

The reaction products of the above (1) to (d) are usually viscous substances containing water. However, if the product is dried at a temperature to remove water, the condensation reaction proceeds and hardens. When the oxidizing agent described below is added to the viscous material, the oxidizing agent is included in the hardened material of the box, so that the oxidizing agent serves as a filler, and the molded gas generating agent Has high strength and is hardly powdered. By the way, among the above-mentioned amines, azodicarbonamide, tetrazole

Aminotetrazole (for example, 5-aminotetrazole), bitetrazole (for example, 5,5-B1H-tetrazole), melamine, triazole (for example, 5-year-old 1,2,4-to-1) Lyazole) or these golds (Group 1) are liable to react with aldehydes in an aqueous solution to form a solid reaction product. Triaminoguanidine nitrate, guanidine, guanidine nitrate , Guanidine carbonate, dicyandiamid, hesa methylenetetramamine, biuret, hydrazine, carbohydrazide, citrate dihydrazide, hydrazine salt, urea or their salts (Group 2) in aqueous solution One or more types selected from the first group and selected from the second group because they easily react with aldehydes to produce liquid reaction products It preferred to use species or two or more thereof.

That is, a solid reaction product and a liquid reaction product are simultaneously obtained by the reaction with the aldehydes, and as a result, the slurry in which the solid reaction product is uniformly distributed in the liquid reaction product is obtained. Is obtained. Further, if the reaction product slurry is mixed with an oxidizing agent, a slurry containing water and having an appropriate viscosity is formed. However, since this slurry is a slurry containing water, it is safe to handle. In addition, this mixture slurry can be processed into a gas generating agent having a desired shape by various molding methods as it is, and the degree of freedom of combustion adjustment by shape control is increased. In addition, since there are various amines that can be used, the degree of freedom in adjusting the gas composition is high, for example, when the combustion gas contains a large amount of nitrogen gas. From the above-mentioned viewpoints, amines used as a gas generating agent suitable for a bag inflator include those selected from the first group, mainly composed of aminotetrazole or azodicarbonamide, and appropriately mixed with the second group, or Or from the second group, with triaminoguanidine nitrate as the main component, and appropriately mixing the first group, or the first group of aminotetrazole or It is particularly preferable to appropriately mix azodicarbonamide and the second group of triaminoguanidine nitrate. Since the azodicarbonamide of the first group does not easily react with the aldehydes, it is preferable to supplement with the amides which easily react with the aldehydes of the second group. The second group, triaminoguanidine nitrate, reacts easily with aldehydes, but the viscosity of the oxidizing agent tends to be insufficient, so it is difficult to react with the first group aldehydes. It is preferable to supplement this.

 For the reaction between amines and aldehydes, a pH adjuster is added as necessary, and any known PH adjuster can be used.

 Next, compounds capable of obtaining the above reaction products (a) to (a) are shown below.

Examples of the compound having one NH ₃ group or one NH— in the structural formula described in the above (a), (c) or (d) include monoethanolamine, human'T3 xyamine, and formamide. C. Carbonamide, azodicarbonamide, hydrazodicarbamide, aminomonopropanol, azobisformamide, semicarbazide, acetate semicarbazone, hydrazine, formylhydrazine, formamidine, monoethylhyd. Drazin, Colepohydrazide, Cianamid, Dicyandiamide ', Aminotetrazol, Guanidine, Aminoguanidine, Triamino Guzine Nitrate, Nito Guzin, Hazo Di Guzin, Big Guid , Monohydro beef siurea, thiourea, melamin. Ruami down, mono Echiruami Roh monoethanolamine § Mi emissions, cattle Samechirente tiger Mi emissions. Door Riazoru, Te Torazoru. The Activity door Razoru or one or more selected from the salts thereof or Ranaru group, and the like to.

When these substances are treated with N-methylol, the above (a), (c) or (d) It is a compound having one: NH— in the described formula.

The foregoing (a), the compound K or give as the specific examples of compounds that chromatic in構迫formula an NH _a group or one NH- according to (c) or omega, these things N- main switch When the N-methylated substance is further subjected to N-methylolation treatment, the N-methylol compound described in the above (c) is obtained.

The foregoing (a), when treated N- alkoxylated said substance raised as an example of a structure compound to chromatic an NH _a group or one NH- in formula described in (c) or (d), above And N-alkoxy compounds described in (id).

 Specific examples of the organic compound having one CH 0 group in the structural formula described in () include formaldehyde, acetate aldehyde, propyl aldehyde, n-butyl aldehyde, n-butyl aldehyde, and n —One or more species selected from the group consisting of forceprodaldehyde, acrolein, crotonaldehyde, and glyoxal.

 Specific examples of the organic compound capable of forming one CH 0 group described in the above (a) include formamide, paraformaldehyde, triodisan, hexamethylenetetramine, tetraxane, metaaldehyde, and azo. One or more selected from the group consisting of bisformamide.

 The compound having a 10 H group in the formula shown in the above (h) is a compound having a 1 O H group sugar-linked to carbon (C) or nitrogen (N).

 Specific examples of such a compound having an OH group bonded to carbon (C) or nitrogen (N) include methanol, ethanol. Monoethanolamine, aminobanol, diethanolamine. One or more species selected from the group consisting of, for example, sheep hydrazine, human beef, ethylaminoethanolamine, hydroquinamine, and xylurea hydrate. Formamide dosim, formaldehyde beef shim.

The specific composition of the gas generating agent of the present invention is as follows. Including a generating component and 50 to 8% by weight of an oxidizing agent, 10 to 40% of a gas generating component, 50 to 80% by weight of an oxidizing agent, and 1 to 10% by weight And a combustion catalyst component.

 The gas generating agent basically consists of a gas generating component and its oxidizing agent, and the content ratio of these components varies theoretically depending on the type of the gas generating agent and the type of the oxidizing agent. However, when the above-mentioned gas generating component of the present invention is used, generally, mixing of 10 to 40% by weight of the gas generating component and 50 to 80% by weight of the oxidizing agent is carried out at a pace. Become. If the gas generating component is less than 10% by weight, the gas generation rate is poor, and if it is more than 40% by weight, incomplete combustion tends to occur. If the content S of the oxidizing agent is less than 50% by weight, incomplete combustion of the gas generating component tends to occur. If the content S is more than 80 SS96, the ignition S of the gas generating component decreases and the amount of gas generated decreases. Therefore, the most suitable range for the content ratio of the gas generating component and the oxidizing agent according to the specified substance is selected from the above range.

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 In addition, when an oxidizing agent containing nitric acid clay as a main component is used, the reaction is not completed due to a small amount of exothermic S, and unburned matter tends to remain. However, when the combustion catalyst component is included, there is an effect that the combustion SStt medium component completes the reaction and does not leave unburned substances. As described above, depending on the components of the oxidizing agent, a combustion catalyst may be used. In this case, the addition of the combustion catalyst g is performed within a range that does not inhibit the gas generation S. ~ 10 weight β added in the range of 90

The oxidizing agent used in the present invention is one which is usually mixed in the gas generating component obtained as the above-mentioned reaction product. In the present invention, an oxidizing agent is added to and mixed with the reaction product, and then the condensation reaction product is heated and condensed and cured, so that the oxidizing agent and the combustion agent are uniformly dispersed and brought into close contact. become. As a result, it has excellent heat aging resistance, but it has a long ignition time Even with oxidizing agents such as nitric acid and chlorate, which have characteristics, the ignition characteristics can be significantly improved.

 As the oxidizing agent, 1a or 2 or more kinds of nitric acid.

 Specific examples of pre-nitric acid * include sodium nitrate, potassium nitrate. Nitric acid, 'ium, ammonium nitrate, and strontium nitrate. Chlorates, chlorites, bromates, perbromate clay, iodate clay, and iodic clay are examples of the above-mentioned acid salt.

 Further, specific examples of the above-mentioned oxohalogenate compounds include sodium hydrochloride, rhodium oxalate, sodium oxalate, rhodium chlorate, ammonium chloride, ammonium chlorate, and bromate. Lithium, perbromate lime, iodate lime, and periodic lime.

 Specific examples of the gold is oxide include manganese dioxide, iron oxide, zinc dioxide, potassium peroxide, potassium permanganate, barium peroxide, and molybdenum trioxide.

 As the combustion catalyst, one or two selected from zirconium, hafnium, molybdenum, tungsten, manganese, iron, nickel, chromium, titanium, or an oxide or sulfide, carbon, phosphorus, or sulfur alone The above is usable.

 Next, a method for producing the gas generating agent of the present invention will be described. The present invention includes a step of reacting the above compound in an aqueous solution to obtain a slurry of the above-mentioned) to ω reaction product having an appropriate viscosity, and a step of drying or heating the slurry to solidify the slurry. It is a thing.

It is considered that the reaction for obtaining the reaction product of any of the above-mentioned) to (d) in an aqueous solution is an addition / condensation reaction in which the compounds contain water and repeat addition and condensation. When the water is removed by drying or heating, condensation curing The viscosity of the slurry, which is considered to produce advanced resin such as ffl amino resin, differs depending on the type of compound, PH, and water content. Can be adjusted. The reaction for obtaining such a reaction product proceeds relatively easily, and there are countless combinations of compounds from which the reaction product can be obtained, and a gas having a desired component is generated. The possible combinations can be arbitrarily selected, and can be combined as a desired gas generator for inflator or a gas generator for propelling a flying object.

 In addition, when the above-mentioned condensation curing is performed, the oxidizing agent uniformly divided in the beret-shaped gas generating agent and the combustion agent, which is the reaction product, come into close contact with each other. As a result, the heat conduction of each component particle に な る is improved. As a result, the ignitability of the gas generating agent is greatly improved, so that conventional gas generating agents such as nitrate and chlorite clay have excellent heat aging resistance but poor ignitability ( Even if the oxidizing agent is used as the oxidizing agent, in the present invention, the gas generating agent can be excellent in both heat aging resistance and ignition performance.

 The method for producing a gas generating agent of the present invention will be described in more detail. The production method of the present invention can be roughly divided into the following two types.

 [First method]

 1-①: a step of reacting the above compound in an aqueous solution to obtain a slurry of the above-mentioned reaction product having the above-mentioned) to (d) having a sufficient viscosity.

 1-②: A process of adding an oxidizing agent necessary for generating nitrogen gas to the obtained reactant and mixing the oxidizing agent into a slurry having a predetermined viscosity.

 1-3: Step of forming this slurry into a desired shape.

1-④: The step of drying and solidifying this compact. [Second method]

 2-①: a step of reacting the above compound in an aqueous solution to obtain a reaction product slurry of the above-mentioned) to ω having an appropriate viscosity.

 (2-① ': Step of adding and mixing at least a part of the necessary oxidizing agent into the obtained reaction product to form a slurry.)

 2-②: a step of drying the slurry and pulverizing the slurry to form a powder.

 2--3: A process in which an oxidizing agent is added to and mixed with this powder, and pressed into a predetermined shape by tableting or the like.

 2—④: Step of heating and compacting this molded body.

 Next, each method will be described.

 The first method will be described by taking, as an example, a case in which an amine that produces the reaction product of the above (a) is reacted with an aldehyde.

The ratio (molar ratio) of amines and aldehydes in this reaction affects the basic physical properties of the reaction product and the physical properties resulting from the concept of polymerization reaction. From the viewpoint of reducing the inspection removal step, the amines: aldehydes = 1: preferably in the range of 0.5 to 1.5. When a plurality of amines are added, it is desirable to add them at the same time in order to prevent variation in the progress of the reaction depending on the type. The amount of water used is preferably S, which gives an aldehyde concentration of 10 to 50%. The reaction is exothermic, but if the reaction is exothermic, the reaction mixture is allowed to react while cooling, if necessary, so that the reaction solution does not boil.If the reaction is less exothermic, the reaction does not boil to promote the reaction. The reaction is carried out while heating to a moderate degree, and the slurry having the appropriate fluidity required in the next process is converted. Here, the slurry concentration 118 is adjusted by removing water after the reaction, and a method of removing water by decompression in principle is adopted. In the heating evaporation method, a condensation reaction of a reaction product described below proceeds, and at this stage, a window for suppressing the condensation reaction is used. Therefore, it is preferable to avoid a stinging heating.

 In the first method, in the step of adding and mixing the oxidizing agent of 1-② to form a slurry for molding raw material, the oxidizing agent is added to the reaction product slurry having an appropriate viscosity as described above. A slurry is formed. Here, the specified viscosity is a viscosity suitable for the molding method used in the following step 1-3.

 In the process 1-3, since the combustion agent is a slurry containing water, it is possible to apply a molding method for general polymer materials such as extrusion while maintaining safety while being an explosive composition. Extrusion into a rod, cutting into a predetermined shape, forming into a sheet, such as a rubber sheet, and cutting into a pellet, or punching from this sheet It is molded into a desired shape by an arbitrary molding method such as a method.

 The drying and solidifying step 1-④ is a step of removing water and condensing and curing the reaction product. The degree of condensation by drying is natural drying. It can be adjusted by a combination of low-temperature heat drying of 50 or less and high-temperature heat drying of 9 Ot or more. The condensation reaction is stable at 90 ° C or more high-temperature heating. And proceed. Therefore, this drying and solidification step is preferably performed under heating of 9 D 1C or more.

 In the first method described above, the work of adding and mixing the oxidizing agent to the combustion product, which is a reaction product, is performed in the concept of a water slurry, so it is an extremely safe operation without explosion risk and uniform. A good mixture can be obtained. The slurry viscosity of this homogeneous mixture can be adjusted by adjusting the amount of water, addition of oxidizing agent S, etc., and is adjusted to a viscosity appropriate for the next molding step. It can be supplied to a molding machine to form a pellet of a desired shape. Therefore, the choice of the pellet shape is free, and the degree of freedom in adjusting the combustion speed of the gas generating agent is increased.

More notable is the fact that conventional manufacturing processes have the highest Can be performed with the concept of a water slurry, which has the effect of dramatically improving the safety of the fruit forming process.

 Next, the second method will be described. The main difference between the second method and the first method is

, 2—② and ③, ie, drying and molding. The first method directly molds from the slurry of the gas generating composition containing the reaction product and the oxidizing agent, which is the gas generating component, while the second method forms the reaction generating as the gas generating component. The product slurry or the slurry of the gas generating composition to which the oxidizing agent necessary for the reaction product slurry is added is first dried to form a powder, which is then press-formed by tableting or the like. It is a method to do.

 As a method of drying the slurry of the above item 2 to powder, the fine powder can be easily obtained by hot air drying while spraying the slurry by a spray dryer method. In this case, the drying ffl degree needs to be a temperature at which the condensation reaction of the reaction product does not easily proceed, and differs depending on the raw material K and the reaction system. Preferably it is 80 or less. Further, when a plate-shaped or lump-shaped dried product is obtained by another drying method, ii, it is necessary to appropriately pulverize the dried product to form a powder.

 Next, in the molding of 2-3, this powdery composition is molded into a predetermined shape by a pressure molding method. At this time, the reaction product, which is a gas generating component, is polymerized with a certain degree of flexibility and caking properties, and is in a powder form in such a manner as to contain oxidizing particles. It is extremely low or non-ignitable in all cases of impact intensity, friction port intensity, and aerobic sensitivity. Therefore, unlike the conventional pressure molding process, there is no problem in terms of safety.

Furthermore, since the powder particles have an appropriate caking property, the concept of compaction is easily maintained even after pressure molding, and the shape and density of the compact are uniform due to a synergistic effect with condensation hardening by heating in the next step. As a result, it is possible to obtain a gas generating agent having a high strength of the compact and a stable burning rate. On the other hand, because of its viscous properties, there is a point that it is easily added to the molding biston at the time of pressure molding, but this point can be solved by adding the necessary oxidizing agent separately before molding. BP, the oxidizing agent powder is added to the powder obtained in the step 2−3, and the surface of the reaction product powder is added to the powdered oxidizing agent in the step 2−3. Because of the coating, this oxidizing agent prevents the raw material powder from adhering to the bistone. The addition of the oxidizing agent S in 2−3 before the process in 2− 、, that is, when a part of the necessary oxidizing agent was added and mixed in 2−① ′ to form a slurry, The remaining amount is appropriately added.

 The following heat-condensation step 2—④ is a step of heating and compacting and compacting the reaction product, which differs depending on the raw material K and the shape of the reaction product. The ripening is performed at a temperature of at least C, preferably at 100 and at a high temperature of at least.

 In the second method, there is a step of drying the slurry in which an oxidizing agent is appropriately mixed to form a powder, but the reaction product at this stage is a "hydrated substance" before condensation, Sensitivity, friction sensitivity, static air permeability, etc. are all extremely low or non-ignitable. Therefore, it can be said that the drying operation, the crushing operation and the pressure molding operation under this concept basically ensure safety o

Since the gas generating agent manufactured by the above-mentioned method has a structure in which the oxidizing agent is uniformly dispersed and taken into the resin cured and condensed in the compaction process after molding, the oxidizing agent is used. The particles act as fillers as a reinforcing material in the resin molded article, and the beret strength after molding becomes remarkably large. Incidentally, the crushing strength of the tablet-formed pellets with a diameter of 7 mm and a thickness of 5 mm before the condensation hardening treatment is around 6 kgf, but after the condensation hardening treatment, it is as large as 22 to 30 kgf. I do. Therefore, the degree of powdering of the compact is reduced to a negligible level. In addition, the cured polymer material 0 As a pellet with the concept of uniformly dispersing the oxidizing agent in the broadening agent is obtained, its shape and density become constant, and a gas generating agent whose viscosity and burning rate are stable can be obtained. Become. In addition, since the combusting agent and the oxidizing agent are in close contact in the pellet, the thermal conductivity of the rain is extremely good. As a result, conventionally, the heat aging resistance is excellent, but the flammability is poor. And nitrates that are: Even in combination with an oxidizing agent such as hydrochloride, the ignitability is greatly improved, so that a gas generating agent using these oxidizing agents and having both excellent heat aging resistance and ignitability can be obtained.

 In addition, as a method of manufacturing a gas generating agent suitable for forming the above gas generating agent into a pellet more safely, the above (a) to! An oxidizing agent is added to any of the reaction products of d) and mixed to form a slurry having a predetermined viscosity, and this slurry is poured into a flexible non-gold-molded mold having a predetermined shape to obtain a slurry. There is a method for producing a gas generating agent by heating and solidifying this.

 Since the slurry is a water slurry containing water as described above, the safety at the time of molding is improved, and at the same time, the risk of forming a gas generating agent, which is a kind of explosive, is always dangerous. It is now possible to use the "heating" process, which had been described as "the process", thereby shortening the solidification time and increasing productivity.

 In order to carry out the above-mentioned method for producing a gas generating agent, for example, a mold is formed on a rotatable annular belt such as an airless belt, and a slurry is injected with a brittle belt. It is reasonable to take out the molded product that has been solidified by heating and to heat and solidify it during that time.

That is, an annular belt-shaped molding frame formed of a non-metallic material having flexibility and having a plurality of recesses on its surface nodes to be a gas generating agent molding die, and a drive for rotating the frame. A mechanism, a slurry injection mechanism provided at one end of the frame body, and a heating mechanism for ripening and solidifying the gas generating agent slurry in the recess. A molding device having is suitable. This is to solve the problem of spark caused by the metal mold R and the problem at the time of removing the molded product by forming the molding die from a non-metallic material having soft blowing properties.

 The molding frame includes a flat plate, and a plurality of non-metallic (R) members that are erected in the shape of a K flat plate and have flexibility. The inside of this ffi body becomes a concave part of the molding die, and at least one portion of the peripheral wall ffi of the tongue body has a slit in the axial direction and in a direction orthogonal to the frame body moving direction. Then, the body is erected by fitting into a shallow recess provided in a flat plate of the molding frame.

 In addition, the concave portion serving as a molding die may be formed by forming the molding frame itself from a non-metallic material having flexibility and forming a concave portion serving as a molding die in a surface node thereof. Good. In this case, a cut-out is provided in at least a part of the frame base material portion between the tongue and dent in the axial direction, or a rear surface of the molding frame is orthogonal to the traveling direction of the frame. It is desirable that a groove be formed in the direction.

 As described above, according to the production method and Apparatus B of the gas generating agent of the present invention, the gas generating agent S compound is formed from a water slurry state, so that the gas which has been regarded as the most dangerous The safety of the molding process of the generator can be greatly improved.

 In addition, since the method of injecting the slurry into the mold is adopted, the shape of the mold is not limited to the conventional elliptical tablet shape, but the selection of the shape is widened and the combustibility is considered. It is possible to select the optimal gas generating agent shape that has been obtained.

In addition, since the molding is started with the idea of a water slurry, a heating method that could not be adopted because it was conventionally dangerous can be adopted, and a large improvement in solidification speed is achieved. , It is possible to adopt a drying and solidification system, and as a result, it is possible to reduce the equipment space and achieve continuous production. , Productivity is also improved.

 Furthermore, in the manufacturing apparatus of the present invention, a concave node serving as a molding die is formed on the surface of the molding frame. Injection, heating and solidification of the slurry-like gas generating agent composition injected, and R solidification of the molded body by sexually deforming the molding die, so that the gas is continuously discharged. It is easy to mold and generate the generator, and the productivity is dramatically improved.

 In addition, since the mold is made of a flexible material, it can be easily extracted from the mold only by elastically deforming it, and no special tool for extraction is required and the gas generating agent is used. There is no breakage during removal of the molded body, and the product yield is improved.

 In addition, the mold is made of a flexible non-gold JS material, and the molded article can be extracted only by its elastic deformation, so that the friction between the molded article and the mold is reduced. However, there is no spark at the time of removal, which is a major problem in the conventional method, and safety is dramatically improved.

 In addition, when a mold is made of a flexible non-metallic material and an axial cut is made on its peripheral wall, it is easy to remove a molded product due to its elastic deformation. Become.

 In addition, the structure of the model is a combination of a flat plate and a plurality of cylinders erected in the form of a flat plate, or a flat plate having a shallow dent and a 简 body fitted to the dent. Alternatively, various applications are possible, such as forming a cut in the body in the axial direction to facilitate the property deformation of the mold when removing the molded product. The applicable range is wide such that the form can be adopted.

Further, as a material having flexibility, silicone rubber, polybutadiene, polychlorinated bure, polyisoprene, butyr rubber, isobutylene, and α Since it is possible to use one or more of krill rubber, ketirosulfonidani polyethylene, ethylene propylene, fluorine rubber, and urethane rubber or a mixture thereof, molding of a mold can be performed easily and at low cost.

 As described above, the method and the apparatus for producing a gas generating agent according to the present invention firstly consider the danger of ignition caused by the molding technique when the gas generating agent is tableted from a powdery raw material mixture. Second, it solves the problem of danger of ignition and the problem of low productivity caused by the mold during propellant molding, and provides an extremely safe and productive technology. The company provides production technology for highly efficient gas generating agents. Simple sharps of the drawing

FIG. 1 is a typical example of a graph showing characteristics obtained in a one-liter tank test, and FIG. 2 is a cross-sectional view showing an example of a configuration of a gas generating agent forming apparatus according to the present invention. Fig. 3 is a top view of the device IB of Fig. 2, and Figs. 4 (a) and 4 (b) show the procedure of the method for manufacturing a gas generating agent according to the present invention. Fig. 40 (a) is a side view, Fig. 4 (b) is a side view, and Fig. 5 is a schematic view of a gas generating agent molding apparatus S according to the present invention. FIG. 6 is a perspective view showing another embodiment of the injection mechanism of the present invention. FIG. 6 is a perspective view showing another embodiment of the molding frame of the molding apparatus B for the gas generating agent according to the present invention. FIG. 7 is a perspective view showing another embodiment of the molding frame of the gas generating agent molding apparatus according to the present invention, and FIGS. 8 (a) and 8 (b) show the present invention. The configuration of such a gas generating agent forming apparatus Fig. 8 (a) is a top view, Fig. 8 (b) is a lateral view, and Figs. 9 (a) and 9 ( b) is H showing still another embodiment of the molding frame of the gas generating agent molding apparatus according to the present invention, wherein FIG. 9 (a) is a top view, and FIG. 9 (b) is a lateral surface. FIG. BEST MODE FOR CARRYING OUT THE INVENTION

Hereinafter, examples of the gas generating agent of the present invention will be described. The properties of the converted gas generating agent were evaluated by a one-liter tank test. This one-liter tank test has a pressure sensor attached to a stainless steel container with an inner volume of 1 ') and the igniter can be attached freely. Put the prototype gas generant pellet in this container, ignite it with the igniter, measure the ignition time from when the ignition current of the igniter flows until the pressure is generated, and measure the generated pressure. . Incidentally, the igniter was used 0. 6 fir entering the DD NP (Jiazojutorofu Nord) ignition Ball + B / KNO _a (Bo n down mortar stones).

A typical example of a graph showing the characteristics obtained by this one-liter tank test is shown in Fig. 1 (1). Is the ignition time 、, Ρ _{ββ> (} is the ft high pressure, and t -P .. indicates the «time to high pressure 閱. For example, t in the case of the gas generator for inflator _t is about 1 Oms, ββ1 _< and t-P »a« are within a predetermined range, and it is necessary to have an appropriate combustion rate.

(Example 1 1)

PH adjusted to 45.1 g (0.27 mol) of triaminoguanidine salt (TAGN) and 62.1 g (0.773 mol) of 5-aminotetrazole (5-1 ATZ) Magnesium oxide for use 4. Os was mixed, and 81 g of formalin solution (310-96 product) was added while stirring the mixed solution. The formalin aqueous solution was added gradually so as not to cause foaming, and the reaction was carried out while cooling with water in order to suppress foaming. When this reaction was carried out at room temperature for about 1 hour, an emulsion-like viscous reaction product was obtained. This reaction product is thought to be a type of amino resin formed by the addition condensation reaction of an amino group (one NH _A ) and an aldehyde group (one CH 0). The product of the reaction with the salt is water-soluble, but that of 5-ATZ is not water-soluble. Therefore, it is a slurry-like reaction product in which both are mixed. This slurry one like reaction product, chlorate force Riumu powder (KC] 0 _a) 1 72. 5 g of adding and mixing viscous slurries and without the oxidizing agent, the scan slurry one like composition A string was extruded onto a polyethylene sheet using a syringe to form a string having a width of about 5 mm and a height of about 5 mm and having a semicircular cross section. This was dried in a constant-temperature oven at 70 for 24 hours to obtain a solid that was condensation-cured by Ichiro. The solid was cut into three types, 15 mm in length, 25 mm and 35 mm, and used as a gas generating agent. When the above-described 1 liter tank test was performed using 10 g of each of the gas generating agent pellets, the results shown in Table 1 were obtained.

As shown in Table 1, the ignition time t, is less than 1 Oms, and t-Pmax and Pmax are also within appropriate ranges, and the gas generating agent for the inflator for airbags. Was a good value. Incidentally, C 0澳度in the product gas is any even less than 1% 0., was not in an amount sufficient to provide Q S _beta

 [Table 1: 1-litre torque test results]

(Example 1-2)

After mixing and crushing 0.7 g of potassium carbonate for adjusting pH to 8.4 g of T AGN, add 1 s of water and mix to make sure that it is at pH 7 to 8, and To this, 2.1 g of formalin solution (37% product) was gradually added in the same manner as in Example 1 so that foaming due to the reaction did not occur. After a minute reaction, a viscous liquid reaction product was obtained. It is thought that this reaction product was also generated by a kind of so-called amino resin. The reaction product of the AGN and the aldehyde was water-soluble and different from the slurry containing solids. This liquid reaction product was mixed with 13.7 g of clay as an oxidizing agent, mixed, and the resulting viscous slurry was dropped on a polyethylene sheet using a syringe. It was dried for 24 hours in the same manner as in Example 1 to obtain a hemispherical gas generant pellet with a diameter of about 7 mm. The above-mentioned one-liter tank test was conducted using 10 g of this belt at t, -7.6 ms, t-Pmax. = 33.6 ms.Pmax. = 63.32 atm. Yes, the C 0 concentration in the generated gas was 0.1% or less, which was a good value as a gas generator for inflators.

 (Example 1-3)

 Alkaline was added to 11.6 g of azodicarbonamide (ADCA) and 4.2 g of the formalin solution, and the mixture was stirred and mixed with PH 6.5 to 7.5 at room temperature for about 2 hours. After the reaction, a slurry-like reaction product was obtained. This reaction product is also considered to be a kind of so-called amino resin, but the reaction product of ADC A and aldehyde is a water-insoluble solid, and is a small slurry separated in the reaction solution. Met. In this slurry, potassium chlorate 27.8 was added and mixed as an oxidizing agent to form a viscous slurry, which was extruded using a syringe and cut to a length of 5 to 1 Omm to carry out the condensation reaction. It was air-dried without advancing, and a short string-shaped gas generant having a diameter of about 4 mm and a length of 5 to 1 Omm was obtained. Using the gas generating agent (10 g), the above-mentioned one-liter tank test was carried out, and the results were as follows: 1, -8.4 ms.t-Pmax. = 43.6 ms, Pmax. = 46.57 at m., and the C 0 concentration in the generated gas was 0.1% or less, which was a good value as a gas generator for inflators.

(Example 1-4)

TAGN 1 6.7 g and 4.2 g of the formalin solution were added without alkali When the reaction was carried out at room temperature for about 1 hour under the above conditions (PH 6.5-7.5), a transparent syrup-like reaction product was obtained. This reaction product is also considered to be a kind of so-called amino resin. To this reaction product, 27.3 g of potassium chlorate was added and mixed to form a viscous slurry, which was dropped on a polyethylene sheet using a syringe similarly to Example 12. It was air-dried for 24 hours to obtain a hemispherical gas generating agent pellet having a diameter of about 8 mm. When the 1 liter tank test was performed using 10 g of this pellet, tt = 9.6 ms.t-Pmax. = 46.8 ms, Pmax. = 61.4 atm. The C 0 concentration in the produced gas was 0.396, which was a good value as a gas generator for inflators.

 (Example 1-5)

 TAGN 12.5 ε (0.075 mole) and 5 一 2.1 ε (0.025 mole) were mixed with 0.8 g of magnesium carbonate for silk shaping, and 4 g of water was added thereto. After the addition and kneading, 11.4 g of the above formalin solution (37% product) was gradually added and mixed with stirring, and the mixture was reacted at room temperature for about 1 hour to produce a transparent syrup-like reaction. Thing was obtained. 27 g of chlorinated acid powder) as an oxidizing agent was added to and kneaded with the resulting reaction product in the form of a syringe, and the obtained slurry-like composition was injected into a syringe in the same manner as in Example 12. Then, the mixture was dropped on polyethylene sheet and dried at Ί0 for 24 hours to obtain a hemispherical gas generant pellet having a diameter of about 5 mm in which a partial condensation reaction had progressed. When the one-liter tank test was performed using the pellet 10 s, t, = 8.4 ms, t-Pmax. = 32.4 ms, Pmax. = 70.11 atm., which was a good value as a gas generator for inflation.

(Example 1-6)

TAGN l O g (0.06 mol) and 5-ATZ 3.4 ε (0.04 mol) are mixed with 0.8 g of magnesium carbonate for inversion and mixed with 4 g of water. And then kneaded to form a base by mixing with S. Then, while gradually adding 11.4 g of the formalin solution (37% product), the mixture was stirred by ft and allowed to react at room temperature for about 1 hour. A clear, sipping reaction product was obtained. To this reaction product, 26.7 g of potassium chlorate powder as an oxidizing agent was added and kneaded, and the obtained slurry composition was dropped on a polyethylene sheet using a syringe in the same manner as in Example 15. Then, the mixture was dried at 9 for 24 hours for 1 hour to obtain a hemispherical gas generant pellet having a diameter of about 5 mm in which the condensation reaction had progressed. Using the pellet of 10 g and performing the one-liter tank test, t, = 8.4 ms, t-Pma. = 32.8 ms pmax. = 67.31 atm. This was a good value as a gas generator for inflators.

 (Example 1-7)

 TAGN 7.5 g (0.045 mol) and 5-ATZ 4.7 e (0.055 mol) were mixed with 0.8 s of magnesium carbonate for PH 睏, and 4 s of water was added. After kneading to form a paste, the formalin solution (37% product) was stirred and mixed while adding 11.4 ε gradually, and allowed to react at room temperature for about 1 hour. A reaction product was obtained. To this reaction product, 26.5 g of citrate powder as an oxidizing agent was added and mixed, and the resulting slurry composition was mixed with a polyethylene syringe using a syringe in the same manner as in Example 15. The mixture was dried at 90 at 24 hours to obtain a hemispherical gas generant pellet having a diameter of about 7 mm in which the condensation reaction proceeded. Using the 10 g of this belt, the above-mentioned 1-torque tank test was performed, t, = 10 Oms.t-1 Pmax x = 52.8 ms, Pmax x = 58.92 at m. This was a good value as a gas generator for an inflator.

 (Example 1-8)

TAGN 5.0 E (0.03 mol) and 5.0 g ATZ 6.0 g (0.07 mol) were mixed with 0.8 g of magnesium carbonate for PH adjustment, and water 4 After adding s and kneading into S to form a paste, the mixture was stirred and mixed while gradually adding 11.4 g of the above formalin solution (37.5 products), and reacted at room temperature for about 1 hour. Thus, a viscous slurry-like reaction product was obtained. To the reaction product, 26.2 g of potassium chlorate powder as an oxidizing agent was added and kneaded, and the mixture was dropped on a polyethylene sheet using a syringe in the same manner as in Example 15 to obtain 24 hours at 90 t. H-drying was performed to obtain a hemispherical gas generating pellet with a diameter of about 7 mm in which the condensation reaction was advanced. When the one-liter tank test was performed using 10 g of this pellet, ti = 10 Oms, t-Pmax. = 47.2 ms, Pmax = 60.05 atm., which was a good value as a gas generator for inflators.

 (Example 1-9)

 TAGN 4.2 ε (0.025 mol) and 5 一 6.4 ε (0.075 mol) are mixed with 0.4 g of magnesium oxide for 、 adjustment, and 4 g of water is added thereto. After adding and kneading to form a base, 11.4 g of the above formalin solution (37% product) was gradually added, mixed with stirring, and allowed to react at room temperature for about 1 hour. A slurry-like reaction product was obtained. To this reaction product, 2 &. Lg of potassium chlorate powder as an oxidizing agent was added and kneaded, and the mixture was dropped on a polyethylene sheet using a syringe in the same manner as in Example 15 to obtain 90 * C For 24 hours to obtain a hemispherical gas generant pellet having a diameter of about 7 mm in which the condensation reaction has progressed. When the one-liter tank test was performed using 10 g of this pellet, ti-8.8 ms, t-P max. = 53.6 ms.P max. = 58.06 at m. Yes It was a good value as a gas generator for inflators.

 (Example 10)

TAGN 3.3 g and ADCA 9.3 S are mixed with 0.4 g of magnesium oxide for pH adjustment, and 4 g of water is added to the mixed mixture to form a base. After that, the former ε-formalin solution (37% product) 8. The mixture was mixed slowly while adding lg slowly, and allowed to react at room temperature for about 1 hour while cooling with water. Thing was obtained. To this reaction product, 20.5 r / min of acid lime powder as an oxidizing agent was added and kneaded. The mixture was extruded from a syringe in the same manner as in Example 13 and cut into a length of about 7 mm. At 24 hours to obtain a gas generant pellet having a diameter of 5 mm and a length of 7 mm in which the condensation reaction had progressed. When the one-liter tank test was performed using 10 g of this pellet, t, = 8.4 ms, t-Pma. = 71.6 ms, Pmax. = 56.17 at m., which was a good value as a gas generator for inflation.

 (Example 1 1 1)

 TAGN 5.0 g (0.03 mol) and 5-ATZ 6.0 z (0.07 mol) were mixed with 0.4 g of magnesium oxide for PH adjustment, and 4 g of water was added thereto. After mixing and kneading to form a base, 8.1 g of the formalin solution (31% product) was gradually added and mixed with stirring, and the mixture was allowed to react at room temperature for about 1 hour while cooling with water. Reaction product was obtained. To this reaction product were added 6.7 g of potassium nitrate powder and 18 g of potassium oxalate powder as oxidizing agents, and the mixture was mixed. The mixture was dropped on a plate and dried at 90 at 24 hours to obtain a hemispherical gas generant pellet having a diameter of about 8 mm in which the contraction reaction had progressed. Using 10 g of this Bellette for the previous K 1 little tank test, t! S S O. 4 ms.t- 1 Pma x. = 9 1.6 ms, Pma x. = 5 1.32 at m., the Iffl at ignition is slightly slower and the pressure rises slightly, which is a problem as a gas generator for airbag inflators, but a problem as a gas generator for flying objects. It was a value without transliteration.

(Example 1 1 2) Example 11 In Example 11, a chloric acid power was used in place of the lithium chlorate.

The beret 20 s prepared using 13.5 g was heated at 110 ° C. for 48 hours to be completely condensed and cured. Using the obtained pellets (10 g) to perform the above-mentioned 1 liter tank state, t! -L l. 2 ms, t-P max. = 5 1.2 ms, Pmax. = 60.77 atm., the ignitability was improved as compared with that of Example 11 and the value could be used as a gas generator for inflators.

 (Example 1-13)

 A mixture of 4.2 g (0.025 mol) of T AGN and 6.4 g (0.075 mol) of 5—ATZ with 0.4 g of magnesium oxide for adjusting PH81 was added to the formalin solution. (37% product) 8.1 g was gradually added and mixed with stirring for 10 minutes at room temperature to obtain a viscous reaction product. To this reaction product was added 18.8 g of sodium oxalate as an oxidizing agent, kneaded with fB, dropped on a polyethylene sheet, dried at 45 for 24 hours, and completely cured to a diameter of about 7 A hemispherical beret of mm was obtained. When the one-liter tank test was performed using 1 Pg of this pellet, t, = 53.0 ms, t-Pmax. = 262 ms, Pmax. = 44.6 atm. However, the ignition time was slow and the pressure rise was slow, making it unsuitable as a gas generating agent for airbags, but it was a value that could be used as a gas generating agent for projectiles.

 (Example 1-14)

20 g of the beret obtained in Example 13 was heated at 110 ° C. for 48 hours to be completely condensation-cured, and 10 g of the obtained beret was used for the above-mentioned 1) Ti-l l. 2 ms, t-P max. = 1 1 1.6 ms. P max. = 39.4 7 at m., Which is much more ignitable than Example 1-13. Revised, gas generation for airbag inflator It was a good value as a crude drug.

 (Example 1-15)

 TAGN 66.8 e (0.40 mol) and 5-ATZ 102.0 g (1.20 mol) were mixed, and the S mixture was stirred while formalin solution (37% product) 1 29.8 g was added. The formalin solution was gradually added so that foaming did not occur. When this reaction was carried out at 70 for 30 minutes, a viscous milky reaction product (a kind of amino tree) was obtained. To this reaction product, potassium oxalate powder (ΚΝΟ,) 31 1.? (3.08 mol) and potassium periodinate (KC10,) 38.3 g (0. Was added and kneaded for 20 minutes to form a viscous slurry. This slurry-like composition was extruded onto a polyethylene sheet to form a 1 mm-thick plate-like body, which was dried and solidified in a 50% moisture oven at 24 hours. Next, the plate-like solid is roughly crushed and further crushed in a mortar to obtain a powder having a particle size of 1 mm or less. Then, using a tableting machine, a pellet of 6, 7, 8 mm in diameter and 5 mm in thickness is used. Each 150 g was produced. The pellets were subjected to a condensation hardening reaction at X 24 hours in 107 in a high-temperature furnace to obtain a gas generating agent. The crushing strength of this gas generant pellet was extremely high at 20 to 30 kgf. Incidentally, the crushing strength before the condensation reaction was 5-6 kgf.

 When the above-described one-liter tank test was performed using 10 g of each of these three types of gas generating agent pellets, the results shown in Table 2 were obtained.

 [Table 2: Results of 1-litre tank test]

As shown in Table 2, each ignition time t, is within 1 Dms At the same time, t-Pmax and Pmax were also within the range of conductivity, and were good values as gas generating agents for inflators for airbags. In addition, the C 0 degree in the generated gas was 0.1% or less in each case, which was not an amount sufficient to satisfy the question S.

 (Example 1-16)

The reaction product obtained by reacting under the same conditions as in Example 15 was compacted and dried at room temperature to form a solid mass, which was sufficiently crushed and ground in a mortar. Nitrate Ca Li um powder as an oxidizing agent to the powder material _{(KNO s) 3 1 1. 4} g (3. 0 8 mole "and Guhani periodate mosquito Li um _{(KC 1 0 4> 38. 3} g (0 .28 mol) were added to each of them, and the mixture was kneaded in 2D pieces, and using a punching machine, 150 g each of 6.7, 8 mm mxj 5 mm diameter berets were produced. Was subjected to a simple condensation curing reaction in a high-temperature furnace at 105 for 24 hours to obtain a gas generating agent.The crushing strength of this gas generating agent pellet was an extremely high value of 20 to 30 kgf. The previous crushing strength was 5 to 6 kgf A 1 liter sunset test was performed using 10 g of each of these three types of gas generant pellets, and the results shown in Table 3 were obtained. .

 [Table 3: Results of one-liter tank test]

As shown in Table 3, Kt at ignition is within 1 Oms, and P-x and P-x are also within appropriate ranges, and are good gas generators for air flakes. Value. In addition, the C 0 concentration in the generated gas was 0.1% or less in each case, and was not S which was a problem. 00

(Example 17)

TAGN 66.8 g (0.40 mol) and 5-ATZ 102.0 g (1.20 mol) were mixed with 37.9 g (0.27 mol) of beef samethylene tetramine. After adding 70 g of water thereto, the mixture was heated to 9 D1C and reacted for 30 minutes to obtain a clear liquid viscous reaction product (a kind of amino resin). to the reaction product, nitrate mosquito potassium powder as an oxidizing agent _{(KN 0 8) 31 1. 4} ε (3. 08 mol) and suitable chlorate force potassium (KC 1 0 «) 38. 3 « (0. 28 mol) The mixture was then closed and mixed for 20 minutes to form a viscous slurry.The slurry-like composition was extruded onto a polyethylene sheet to form a 1 mm rhinoceros plate, Next, the plate-like solid was roughly crushed and crushed in a mortar to obtain a powder having a particle size of 1 mm or less. , 8mmX 5mm thick berets were removed for 150s each. The pellets were subjected to a condensation hardening reaction at 107 tx for 24 hours in a high-temperature furnace to obtain a gas generating agent, and the crushing strength of the gas generating agent pellet was extremely high at 20 to 30 kgf. Incidentally, the crushing strength before the binding reaction was 5-6 kgf.

 When the above-described one-liter tank test was performed using 10 g of each of these three types of gas generating agent pellets, the results shown in Table 4 were obtained.

 [Table 4: 1 liter tank test results]

As shown in Table 4, at ignition fflt! Were within 1 Oms, and t-Pmax. And Pmax. Were also within appropriate ranges, which were good values as gas generating agents for air flakes for airbags. In addition, generate The CO transmission in the gas was less than 0.1% in each case, not enough to make an inquiry.

 (Example 18)

 5-AT Z 85 g, nitric acid 185 g, molybdenum oxide 13.5 g, shark ethoxymethyl melamine 17 g, add water 50, knead well, and then knead with 75 t It was dried into a plate having a thickness of 5 mm for 0 hours. The dried product was pulverized until it passed a 1 mm-diameter joint, and then tableted with a diameter of 7 mtn, a height of 4.7 mm, and 300 mg / particle. The crushing strength was 20 kgf. When the tablet was dried at 11 Ot for 10 hours, the crushing strength was increased to 22 kgf.

 After sealing this in an aluminum container, a thermal shock wiping test was performed (at +90, a test was performed in which 200 cycles were repeated in a period of 1.1 to 14 hours. The weight change after the test was 0, and crushing was performed. The strength was 21 ksf, and there was almost no change.Similarly, a heat aging test in which the temperature was kept at 120 for 100 hours showed that the weight change was 10.3%. However, there was no change in appearance.

 [Example 1 of Kiko]

 5—A mixture consisting of 85 g of ATZ and 142 g of potassium nitrate was tableted into 300 mm Z granules having a diameter of 7 mm and a height of 4.7 mm. The crushing strength was 19 kgf. After sealing this in an aluminum container, a thermal shock test K (+ 90-C to 140, 1.1 hours, 200 cycles) was performed.

When the above-described 1 liter tank test was performed using 10 g of each of the gas generant pellets in Example 18 and Example 1 of Comparative Example, the results shown in Table 5 were obtained. [Table 5: Results of one-liter tank test]

The numbers in the above-mentioned conditions indicate the state of the environmental test, where 1 is the initial state, 2 is after the thermal shock test, and 3 is after the heat aging test.

 As shown in Table 5, there was no change in the combustion characteristics of the device according to the present invention even after the environmental test K. The ignition times t, were all within 1 Oms, and t-Pma X. and Pma X. were also within appropriate ranges, and were good values as gas generating agents for inflators for airbags.

 On the other hand, in Comparative Example 1, after the environmental test, it was powdered and tank testing was not possible.

 [Example 1 1 9]

 A 37.38 formalin solution 13.88: previously adjusted to pH 8.0 with sodium hydroxide was heated to 90. A 10% aqueous solution of 50% urea was gradually added to the mixture, and the mixture was stirred at 9 Ot for 30 minutes. To this, 7.8 g of ethanol was added, and further, phosphoric acid was added to obtain pH 5.5. The mixture was further heated at 90 ° C. for 1 hour to obtain a slightly viscous liquid.

To this liquid, 75,58Γ of potassium nitrate and 11.8 g of potassium persulfate were added and kneaded for 10 minutes to form a viscous slurry. This was extruded onto a polyethylene sheet to form a plate having a thickness of 2 mm, and dried in a constant temperature oven at 0 ° C for 24 hours. Next, the plate-like solid material was pulverized into a powder having a particle size of 1 mm or less, and then a tablet having a diameter of 7 mm and a thickness of 4 mm was formed using a tableting machine. This pellet was subjected to a condensation hardening reaction in a high-temperature furnace at 120 for X 10 hours to obtain a gas generating agent. The crushing strength of the beret was 13 kgf before condensation and 18 kgf after condensation.6 A 10 liter bevel was used to conduct a 1 liter sunset test, and the following results were obtained. .

[Table 6: Results of one-liter tank test]

 The ignition time t, was within 1 Oms, and t-Pmax and Pmax were also within appropriate ranges.

 Next, a method and an apparatus for producing a gas generating agent according to the present invention will be described.

 FIG. 2 is a lateral view BI showing the configuration of an embodiment of an apparatus for carrying out the method for producing a gas generating agent according to the present invention, FIG. 3 is a top view of the embodiment, FIG. 4 (a) to FIG. FIG. 4 (d) is a schematic diagram for explaining the steps of the method for producing a gas generating agent of the present invention.

 In FIGS. 2 and 3, reference numeral 1 denotes a molding device g for a gas generating agent, which is a belt-shaped molding frame 4A to 4A, which is rotated, an IB driving mechanism 2, and slurry injection. »Composition 3

The drive mechanism 2 includes rotations 轴 8 A and 8 B rotatably supported between the front support columns 6 A and 6 B and the rear support columns 7 A and 7 B fixed on the ground 5, respectively. The rotating shaft 8B has a shaft 9a that engages via a gear 9A, and the main body 9B has a rotating device S9 (motor) fixed to the rear support column 7B. The cylindrical members 11 and 12 serving as a deformation function of the drive mechanism 2 are externally fitted and fixed along the axial direction, respectively. This The outer peripheral surface 1 1a, 1 2a of the cylindrical member 1 1.12 is formed in a shape in which the convex 13A and the concave 13B are continuous along the circumferential direction. 13 A and concave W l 3B are crawled along the axial direction of columnar material 11, 1 2 by li b. 1 2 b and other 0 »surface 1 1 c, 1 2 clS ing. The cylindrical members 11 and 12 have a convex 14 A and a concave 14 B associated with the convex 13 A and concave 13 B shapes, respectively. An annular belt 15 is stretched. Thus, when the motor 9 is driven, the rotating shaft 8B is rotated via the shaft 9a, and the annular belt 15 is connected to the rotating shafts 8A, 8BK via the columnar material 11.1.2. Rotated to circulate. In addition, the simplicity of the rotating shafts 8A and 8B is sufficiently simple to remove the water contained in the slurry-like gas generating composition P and to heat and solidify the gas generating agent. Have been.

A plurality of molding frames 4A to 4L are detachably fixed on the surface 15a of the annular belt 15 in the direction of the circulation movement. The molding frames 4A to 4L are made of silicone rubber, polybutene rubber, polybutylene chloride, butyl chloride, polyisoprene, nitrile rubber, isobutylene, acrylamide rubber, styrene sulfonated polyethylene, ethylene propylene rubber, It is made of one or more of fluororubber and urethane rubber or a mixture thereof, and is a non-gold flexible material having no adhesiveness with the gas generating composition Ρ. It is formed in a flat plate shape having the same width as 5 and a predetermined thickness. Also, in the forming frames 4A to 4L, a concave part 16 serving as a circular cross-sectional forming die having a predetermined diameter d and a depth h is provided in the direction of the circular belt 15 and the direction of circulation movement. , N columns · n rows (N-1, 2. · · ·, N, n = 1, 2, 3, · · ·, n, where n is an arbitrary numerical value. Only 10 6 = 60 in column 6 are formed.)). The diameter d and the depth h of the recess 16 are determined by the shape of the gas generating agent (tablet). The shape can be changed as appropriate.

 In addition, the slurry-like gas generating composition P is injected into each of the recesses 16 of the molding frames 4A to 4L on the side of the rotating shaft 8A, which is the side of rotation of the belt 15 of rotation. The slurry injection mechanism 3 is provided, and the rotating shaft 8B, which is the end-of-rotation side, is located on the rotating shaft 8B side. An inclined shooter 17 is thrown. A cushioning material 18 (rubber or the like) is attached to the surface of the shutter 17 facing the cylindrical member 12, and extends to the upper part of the product hopper 19. Injecting the slurry into the structure »No. 3 comprises a nozzle 3 A for injecting the slurry-like gas generating composition P into each of the recesses 16 of the molding frames 4 A to 4. And a moving device 3B that can move in multiple axes directions (vertical direction A, left and right direction B, front and rear direction C in FIGS. 2 and 3). It is connected to a slurry gas generating tank (not shown) via C. The nozzle 3A is provided with means (not shown) for controlling the injection S of the slurry to be injected into the recess 16 of the molding frames 4A to 4L (the diameter d of the recess 16 and the depth thereof). (The one that changes and controls the injection S based on the h and the tablet shape of the gas generating agent).

 Further, in the gas generating agent molding apparatus S1 in this embodiment, a heating method is employed in the drying and solidifying step of the gas generating agent composition P, so that the rotating shafts 8A and 8BK A heater 20 is provided, and while each of the molding frames 4A to 4L moves linearly between the rotating shafts 8A and 8B, each of the frames 4A to 4 is approximately 50 to 120. The hot air or hot air is blown out, whereby the slurry fibrous gas generating composition fiPP injected into each recess 16 is heated and dried to be solidified.

The apparatus 1 for forming a gas generating agent in the present embodiment has the above-described configuration. Next, a method for forming a gas generating agent using the apparatus S 1 will be described. , Figures 2, 3, 4 (a) to 4 (b)

(1) First, moving and hiding 3B of the slurry injection mechanism 3 is moved in the multi-axial direction, and the respective recesses 16 of the molding frame 4A on the annular belt 15 on the rotation start side are formed. An injection step of injecting a predetermined S slurry P from the nozzle 3A is performed within the state shown in the twentieth and third EIs. Then, the motor 9 is driven to move the annular belt 15 to the molded product shutter 17 side, and the molding frame 4A is linearly moved so as to retreat from the nozzle 3A. A molding frame 4B associated with A is positioned so as to face the nozzle 3A, and a predetermined amount of slurry P is injected from the nozzle 3A into each recess 16 of the molding frame 4B. Hereinafter, similarly, the slurry P is sequentially injected into the respective concave portions 16 of the forming frames 4C to 4L by the nozzle 3A.

 (2) While this injection step is being performed, the molding frames 4A, 4B.- are sequentially linearly moved to the molded product shutter 17 side, and the molding frames 4A, 4B. The slurry-like gas generating composition P injected into each of the recesses 16 of FIG. 6 reaches the heater 20 of Shimoguro, where hot air or hot air of about 50 to 120 described above is blown. The water in the slurry is evaporated and the gas generating agent is solidified to form a gas generating agent tablet Q having a predetermined shape. In particular, in the case of the above-described reaction-curable gas generating agent, a condensation reaction proceeds in this heating step, and a strong solid gas generating agent is generated.

(3) Further, when the molding frame 4A is moved linearly, the molding frame 4A moves along with the »pelt 15 around the rotation axis 8B on the circumference of the columnar material 1 2. It is rotated along. As a result, as shown in FIGS. 4 (a) and 40 (b), each of the recesses 16 of the molding frame 4A formed of a flexible non-metallic material has an opening 16a. (The elliptical shape is larger in the direction of circulating movement of the S-shaped belt 15 and smaller in the direction perpendicular to this direction.) Become. ) While being deformed elastically so as to reduce the diameter of the bottom 16b side, the gas deformation agent which is a molded product is separated from each hollow 16 by this elastic deformation, Due to the pressing force acting to push the gas generating agent Q out of each recess 16 by reducing the bottom 16 b side of the recess 16, the gas generating agent Q, which is a molded product, is placed in each recess 16. It jumps out of the box, falls on the scooter 17, and is collected in the molded article hobber 18 while rolling on the scouter 17. As described above, in the process of rotating each of the forming frames 4A to 4L along the circumference of the cylindrical member 12 together with the annular belt 15, each of the forming frames 4A to 4L is rotated. By elastically deforming the hollow 16 formed on the surface of L, a sampling step of extracting the gas generating agent Q as a molded product from each ω® 16 is performed.

 (4) After that, the molding frame 4A, on which the above-described extraction process is completed, is returned to its original shape (circular cross-section) in each of the concave portions 16 and the other molding frames 4C, In the opposite situation, the slurry is circulated back to the position S facing the nozzle 3 A of the slurry injection mechanism 3 on the rotating glaze 8 A side, and from above (1)

(3) In the same manner as described, the gas generating agent Q is formed through the above-described injection step, heating solidification step, and extraction step. Also, after the molding frame 4B to 4 is subjected to the extraction process in which the gas generating agent Q, which is a molded product, is extracted from each of the concave portions 16, the annular belt 15 sequentially rotates the rotating shaft side 8A. The slurry is circulated back to the position B facing the nozzle 3A of the slurry injection mechanism 3, and the above (

In the same manner as described in 1) to (3), the gas generating agent Q is formed through the above-described injection step, heating solidification step, and extraction step sequentially.

As described above, according to the method of manufacturing the gas generating agent of the present embodiment and the apparatus for forming the same, the forming frame 4 having the forming die formed by the large number of concave portions 16 made of non-metal having flexibility. The gas generating agent Q can be mass-produced by sequentially repeating A to 4 L in the order of the injection step, the heating solidification step, and the extraction step. Also, in order to extract the gas generating agent Q from the molded article formed in each of the concave molds 16, it is only necessary to elastically deform the concave mold 16 formed of this flexible material. Since it can be easily extracted, the gas generating agent Q, which is a molded product, is not chipped or cracked, and the yield of molded products can be improved. Since the friction between the agent Q and the concave portion 16 can be reduced, there is no danger of ignition and the safety at the time of molding the gas generating agent can be greatly improved.

 In the present embodiment, a heater is arranged at the upper part of the transfer of the molding frames 4A to 4L. The heater is arranged SB. However, this is another similar ripening and drying system, for example, a tunnel. It goes without saying that a method in which a wireless compare moves in the mold heating port or a far-infrared bran heating method can be adopted.

 In addition, in the molding apparatus fi of the gas generating agent in this embodiment, the nozzle 3A of the slurry injection mechanism 3 is shown as a single nozzle, but is not limited to this, as shown in FIG. In addition, the number of the nozzles 3A corresponding to the number of dents 16 (10 in this embodiment) formed in one row of the molding frames 4A to 4L is set to each dent. It may be thrown to correspond to 16 ο

 In this embodiment, the moving mechanism 2 is configured to circulate and deform the forming frames 4A to 4L by the configuration of the annular belt 15, the cylindrical members 11 and 12 and the motor 9. However, the present invention is not limited to this, and any configuration may be used as long as it effectively circulates and deforms the molding frames 4A to 4L, and the same effects as in the present embodiment can be obtained.

Further, the structure of the concave portion 16 serving as a molding die formed in each of the molding frames 4A to 4 is not limited to that of the present embodiment, and is shown in FIG. 6 to FIG. Such a structure may be used. The following shows the structure of the molding frame 4 A to 4 Modifications will be described with reference to FIGS. 6 to 9.

 No. 6E, the molding frame itself is formed of a material made of non-gold (5) having flexibility, and the molding die 16 is directly drilled into the glare frames 4A to 4L. It is formed, and »The base portion 16 A of the dents 16, 1 in contact is cut in the axial direction along the peripheral wall 16 c of the dent 16 and extends to this bottom 16 b. At least one line 25 is thrown into the base material of each recess in the row direction of the recess (the width direction of the frame). Are provided at two places in the frame width direction). As a result, when the molding frames 4A to 4L are elastically deformed, each of the recesses 16 having a circular cross section at the boundary of the break line 25 is deformed into a chair shape so as to increase the diameter d. This makes it easier to extract the gas generating agent Q formed in each of the recesses 16.

 In the seventh EI, the molding frame itself is formed of a non-gold JS material having flexibility, and a hollow 16 serving as a molding die is directly drilled in the truss frame 4A to 4L. This is an example of a case in which a substantially V-shaped groove having a predetermined depth is provided in a direction orthogonal to the circulation movement direction of the » 30 is thrown. As a result, when the molding frames 4A to 4L are elastically deformed, each of the concave portions 16 having a circular cross section at the boundary of the groove 30 is deformed into a circular shape so as to increase its diameter d. Then, it is easier to remove the formed gas generating agent Q.

In FIGS. 8 (a) and 8 (b), the molding frames 4A to 4L are composed of a flat plate 35 and a frame 36 having flexibility. In this frame 36, for example, seven cylindrical bodies 37 are integrated in one row (circular movement direction of the annular belt 15) in units of two rows (the width direction of the annular belt 15). Each of the cylinders 37 has its peripheral surface joined by an adhesive such as silicon or the like, and an end surface portion of the joined side (so that a part of the end surface is projected on the flat plate 35). Contact The flat plate 35 and the cylindrical body 37 form a hollow 16 as a forming die. Further, at least Ichiro of the peripheral wall 37 A of each cylindrical body 37 is cut in this axial direction, and a breaking line 38 orthogonal to the circulation movement direction of the annular belt 15 is formed. As a result, when the molding frames 4A to 4L are elastically deformed, they expand so that the peripheral wall 37 of the circular body 37 is divided into two parts by the break line 38, and the gas generating agent Q It is easy to extract from the drawer.

 In FIGS. 9 (a) and 9 (b), the molding frames 4A to 4L are formed by forming shallow recesses 42 on the surface of a flexible flat plate 35. The cylindrical body 40 is fitted into the inside of the tube 42 and raised, thereby forming a hollow 16 serving as a molding die. Further, each cylindrical body 40 is cut in the axial direction to form at least one force line at a breaking line 41 force <orthogonal to the circulating movement direction of the annular belt 15. As a result, the gas generating agent Q molded in each hollow 16 is deformed by the elastic deformation of the molding frames 4 A to 4 L so that the cylindrical body 40 is surrounded by the peripheral wall 41 A at the breaking line 41. The gas generating agent Q can be easily extracted since the gas generating agent Q can be spread and deformed so as to be divided into two parts.

 In addition, the shapes of the dents 16 serving as the molding dies formed on the molding frames 4A to 4L in the molding apparatus S1 of the gas generating agent of the present example are all circular oval. However, the shape of the concave portion 16 serving as a molding die is not limited to this, and the cross section of the concave portion 16 may be various shapes such as a rectangular shape or an elliptical shape, and the bottom shape of the K portion may also be changed. However, instead of being a flat surface, it may be a curved surface that is downwardly convex, and furthermore, the tokuburo 16 may be either integral with or separate from the molding die. Needless to say, a great effect can be obtained.

Also, the recess 16 may be integral with or separate from the molding dies 4A to 4L. Further, the S-shaped belt 15 and the molding dies 4A to 4L may be integrally formed. Needless to say, it may be a structure that can be replaced according to the application. With any of these structures, the same effect as in the above embodiment can be obtained.

 As described above in detail, according to the production method and apparatus of the present invention in which the gas generating agent is pelletized, the gas generating agent mixture is formed from a water slurry state, and thus has been regarded as the most dangerous in the past. This greatly improves the safety of the gas generating agent forming process.

 In addition, since a method is used in which the slurry is injected into the molding die in a single state, the molding shape is not limited to the conventional ridge-shaped tablet shape.

The choice of S is widened, and it is possible to select the optimal gas generating agent shape considering flammability.

 In addition, since the molding is started with the idea of a water slurry, a heating method which could not be adopted because it was conventionally dangerous can be adopted, so that the solidification speed is greatly improved, and therefore, the moving conveyor method is employed. The adoption of a drying and solidifying system is possible, and as a result, the equipment space can be reduced in size and continuous production can be achieved, and productivity can be dramatically improved.

 Further, in the molding apparatus B relating to the gas generating agent of the present invention, a concave portion serving as a molding die is formed on a surface node of the molding frame, and the slurry-like gas generating component is moved while moving the molding frame. Into the concave portion, heat-solidify the injected slurry-like gas generating composition, and remove the molded solid that has been solidified by elastically deforming the molding die. In addition, the gas generating agent can be easily formed and self-K can be easily formed, and the productivity can be dramatically improved.

In addition, since the molding die is formed of a flexible material, it can be easily extracted from the mold only by elastically deforming it, so that a special jig for extraction is not required, and the gas generating agent molded body is not required. There is no damage when extracting Product yield also improves.

 In addition, the mold section is formed of a non-metallic material having flexibility, and the molded article can be extracted only by its elastic deformation, so that there is almost no friction between the molded article and the mold portion. The generation of sparks at the time of removal, which was a major problem with the conventional method, is eliminated, and safety is dramatically improved.

 In addition, if the mold is made of a flexible non-gold JS material and has an axial cut in its peripheral wall, it is extremely easy to remove the molded product due to its elastic deformation.

 In addition, a combination of a plate with a flat plate and a plurality of rods erected in the form of a flat plate, or a flat plate having a shallow recess with a rod that is fitted in a triangular shape, or Various applications are possible, such as forming a cut in these cylinders in the axial direction to facilitate the elastic deformation of the mold when removing the molded product. It has the advantage that it can be adopted.

 In addition, silicone rubber, polybutadiene, buried clay, polyisoprene, nitrile rubber, isobutylene, acrylamide rubber, chlorosulfonated polyethylene, ethylene propylene rubber, and fluorine rubber are used as flexible materials for mold parts. Since one or more urethane rubbers or a mixture thereof can be used, molding of a mold can be performed easily and at low cost. Productivity availability

 INDUSTRIAL APPLICABILITY As described above, the present invention relates to a gas generating agent which is excellent in moldability and combustion stability, and whose combustion characteristics can be easily and safely adjusted, and a method for producing the same. It is most suitable as a gas generating agent to be used or a gas generating agent for projectile propulsion, and a production method thereof.

Claims

Scope of request

 1. A gas generating agent containing a gas generating component and an oxidizing agent, wherein the gas generating component is at least one of the following reaction products of (1) to (d): .

(a) with ammonia or a compound having an NH- one NH _a Motowaka properly during the or structural formula, an organic compound is also an organic compound having one CHO group in the structural formulas, which may occur an CH 0 groups Reaction product obtained by reaction o

 (W A secondary reaction product obtained by reacting the reaction product obtained in the above (a) with a compound having a mono-OH group in the structural formula.

(c) a compound having an NH _a group or one NH- in the structural formula and the reaction product obtained by reacting a N- methylcarbamoyl o- le compound.

(d) A reaction product obtained by reacting a compound having one NH _a group or one NH— in the structural formula with an N-alkoxy compound.

2. The of claim 1 (a), the compounds in the structural formula with an NH _a group or one NH- according to (c) or (d), mono E pentanol § Mi emissions, human Dorowishiami down, Horumuami Amide, carboxylic acid amide, carboxamide, azodicarbonamide, hydrazodicarbamide, aminomonopropanol, azobisformamide, semicarbazide, acetonsemicarbazone. Hydrazine. Forminolehydrazine, formamidine Carbohydrazide, Cyanamide, Dicyandiamide, Aminothetrazole, Guanidine. Aminogudine. Triaminonoguanidine nitrate, Nitogazin, Hazodiguanidin. Biuret, urea, monohydrokine urea. Thiourea, melamine, gel Roh Lumpur § Mi emissions, mono Echiruami Nomono Etanoruami down, to Kisamechirente door La Mi emissions, door Li Azoru, Te Torazoru, the Activity Torazo Ichiru or of these At least one kind selected from the group consisting of salts;

3. The compound having one NH _a group or one NH— in the structural formula according to claim 1 (a) is azodicarbonamide, tetrazole, aminotetrazole, bitetrazole, triazole, One or two or more selected from the group consisting of melamine or metal salts thereof;

 Guadine, triaminoguanidine nitrate, guanidine diacid, guanidine carbonate, dicyandiamide, hexamethylenetetramine, biuret, hydrazine, carbohydrazide. 2. The gas generating agent according to claim 1, wherein the gas generating agent is a combination of at least one selected from the group consisting of gold and clay.

 4. The compound having one NH— in the structural formula according to claim 1 (a), (c) or (d) is obtained by subjecting the product K according to claim 2 to N-methylol treatment. The gas generating agent according to claim 1, which is a gas generating agent.

 5. The organic compound having one CH 0 group in the structural formula according to claim 1 is a formaldehyde, an acetoaldehyde, a σ-pionaldehyde, an η-butyl aldehyde, an η-butyl aldehyde. The gas generating agent according to claim 1, which is at least one member selected from the group consisting of viraldehyde, η-bronaldehyde, acrolein, quenth aldehyde, and glyozal.

 6. The organic compound capable of forming one CHO group according to item (a) of the above-mentioned S claim 1 is formamide, paraformaldehyde. Trioxane, hexamethylenete tramine, tetraooxansan, metaaldehyde, azobis. The gas generating agent according to claim 1, which is at least one member selected from the group consisting of formamide.

7. The compound having a single OH group in the formula shown in claim 1 (b) is a compound having a single OH group combined with carbon (C) or nitrogen (N). Item 7. The gas generating agent according to item 1.

8. The compound having a mono-OH group bonded to carbon (C) or sulfur (N) is selected from the group consisting of methanol, ethanol, monoethanolamine, aminopropanol, diethanolamine, and hydride. 8. The gas generating agent according to claim 7, wherein the gas generating agent is at least one selected from the group consisting of oral kissil hydrazine, ethylaminoethanol, hydroxylamin, hydroxyylurea, formamide, annual sim, and formaldoxime.

 9. The N-methylol compound according to (c) of the claim 1 is obtained by subjecting the product K according to claim 2 or 4 to an N-methylolation treatment. The gas generating agent according to the above.

 10. The claim 1 wherein the N-alkoxy compound described in (d) of the S claim 1 is obtained by subjecting the substance described in the claim 2 to N-alcoholization. The gas generating agent as described.

 11. The gas generator according to any one of claims 1 to 10, wherein the gas generating agent contains 10 to 40% by weight of a gas generating component and 50 to 80% by weight of an oxidizing agent. Gas generating agent.

 12. The gas generating agent contains 10 to 40% by weight of a gas generating component, 50 to 80% by weight of an oxidizing agent, and 1 to 10% by weight of a fuel catalyst component. The gas generating agent according to any one of claims 1 to 10.

 13. The method according to claim 11, wherein the oxidizing agent is at least one member selected from the group consisting of nitrates, oxohasgen D-genates, and gold oxides. The gas generating agent as described.

 14. The method according to claim 13, wherein the nitrate is at least one member selected from the group consisting of sodium nitrate, potassium nitrate, barium nitrate, ammonium nitrate, and sodium nitrate. The gas generating agent according to the above.

15. The oxalate salt is one or two selected from the group consisting of chlorate, perchlorate, bromate, bromate, iodate, and periodate. 14. The gas generating agent according to claim 13, which is at least one species.

 16 6. The above-mentioned ox-sodium p-genate is tt [sodium citrate, potassium oxalate, sodium perchlorate, potassium perchlorate, ammonium nitrate, element 14. The gas generating agent according to claim 13, wherein the gas generating agent is at least one member selected from the group consisting of acid lime, potassium bromate, iodate lime, and iodate lime.

 17. The gold) S oxide is one selected from the group consisting of manganese dioxide, iron oxide, zinc dioxide, potassium peroxide, and potassium manganate. Barium oxide and molybdenum trioxide 14. The gas generating agent according to claim 13, which is at least two types.

 1 8. The combustion catalyst is an element selected from the group consisting of zirconium, hafnium, molybdenum, tantalum, manganese, iron, nickel, kum, titanium and oxides or sulfides, carbon, phosphorus, and sulfur. 13. The gas generating agent according to claim 12, wherein the gas generating agent is at least one kind.

 1 9. A method for producing a gas generating agent comprising a gas generating component and an oxidizing agent, wherein the gas generating component has the following (a) to! d) comprising one or more of the reaction products, and adding an oxidizing agent to the reaction product to form a slurry having a predetermined viscosity; forming the slurry into a desired shape; A method for producing a dry-solidified gas generating agent.

(a) Ammourea or a salt thereof, a compound having one NH ₃ group or one NH— in the structural formula, and an organic compound having one CH 0 group or one capable of generating a CHO group in the structural formula Reaction product obtained by reaction

(b) A secondary reaction product obtained by reacting the reaction product obtained in the above (a) with a compound having a 10 H group in the structural formula.

(C) a structural compound having an NH _a group or one NH- in formula, N- methylcarbamoyl A reaction product obtained by reacting with a roll compound.

(ci) compound in the structural formula with an NH _a group or one NH- and the reaction product obtained by reacting N- alkoxy compound.

20. A method for producing a gas generating agent comprising a gas generating component and an oxidizing agent, wherein the gas generating component comprises at least one of the following reaction products (1) to (W). An oxidizing agent is added to the reaction product and mixed to form a slurry having a predetermined viscosity, and the slurry is dried and solidified to form a powder, and then, the powder is pressed into a desired shape. A method for producing a gas generating agent.

 (a) Ammonia or a salt thereof or a compound having a hydroxyl group or 1 NH- in a building formula, and an organic compound having a 1 CHO group or a general compound capable of generating a 1 CHO group in a structural formula Reaction product obtained by reacting

 (U) A secondary reaction product obtained by reacting the reaction product obtained in (1) with a compound having a mono-OH group in the structural formula.

(c) A reaction product obtained by reacting a compound having one NH ₂ group or one NH— in the structural formula with an N-methyl compound.

(d) A reaction product obtained by reacting a compound having one NH _a group or one NH— in the structural formula with an N-alkoxy compound.

 21. The reaction product according to claim 19, wherein the reaction product is condensation-cured by subjecting the molded product formed into the desired shape to a heat treatment at a temperature of 90 "C or more. Production method of gas generating agent.

22. A method for producing a gas generating agent comprising a gas generating component and an oxidizing agent, wherein the gas generating component comprises at least one of the following reaction products (1) to (d). Yes, an oxidizing agent is added to this reaction product and mixed to form a slurry having a predetermined viscosity, and this slurry is poured into a flexible non-gold IS mold and then solidified by heating. A method for producing a gas generating agent. (a) Anmoyua or reaction with a compound having an NH _a group or single NH- in its salt or構迪formula, an organic compound is also an organic compound having one CHO group in the structural formulas, which may occur an CHO group Reaction product obtained

(b) A secondary reaction product obtained by reacting the reaction product obtained in the above (a) with a compound having a 10 H group in the structural formula.

(c) a compound having an NH _a group or one NH- in the structural formula and the reaction product obtained by reacting a N- methylcarbamoyl o- le compound.

(d) compounds in the structural formula with an NH _a group or one NH- and the reaction product obtained by reacting N- alkoxy compound.

 2 3. A step of injecting the slurry into the molding die provided on a rotatable »-shaped belt by means of an annular belt, and rotating the annular belt into the molding die. The gas generation according to claim 22, comprising: a heating and solidifying step of heating and solidifying the composition; and a step of removing a gas generating agent pellet solidified in another part of the annular belt. Method of manufacturing the agent.

 2 4. A device B for producing a gas generant bevel for forming a slurry of a gas generant composition containing a gas generant component and an oxidant into a predetermined shape,

 Molding frame body UA)-() which has a plurality of hollows (16) formed of a material made of gold R having flexibility and serving as a molding die on a surface node, and is formed in an annular belt shape. When,

 tt a drive mechanism (2) for rotating the frame,

 An injection mechanism (3) installed in Ichirou of the K frame and injecting the gas generating composition slurry into the concave portion Q6>;

 7. A gas generator pellet manufacturing equipment that has a heating system (20) that heats and solidifies the gas generator composition slurry of Tokubo Nero!

2 5. The molding frame (4 to (4) is set up on a flat plate (35) and a flat plate The concave portion (16) is formed by a plurality of flexible non-metal bodies (37), and at least one of the ridges (37A) of the body (37) moves in the axial direction and in the frame body. 26. The device for producing a gas generant beret according to claim 24, further comprising a slitter (38) in a direction perpendicular to the direction.

 26. A shallow concave (42) is cast on the flat plate (35), and at least one portion of the peripheral wall is directed in the axial direction and at right angles to the direction in which the frame advances in the Dfl. Item 24. A gas generating agent pellet manufacturing apparatus according to Item 24, wherein the gas generating agent pellet is formed by fitting a flexible non-metallic body (40) having a cut-off portion (41) on the surface thereof.

0

 2 7. The molding frame (4 to (4)) is made of a flexible non-gold JS material, and forms a concave part (16) which is formed in the surface thereof and becomes a molding die. 25. The crack of the gas generating agent beret according to claim 24, wherein a cut portion (25>) is provided in at least one position of the frame base material between the K-Kuro and the axial direction thereof. Manufacturing equipment.

28. The molding frames (4A) to (4) are made of a flexible non-metallic material, and the concave portion (16) is formed on the surface thereof, 24. The apparatus S for producing a gas generating agent pellet according to claim 24, wherein a groove (30>) is formed in a direction perpendicular to a traveling direction of the frame.

Summary Form

 An object of the present invention is to provide a gas generating agent which is excellent in moldability and combustion stability, whose characteristics are easy to adjust, and whose manufacturing process is safe, a fi method for manufacturing the same, and a device B for manufacturing a gas generating agent belt. .

 The present invention relates to a gas generating agent comprising a gas generating component and an oxidizing agent, wherein the gas generating component comprises at least one of the following reaction products (1) to (dj): The production method and the production and production of the gas generant pellets are hidden.

(a) Ammourea or its clay or a compound having one NH _2. group or one NH— in the structural formula, an organic compound having one CHO group in the structural formula or an organic compound capable of generating one CHO group Reaction product obtained by reacting

(b) A secondary reaction product obtained by reacting the reaction product obtained in (a) with a compound having a mono-OH group in the structural formula.

(c) a compound in the structural formula with an NH _a group or one NH-, reaction product obtained by reacting N- methylol compounds.

(d) compounds in the structural formula with an NH _a group or one NH- and the reaction product obtained by reacting N- alkoxy compound.