CN1651360A - Gas producing composition and its preparation method - Google Patents
Gas producing composition and its preparation method Download PDFInfo
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- CN1651360A CN1651360A CN 200510059361 CN200510059361A CN1651360A CN 1651360 A CN1651360 A CN 1651360A CN 200510059361 CN200510059361 CN 200510059361 CN 200510059361 A CN200510059361 A CN 200510059361A CN 1651360 A CN1651360 A CN 1651360A
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Abstract
An aerogenic composition used for protecting the passengers in coach and airplane is prepared from fuel, oxidant, ignition improver and adhesive. Its preparing process is also disclosed. Its advantages are high air output and high properties.
Description
Technical field
The present invention relates to a kind of gas-generating agent composition and preparation method thereof, particularly a kind of automobile, aircraft etc. of being used for are with gas generating powder in protection passenger's the air bag generator and preparation method thereof.
Background technology
As everyone knows, the air bag of using on the automobile comprises: pyrotechnic air bag and hybrid air bag.Wherein the pyrotechnic air bag is to utilize the gas of the burning generation of gas producing medicinal to be full of the protection of airbag realization to the occupant in moment; Hybrid-type air bag is to have mixed the compression cold air that presets in gas producing medicinal burning generation hot gas and the tightness system to be full of airbag, thereby realizes the provide protection to the passenger.
The gas producing medicinal that air bag is used belongs to the pyrotechnics composition category, and with military compound gunpowder many similarities is arranged.As the gas generating powder of pyrotechnic composition because its purposes special has some to can be rated as harsh particular requirement.For example the toxicity of the gas of gas producing medicinal burning generation will be controlled at minimum, gas production rate is big, thermostability will be got well, the smog that produces is minimum, and the temperature of the gas of generation is low, and combustionvelocity is suitable, burning rate pressure exponent is little, burning rate temperature coefficient is little, and ignition-delay period is short, and various mechanical sensitivities and sensitivity are little or the like.Above these all are subjected to the influence of initial composition (starting components), thereby, when producing gas producing medicinal, to satisfy these requirements all the time, if there is the production method that is more suitable for these requirements better.
Producer gas generator often uses the gas generating powder that contains sodiumazide, and this medicine has many shortcomings: sodiumazide is a severe toxicity, in production, use producers and environment is brought harm and pollution; Also have it to adopt the dry blend tablet forming technique, dust is big in the production process, and security incidents such as detonation easily take place.Therefore, at present, brought into use safe non-azide fuel to replace sodiumazide, its toxicity is lower, and performance that aborning human and environment is all had no adverse effects, every can both meet or exceed trinitride type gas generating powder.
Such as, application number 96198112.1, denomination of invention is a kind of gas-generating agent composition, discloses a kind of calorific value low heat value with the gentle reduction of the low combustion of low combustion temperature, and can reduce the volume of producer gas generator self.Contain nitroguanidine and a kind of oxygenant in this gas-generating agent composition as basal component, this oxygenant comprises the nitrate or the nitrite of (a) basic metal and alkaline-earth metal, (b) be selected from the monoxide or the polyoxide of one or more metals of copper, cobalt, iron, manganese, nickel, zinc, molybdenum and bismuth, perhaps the mixture of component (a) and component (b).
Application number is 00813289.5, denomination of invention is basic metal nitrate, its manufacture method and gas-generating agent composition, a kind of basic metal nitrate of the suitable oxygenant of using as gas generating agent is disclosed, and have hypotoxicity, high rate of combustion and low combustion temperature, and can be used for the gas-generating agent composition of the aerogenesis machine that air bag uses; This gas-generating agent composition comprises (a) terazole derivatives, guanidine derivative or its mixture, (b) basic metal nitrate and (c) tackiness agent and/or slag forming agent.
Application number is 01804546.4, and denomination of invention is the gas-generating agent composition that contains pyrrolotriazine derivatives, discloses a kind of comprising of (a) pyrrolotriazine derivatives, (b) basic metal nitrate and optionally (c) tackiness agent and/or (d) gas-generating agent composition of additive.This gas-generating agent composition has reduced toxicity and has improved rate of combustion and reduce temperature of combustion.
Application number is 200310105915.0, denomination of invention is a kind of gas generating powder that is used for automobile safety air bag gas generator and preparation method thereof, this gas generating powder is mixed and is formed by negative oxygen combustible agent, oxygenant, slag former, tackiness agent, it is a kind of non-azide type gas generating powder, every performance all is better than the sodium azide type gas generating powder, and this medicine can substitute the trinitride gas generating powder and be used in the multiple air bag generator of current popular; The wet mixing extruding shaping technique is adopted in its preparation, and this gas generating powder medicine toxicity is very low, during production human and environment is had no adverse effects; Be fit to large-scale low-cost production, the production process dust is few, and security is very high; The gas producing efficiency height of this medicine is about 1.7 times of sodium azide type gas generating powder, and burning back solid residue is few simultaneously, residue fusing point height, easily filter, this makes producer gas generator create essential condition to miniaturization, lightweight development for simplifying the producer gas generator filtering system.
EP1279655 discloses a kind of gas generating powder production method, and wherein gas producing medicinal comprises fuel (a), oxygenant (b) and annexation (c).The normally nitrogenous compound that fuel is used, nitrogenous compound comprises one or both compounds at least, oxygenant comprises in the following nitro material one or both at least as composition b, comprising: basic metal nitrate, base metal nitrate and alkine earth metal nitrate; The production method of gas producing medicinal also is provided, and the first step is a batching, comprises two or more initial compositions, and fuel and oxygenant are arranged, then restir and mixed under dampness; Second step was mixture extrusion molding, re-shearing; The 3rd step was oven dry; Also provide with twin-screw extruder under dampness, mediated, mixed the production method of the gas generating powder of initial composition; By this production method, can obtain high-quality gas producing medicinal.
The gas generating powder of prior art generally is made up of with the binding agent relevant with technology one to two kind of fuel, no more than three kinds of oxygenants and part modifying agent, only pays attention to one of them performance of gas generating powder mostly, big such as gas production rate, maximum reached at 3.6mol/100g.But this gas generating powder has often only been considered oxygen-supplying amount because of oxygenant, and has ignored the sensitivity of gas generating powder, so this type of gas generating powder sensitivity is relatively poor, so just makes it be limited in the selection of production technique, and hazard level is also than higher when using certainly; Thereby make prescription very big shortcoming be arranged at some key property.
Summary of the invention
The object of the present invention is to provide a kind of rational proportion that utilizes various fuel and oxygenant, performance complement, thereby produce and a kind ofly have higher gas production rate and sensitivity is low, Heat stability is good, the technology suitability is good, ignition characteristic is good, the residue rate is low, the gas-generating agent composition of high comprehensive performance.
Another object of the present invention is to provide a kind of preparation method of gas-generating agent composition, on production technique, suit to have adopted continuously extruded kneading of twin screw to extrude, the also production technique that can adopt roll-in to extrude in flakes, solved in the compressing tablet production problem that gas generating powder production efficiency is low, production cost is high.
In order to realize the object of the invention, the invention provides a kind of gas-generating agent composition, comprise following component and content: 20～70% fuel, 25～75% oxygenants, 0.5～5% igniting modifying agent and 0.5～5% binding agent, content is weight percentage.
Preferably: 30～60% fuel, 35～65% oxygenants, 1～3% igniting modifying agent and 0.5～5% binding agent, content is weight percentage.
Content of the present invention is weight percentage.
Wherein, described fuel is two or more the mixing in guanidine class, azole and the nitrogen-enriched compounds such as derivative, pyrrolotriazine derivatives thereof, and is preferred with being mixed into of 2～5 kinds of compositions.On the basis of taking all factors into consideration factors such as oxygen balance, gas production rate, sensitivity and consistency, the component of fuel can be carried out arbitrary proportion and be mixed.
Described guanidine class can be Dyhard RU 100, nitroguanidine, Guanidinium nitrate and allied substances, be at least a kind of in the guanidine class material of introducing below, as Dyhard RU 100, nitroguanidine, Guanidinium nitrate, Guanidinium carbonate, amino-guanidine nitrate, diamino Guanidinium nitrate, triamino Guanidinium nitrate, nitroaminoguanidine nitrate (nitric acid nitre ammonia guanidine) is good with nitroguanidine and dihydro-amine wherein.
Described azole is diazole, triazole, tetrazolium or its derivative, terazole derivatives such as pentaamino tetrazolium and allied substances, oxadiazole derivative such as diazole Secondary ammonium phosphate salt and allied substances, triazole derivative such as tetramino triazole and congener.
Described pyrrolotriazine derivatives can be oxamide, ammonium oxalate, three hydrazine triazines or hydrazodicarbonamide (hydrazo volatile salt) and allied substances etc.
Fuel of the present invention serves as preferred with industrial easy acquisitions such as pentaamino tetrazolium, Dyhard RU 100, nitroguanidine, Guanidinium nitrate, oxamide, ammonium oxalate and cheap nitrogen-enriched compounds; Be the optimum fuel combination wherein with Guanidinium nitrate, nitroguanidine, Dyhard RU 100 or Guanidinium nitrate, nitroguanidine and pentaamino tetrazolium.From producing and economic angle, generally can select to be easy to get, easily processing, fuel that harmful grade is low, cheap.
When fuel when being main with the guanidine compound of Guanidinium nitrate or nitroguanidine, select gas-generating agent composition based on Guanidinium nitrate, the content of Guanidinium nitrate is 20～50%, is preferred plan with 30～45% weight percentage wherein; The amount of nitroguanidine and Dyhard RU 100 or pentaamino tetrazolium is good to be no more than 80% of Guanidinium nitrate, the selection of concrete content and oxygenant has substantial connection, and those skilled in the art can adjust in this scope on the basis of the over-all properties of considering gas generating powder and reasonably oxygen balance.
Described oxygenant can be in nitrate, metal oxide or the perchlorate one or more mixing.
Described nitrate is base metal nitrate, alkine earth metal nitrate or subnitrate, for example lithium nitrate, SODIUMNITRATE, saltpetre, cesium nitrate, beryllium nitrate, magnesium nitrate, nitrocalcite, strontium nitrate, nitrate of baryta, basic copper nitrate, alkali formula iron nitrate or ammonium nitrate.
Described metal oxide can be the oxide compound of copper, iron, zinc or manganese, such as cupric oxide, ferric oxide, manganese oxide or zinc oxide.
Described perchlorate is sodium perchlorate, lithium perchlorate, potassium perchlorate, cesium perchlorate, magnesium perchlorate, calcium perchlorate, perchloric acid strontium, barium perchlorate or ammoniumper chlorate.
Generally primary oxidant in the oxygenant of the present invention with the basic metal nitrate, with conventional nitrate or perchlorate is secondary oxygenant, metal oxide is as the 3rd oxygenant, its effect also can be regarded as burning ratemodifier, can improve the combustioncharacteristics of product, for example combustion speed, duration of combustion, ignition characteristic.
Wherein oxygenant is a best of breed with basic copper nitrate, cupric oxide, ferric oxide and SODIUMNITRATE.Oxygenant of the present invention is main oxygenant with basic copper nitrate, and its weight percentage in total gas generating powder is 25～60%, and optimum is 35～50%.The content of SODIUMNITRATE is 10%～20% of basic copper nitrate, and optimum amount is 15%～17% of a basic copper nitrate.The content of the 3rd oxygenant ferric oxide and cupric oxide is 5～80% of basic copper nitrate, and wherein 30～45% is the most suitable, and the proportioning of ferric oxide and cupric oxide is 1: 0.5～1: 5, and optimum ratio is 1: 2.
Described igniting modifying agent can be selected aluminium sesquioxide, cupric chloride, cupric chromate or potassiumchromate for use; Its content is 0.5～5% of gross weight, is the best with 1～3%.Be preferably ultra-fine high purity aluminium sesquioxide, purity is 99.99%, and median size is 1.6 μ m.
Described binding agent can be water soluble cellulose, water soluble cellulose salt or guar gum (have another name called and be guar gum) etc.Binding agent is preferably Xylo-Mucine or food grade guar gum, and the content of binding agent should not surpass 5%.
Various starting material of the present invention can be by median size 1.4 μ m, median size 6 μ m, three kinds of rational gradation compositions of median size 20 μ m.
Gas production rate 2.5～the 2.8mol/100g of gas-generating agent composition of the present invention, wherein water vapor accounts for 30%～55% (calculated value) of cumulative volume percentage composition, and the nitrogen volumn concentration is 25%～45% (calculated value), and all the other are carbonic acid gas.So the very environmental protection of aerogenesis thing, no chlorine produces, the smell nonirritant.And fuel does not use triazo-compound yet, but the nitrogen-enriched compounds that adopts.
Gas-generating agent composition sensitivity of the present invention is better, and 10kg drops hammer, and 25cm drop height, the impact sensitivity of 50mg dose are 0%～8%.3.92MPa, 90 degree pivot angles, the friction sensitivity that the 20mg dose records is 0%.
Heat-resistant quality is good, records 100 ℃ according to the GJB772A-1997 vacuum stability test, and 48 hours discharge quantity is 0.21～0.45ml/5g.
Decomposition temperature is moderate, and the initial decomposition temperature that the DSC test records is 155～170 ℃.
Combustion temperature is low, because based on the oxygenant of basic copper nitrate and cupric oxide, its after product that burns is a copper, the thermal conductivity of copper is good, and as a kind of metal, it has absorbed the part heat that chemical process is, thereby makes temperature of combustion be lower than used gas generating powder.
Rate of moisture absorption is low, because used starting material are all non-hygroscopic except SODIUMNITRATE, and the content of SODIUMNITRATE in gas generating powder is very few, so gas generating powder was deposited under 65% relative humidity 48 hours, rate of moisture absorption is less than 1%.
And the present invention is because the adding of igniting modifying agent aluminium sesquioxide makes the gas generating powder of this invention be easier to igniting with respect to other basic copper nitrate gas generating powder, the ignition-delay period weak point.
The residue rate that gas-generating agent composition of the present invention generates is lower, is generally 5～15%.And the residue shape that generates is similar to the original shape of gas generating powder, does not have any crushing residua and produces.So just make used filter screen combination to simplify greatly, thereby more help the design of small-sized producer gas generator.
The present invention has adopted the starting material as prescription such as pluralities of fuel, multiple oxygenant, binding agent, burningrate catalyst, make the performance of gas generating powder that lifting significantly be arranged, have not only that higher gas production rate but also sensitivity are low, Heat stability is good, the technology suitability is good, ignition characteristic is good, the residue rate is low, so be a kind of prescription of high comprehensive performance.Gas generating powder gas production rate of the present invention is big, the combustion temperature is low, the ignition delay phase is short, non-hygroscopic, residue filters easily.Gas generating powder of the present invention can be used in automobile, the aircraft etc. the air bag generator with the protection passenger, also can be used for the producer gas generator of other type.
For realizing another goal of the invention of the present invention, gas-generating agent composition of the present invention can adopt three step process to machine, three steps can be produced continuously together, also can be interrupted batch production, except as otherwise noted, the processing parameter of each following step can be applicable to and be interrupted in production and the continuous production.
The preparation method of a kind of gas-generating agent composition of the present invention comprises the steps:
The first step is to mix, wherein comprise confusing between the same raw materials different-grain diameter, the part mixing of various fuel or oxygenant, comprise the preliminary mixing and the last abundant kneading when containing water medium of all raw material, blend temperature range is controlled at 30～80 ℃, optimum temperature is at 40～60 ℃, and soaking time is 4～6 hours; The amount of water medium distilled water is 15%～30% of a starting material total amount;
Second step was moulding, was interrupted extruding of process using plunger tpe or roll-in, and continuous processing adopts the twin screw extrusion moulding, and the moulding jacket temperature is at 40～60 ℃, and extrusion pressure is advisable to be no more than 10MPa, and the water content of extrudate is reduced to and carried out pelletizing below 10%;
The 3rd step was dry, in baking oven or various pan dryer, divide a step, two steps or more multistep carry out drying, the water content that is dried to gas-generating agent composition is less than 0.5%.
Specifically, a kind of preparation method of gas-generating agent composition comprises the steps:
The first step is to mix.Wherein comprise confusing between the same raw materials different-grain diameter, the part mixing of various fuel or oxygenant comprises the preliminary mixing and the last abundant kneading when containing water medium of all raw material.
The confusing of same raw materials different-grain diameter can be looked the relevant mixing equipment of its raw-material sensitivity different choice, such as chemical stabilitys such as Guanidinium nitrate, cupric oxide, ferric oxide preferably material just can select conventional chemical industry mixing equipment; Nitroguanidine, basic copper nitrate etc. have the starting material of certain danger to equip with the mixing of the safety with corresponding explosion proof ratings.If small size production, above-mentioned being mixed in advance can be used manual operations.
For the sake of security, the mixing of oxygenant must use independent mixing equipment.
The difference of process choice is looked in kneading when containing water medium, and different kneading devices is arranged.Between breaking process can select flat mixer, vertical mixer or vertical helical mixing machine, also can carry out continuous married operation merely at mixing step.Form the semicontinuous production technique of this step such as adopting continuous feeding machine, mixing machine, bolt special.The suitable twin screw extrusion equipment of selecting of continuous processing.Wet mixing is still carried out all will being incubated in various upright, horizontal kneaders at twin screw extruder, insulation is carried out in the insulation jacket of each equipment, temperature range should be controlled at 30～80 ℃, and optimum temperature is at 40～60 ℃, and soaking time is 4～6 hours.Used water medium preferably uses the distilled water of low conductivity, can get rid of the institute of water medium metal ion own like this disturbs the accident of prescription, such as influencing its thermostability or stability, make the thermostability of gas-generating agent composition inconsistent, perhaps increasing of mechanical sensitivity value unknown cause, even may become the potential safety hazard of production.
The consumption of distilled water and subsequent technique relation are very big, if adopt the plunger extrusion molding, the water-content during kneading should be 15%～30%; Adopt rolling process, water-content can be 15%～20%; Adopt the continuous extruding technology moulding, water-content is suitably 15%～30%, if twin screw equipment design safety rank is higher, water-content suits 10%～20%.No matter adopt any hybrid mode, for guaranteeing safety in production, mixing section should not be lower than 10%.Because guarantee safety in production.
Second step was moulding, interruption process using of the present invention plunger tpe extruding and roll-in, continuous processing adopts the twin screw extrusion moulding.Between the twin screw extrusion moulding gas generating powder medicine grain net shape of the plunger extrusion molding of breaking process and continuous processing relevant with the prescription of gas-generating agent composition, quality combustion speed own is filled a prescription faster and can be extruded diameter 20～60mm, and the centre has some to reserve cylinder, quincunx cylinder, the Polygons cylinder of through hole.The slower prescription of quality combustion speed, suitable extruding about diameter 3mm has through hole or do not have through hole, and length is the little medicine grain about 3mm.The pressure of extruding also has substantial connection with Types of Medicine.Can control jacket temperature during moulding at 40～60 ℃.The size of extrusion pressure is also relevant with the content of prescription and moisture, when the combustion speed of prescription is very fast, can increase extrusion pressure, helps obtaining more closely knit gas-generating agent composition like this.But be advisable to be no more than 10MPa, because the extrusion pressure that increases causes the generation of dangerous accident easily.If the shape of the gas generating powder of extruding is designed to middle sky, then must partly carry out the strictness design at the mouth mould.
The rupturing operation that extrudate generally must suit just can be carried out next step drying process, for moisture content bigger extrude bar, can be air-dry or in baking oven, spread suitable expelling water out, during to the suitable pelletizing operation of moisture content, carry out pelletizing.The twin screw extrudate of continuous processing can carry out die face cutting, in other words, is exactly the dicing machine of end face design at extrusion neck ring mold, finishes the pelletizing operation by it.In order to make extrudate moulding unanimity, surpass 18% material for moisture content, requirement was carried out expelling water before arriving mouthful mould, the expelling water device is suitable to be arranged on the penult twin screw cylindrical shell, the present invention has adopted vacuum pumping method to carry out expelling water, the water content of extrudate is reduced to below 10%, and the good article rate of pelletizing just can be controlled at more than 95%.For guaranteeing that the safety that twin screw is extruded carries out, pressure transmitter and venting of dust explosion mouth are set at each mixing section and mouthful mould place of twin screw.
Except that above-mentioned pellet cutting method, also can use the check rod pelletizing, just extrudate is involved with track type check rod machine, carry out usefulness behind the machinery or the natural medicine of a cold nature, dicing machine such as reciprocating type, marking knife formula, vertical cut formula and planer-type carries out rupturing operation.Also can select the medicine cutter up and down of the higher special use of precision for use.This kind medicine cutter divides two portions up and down, last medicine cutter by travelling belt, pressure roller, cut chain cover, lead the chain cutting knife and wheel box is formed, following medicine cutter is made up of body, leakage batch pan, transmission shaft, the linear velocity of travelling belt is than the fast 5～10mm/s of extruded velocity.The medicinal strip of being sent here by travelling belt is cut into the medicine section of certain-length by last medicine cutter, and the medicine section enters in the hole of batch pan Lou along conduit, falls on the supporting cup of control length, is leaked the cutting knife cut-out that batch pan rotates below, falls into and connects the medicine funnel.
Rolling process also is that this prescription is fit to one of moulding process that adopts, because adopt rolling process, in the process of roll-forming, can further plastify material, thus the mechanical property of raising gas generating powder finished product.During roll-in, the Types of Medicine thickness of design is the main foundation of dancer rools distance, and roll spacing is generally 0.2～7mm, and the adjusting of rotating speed is according to the viscosity and the processability of material, and rotating speed is generally 10～150 rev/mins.The tablet of roll-forming passes through the slitting shear machine slitting again, is cut into regular Fang Ding through dicing machine or slicing machine again, enters down drying process one.
The 3rd step was the medicine grain that obtains in dry second step, and in batch process and continuous production, drying treatment can be carried out in baking oven, also can carry out in various pan dryers, before entering baking oven, also can carry out preliminary drying, top-baking equipment is of a great variety, and development is very fast, for example, can select portable pre-baking oven, top-baking equipments such as preliminary drying tower, drum-type predryer.Withering purpose is in order to control the fugitive constituent in the gas producing medicinal, and dry intact moisture content of finished products content should be controlled at best below 0.3% (mass ratio) less than 0.5%.Drying means is if a step finishes, and drying temperature is 60～120 ℃, and 80～120 ℃ more suitable.Certainly, also can be two steps or more multistep carry out drying suddenly, to require predrying temperature be 30～75 ℃ to drying process like this, 30～60 ℃ best; The drying temperature in the step is at 75～120 ℃, and 80～110 ℃ more suitable.
The present invention has adopted the starting material as prescription such as pluralities of fuel, multiple oxygenant, binding agent, burningrate catalyst, make the performance of gas generating powder that lifting significantly be arranged, have not only that higher gas production rate but also sensitivity are low, Heat stability is good, the technology suitability is good, ignition characteristic is good, the residue rate is low, so be a kind of prescription of high comprehensive performance.Gas generating powder gas production rate of the present invention is big, the combustion temperature is low, the ignition delay phase is short, non-hygroscopic, residue filters easily.Suit simultaneously to have adopted continuously extruded kneading of twin screw to extrude on production technique, also the production technique that can adopt roll-in to extrude has in flakes solved in the compressing tablet production problem that gas generating powder production efficiency is low, production cost is high.Gas generating powder of the present invention can be used in automobile, the aircraft etc. the air bag generator with the protection passenger, also can be used for the producer gas generator of other type.
Embodiment
Further describe the present invention with embodiment below, help understanding, but described embodiment only is used to illustrate the present invention rather than restriction the present invention the present invention and advantage thereof, better effects if.
Comparative Examples
27.5% nitroguanidine, 33.0% basic copper nitrate, 2% guar gum, 37.5% deionized water add mixing machine and mixed 30 minutes for 70 degrees centigrade.After having mixed, material 80 degree insulation 8 hours removes moisture content by the mixing machine ventilating pit, makes that material is moisture to reach 15.5%.Subsequently, in the mixing machine whipping process, cool the temperature to 45 degree.Discharging then adds forcing machine at the 63Mpa compacted under with material, obtains the single hole tubular grain, and the powder column of extruding cuts into the single hole tubulose gas generator propellant powder column of Φ 2.4/0.7L4.0 through medicine cutter.Then earlier with powder column 30 degree predrys in baking oven, 80 degree are dried to the sample thermal weight loss and reach and obtain product below 0.3% again.
After testing, sensitivity is better, and 10kg drops hammer, and 25cm drop height, the impact sensitivity of 50mg dose are 12%, 3.92MPa, and 90 degree pivot angles, the friction sensitivity that the 20mg dose records is 0%.
Gas production rate 2.6mol/100g, heat-resistant quality is good, records 100 ℃ according to the GJB772A-1997 vacuum stability test, and 48 hours discharge quantity is 0.78ml/5g.Rate of moisture absorption 5%.Residue rate 21%.
Embodiment 1
The described gas-generating agent composition of present embodiment comprises 30% Guanidinium nitrate, 13% nitroguanidine, 4% Dyhard RU 100,34% basic copper nitrate, 3% ferric oxide, 6% cupric oxide, 5% SODIUMNITRATE, 1.5% ultra-fine high purity aluminium sesquioxide, 3.5% Xylo-Mucine.The median size 1.4 μ m of raw material, wherein aluminium sesquioxide purity is 99.99%, median size is 1.6 μ m.
Its course of processing is: earlier with above-mentioned raw materials respectively according to the difference of fuel, oxygenant, igniting modifying agent, binding agent performance, mix respectively, and then tentatively mix at vertical mixer, and adding distilled water mixes, water-content is controlled at 20%, be incubated under 40 ℃, soaking time is 6 hours.
Adopt the plunger tpe extruding then, the pressure of extruding is 8Mpa, and jacket temperature is about 40 ℃, adopt air-dry method to carry out expelling water, the water content of extrudate is reduced to about 10%, extrude diameter 30mm, the centre that is shaped as of moulding has some to reserve the cylinder of through holes, and length is about 25mm.
Establish a dicing machine up and down, medicine cutter at the end face of extrusion neck ring mold.This kind medicine cutter divides two portions up and down, last medicine cutter by travelling belt, pressure roller, cut chain cover, lead the chain cutting knife and wheel box is formed, following medicine cutter is made up of body, leakage batch pan, transmission shaft, the linear velocity of travelling belt is faster than extruded velocity.The medicinal strip of being sent here by travelling belt is cut into the medicine section of certain-length by last medicine cutter, and the medicine section enters in the hole of batch pan Lou along conduit, falls on the supporting cup of control length, is leaked the cutting knife cut-out that batch pan rotates below, falls into and connects the medicine funnel.
Enter the preliminary drying tower then, carry out two step drying treatment at last again in baking oven, predrying temperature is 55 ℃; The drying temperature in second step is dried to the sample thermal weight loss and reaches and obtain product below 0.3% at 110 ℃.
After testing, the gas production rate 2.8mol/100g of this gas-generating agent composition, wherein water vapor accounts for 49.12% (calculated value) of cumulative volume percentage composition, and the nitrogen volumn concentration is 34.60% (calculated value), and all the other are carbonic acid gas.
Sensitivity is better, and 10kg drops hammer, and 25cm drop height, the impact sensitivity of 50mg dose are 8%.3.92MPa, 90 degree pivot angles, the friction sensitivity that the 20mg dose records is 0%.
Heat-resistant quality is good, records 100 ℃ according to the GJB772A-1997 vacuum stability test, and 48 hours discharge quantity is 0.45ml/5g.Decomposition temperature is moderate, and the initial decomposition temperature that the DSC test records is 155 ℃.Rate of moisture absorption is low, and gas generating powder was deposited under 65% relative humidity 48 hours, and rate of moisture absorption is less than 1%.
Embodiment 2
The described gas-generating agent composition of present embodiment comprises 45% Guanidinium nitrate, 5% nitroguanidine, 3% pentaamino tetrazolium, 25% basic copper nitrate, 11% SODIUMNITRATE, 3% calcium perchlorate, 6% zinc oxide, 0.5% cupric chloride, 1.5% food grade guar gum.The median size 6 μ m of raw material.
Its course of processing is: earlier with above-mentioned raw materials respectively according to the difference of fuel, oxygenant, igniting modifying agent, binding agent performance, mix respectively, and then tentatively mix at the vertical helical mixing machine, and adding distilled water mixes, water-content is controlled at 30%, be incubated under 75 ℃, soaking time is 4.5 hours.
Adopt the twin screw extrusion moulding then, the pressure of extruding is 10Mpa, and jacket temperature is about 40 ℃, adopt vacuum pumping method to carry out expelling water, the water content of extrudate is reduced to about 10%, extruded diameter 3mm, the cylinder of quincunx through hole is arranged in the middle of being shaped as of moulding, and length is about 3mm.
Cut off through vertical cut formula dicing machine again.Carry out drying treatment then in baking oven, drying temperature is at 100 ℃, is dried to the sample thermal weight loss and reaches and obtain product below 0.4%.
After testing, the gas production rate 2.7mol/100g of this gas-generating agent composition, wherein water vapor accounts for 35% of cumulative volume percentage composition, and the nitrogen volumn concentration is 40.5% (calculated value), and all the other are carbonic acid gas.
Sensitivity is better, and 10kg drops hammer, and 25cm drop height, the impact sensitivity of 50mg dose are 4%.3.92MPa, 90 degree pivot angles, the friction sensitivity that the 20mg dose records is 0%.
Heat-resistant quality is good, records 100 ℃ according to the GJB772A-1997 vacuum stability test, and 48 hours discharge quantity is 0.39ml/5g.Decomposition temperature is moderate, and the initial decomposition temperature that the DSC test records is 160 ℃.Rate of moisture absorption is low, and gas generating powder was deposited under 65% relative humidity 48 hours, and rate of moisture absorption is less than 1%.
Embodiment 3
With embodiment 2, different is that the described gas-generating agent composition of present embodiment comprises 12% amino-guanidine nitrate, 18% ammonium oxalate, 10% pentaamino tetrazolium, 25% basic copper nitrate, 18% cupric oxide, 10% manganese oxide, 5% cupric chromate, 2% guar gum.The median size 20 μ m of raw material.
Preparation process is with embodiment 2.
Embodiment 4-9
| Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | ||
| Fuel | The guanidine class | 25% Guanidinium nitrate, 15% nitroguanidine | 13% Guanidinium nitrate, 19% Dyhard RU 100 | 28% Guanidinium carbonate, 15% nitroguanidine | 25% Guanidinium nitrate | 20% triamino Guanidinium nitrate | 5% nitroguanidine, 8% Dyhard RU 100 |
| Azole | 6% pentaamino tetrazolium | 8% pentaamino tetrazolium | 15% diazole Secondary ammonium phosphate salt | 17% tetramino triazole | 15% pentaamino terazole derivatives | 3% pentaamino tetrazolium | |
| Pyrrolotriazine derivatives | 9% oxamide | 7% hydrazo volatile salt | 8% 3 hydrazine triazine | 5% ammonium oxalate | 10% oxamide | 4% ammonium oxalate | |
| Oxygenant | Nitrate | 25% basic copper nitrate | 28% basic copper nitrate | 20% basic copper nitrate, 4% SODIUMNITRATE | 40% basic copper nitrate | 48% basic copper nitrate, 2% nitrate of baryta | 60% basic copper nitrate, 8% nitrocalcite |
| Metal oxide | 10% cupric oxide, 7% ferric oxide | 7% ferric oxide, 11% cupric oxide | 5% cupric oxide | 3% cupric oxide, 3% manganese oxide | 3.5% manganese oxide | 6.5% zinc oxide | |
| Perchlorate | 3% potassium perchlorate |
| The igniting modifying agent | 1% ultra-fine high purity aluminium sesquioxide | 4% cupric chromate | 2% aluminium sesquioxide | 1.5% ultra-fine high purity aluminium sesquioxide | 1% cupric chloride | 3.5% potassiumchromate |
| Caking agent | 2% Xylo-Mucine | 3% guar gum | 3% carboxymethyl cellulose | 2.5% guar gum | 0.5% guar gum | 2% carboxymethyl cellulose potassium |
The above is preferred embodiment of the present invention only, is not to be used for limiting scope of the invention process.So all doing according to described feature of the present patent application scope and spirit all is equivalent variations or modification, all should be included within the claim of the present invention.
Claims (10)
1. a gas-generating agent composition is characterized in that, comprises following component and content: 20～70% fuel, 25～75% oxygenants, 0.5～5% igniting modifying agent and 0.5～5% binding agent, content is weight percentage.
2. a kind of gas-generating agent composition according to claim 1 is characterized in that, comprises 30～60% fuel, 35～65% oxygenants, 1～3% igniting modifying agent and 0.5～5% binding agent, and content is weight percentage.
3. a kind of gas-generating agent composition according to claim 1 and 2 is characterized in that: described fuel is two or more the mixing in guanidine class, azole and derivative thereof, the pyrrolotriazine derivatives nitrogen-enriched compounds.
4. a kind of gas-generating agent composition according to claim 3, it is characterized in that: described guanidine class is Dyhard RU 100, nitroguanidine, Guanidinium nitrate and allied substances, be at least a kind of in the guanidine class material of introducing below, Dyhard RU 100, nitroguanidine, Guanidinium nitrate, Guanidinium carbonate, amino-guanidine nitrate, diamino Guanidinium nitrate, triamino Guanidinium nitrate or nitric acid nitre ammonia guanidine are good with nitroguanidine and dihydro-amine; Described azole is diazole, triazole, tetrazolium or its derivative, and terazole derivatives is pentaamino tetrazolium and allied substances, and oxadiazole derivative is diazole Secondary ammonium phosphate salt and allied substances, and triazole derivative is tetramino triazole and congener; Described pyrrolotriazine derivatives is oxamide, ammonium oxalate, three hydrazine triazines or hydrazo volatile salt and allied substances.
5. a kind of gas-generating agent composition according to claim 3, it is characterized in that: when fuel when being main with the guanidine compound of Guanidinium nitrate or nitroguanidine, selection is based on the gas-generating agent composition of Guanidinium nitrate, the content of Guanidinium nitrate is 20～50% of gross weight, is good with 30～45% weight percentage wherein; The amount of nitroguanidine and Dyhard RU 100 or pentaamino tetrazolium is good to be no more than 80% of Guanidinium nitrate.
6. a kind of gas-generating agent composition according to claim 1 is characterized in that: described oxygenant is one or more mixing in nitrate, metal oxide or the perchlorate; Described nitrate is base metal nitrate, alkine earth metal nitrate or subnitrate; Described metal oxide is the oxide compound of copper, iron, zinc or manganese; Described perchlorate is sodium perchlorate, lithium perchlorate, potassium perchlorate, cesium perchlorate, magnesium perchlorate, calcium perchlorate, perchloric acid strontium, barium perchlorate or ammoniumper chlorate.
7. a kind of gas-generating agent composition according to claim 6 is characterized in that: described oxygenant is main oxygenant with basic copper nitrate, and its weight percentage in total gas generating powder is 25～60%, and optimum is 35～50%; The content of SODIUMNITRATE is 10%～20% of basic copper nitrate, and optimum amount is 15%～17% of a basic copper nitrate; The content of ferric oxide and cupric oxide is the 5～80%, 30～45% the most suitable of basic copper nitrate, and the proportioning of ferric oxide and cupric oxide is 1: 0.5～1: 5, and optimum ratio is 1: 2.
8. a kind of gas-generating agent composition according to claim 1 and 2 is characterized in that: described igniting modifying agent is aluminium sesquioxide, cupric chloride, cupric chromate or potassiumchromate; Its content is 0.5～5% of gross weight, is the best with 1～3%; Be preferably ultra-fine high purity aluminium sesquioxide.
9. a kind of gas-generating agent composition according to claim 1 and 2 is characterized in that: described binding agent is water soluble cellulose, water soluble cellulose salt or guar gum, is preferably Xylo-Mucine or food grade guar gum.
10. method for preparing the described gas-generating agent composition of claim 1 is characterized in that: can be interrupted production, but also continuous production comprises the steps:
The first step is to mix, wherein comprise confusing between the same raw materials different-grain diameter, the part mixing of various fuel or oxygenant, comprise the preliminary mixing and the last abundant kneading when containing water medium of all raw material, blend temperature range is controlled at 30～80 ℃, optimum temperature is at 40～60 ℃, and soaking time is 4～6 hours; The amount of water medium distilled water is 15%～30% of a gas generating powder total amount;
Second step was moulding, was interrupted extruding of process using plunger tpe or roll-in, and continuous processing adopts the twin screw extrusion moulding, and the moulding jacket temperature is at 40～60 ℃, and extrusion pressure is advisable to be no more than 10MPa, and the water content of extrudate is reduced to and carried out pelletizing below 10%;
The 3rd step was dry, in baking oven or various pan dryer, divide a step, two steps or more multistep carry out drying, the water content that is dried to gas-generating agent composition is less than 0.5%.
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