CN109438150B - Automatic ignition medicament composition, preparation method, application and gas generator - Google Patents
Automatic ignition medicament composition, preparation method, application and gas generator Download PDFInfo
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- CN109438150B CN109438150B CN201811457864.0A CN201811457864A CN109438150B CN 109438150 B CN109438150 B CN 109438150B CN 201811457864 A CN201811457864 A CN 201811457864A CN 109438150 B CN109438150 B CN 109438150B
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06C—DETONATING OR PRIMING DEVICES; FUSES; CHEMICAL LIGHTERS; PYROPHORIC COMPOSITIONS
- C06C15/00—Pyrophoric compositions; Flints
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60R—VEHICLES, VEHICLE FITTINGS, OR VEHICLE PARTS, NOT OTHERWISE PROVIDED FOR
- B60R21/00—Arrangements or fittings on vehicles for protecting or preventing injuries to occupants or pedestrians in case of accidents or other traffic risks
- B60R21/02—Occupant safety arrangements or fittings, e.g. crash pads
- B60R21/16—Inflatable occupant restraints or confinements designed to inflate upon impact or impending impact, e.g. air bags
- B60R21/26—Inflatable occupant restraints or confinements designed to inflate upon impact or impending impact, e.g. air bags characterised by the inflation fluid source or means to control inflation fluid flow
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
- C06B31/02—Compositions containing an inorganic nitrogen-oxygen salt the salt being an alkali metal or an alkaline earth metal nitrate
- C06B31/12—Compositions containing an inorganic nitrogen-oxygen salt the salt being an alkali metal or an alkaline earth metal nitrate with a nitrated organic compound
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60R—VEHICLES, VEHICLE FITTINGS, OR VEHICLE PARTS, NOT OTHERWISE PROVIDED FOR
- B60R21/00—Arrangements or fittings on vehicles for protecting or preventing injuries to occupants or pedestrians in case of accidents or other traffic risks
- B60R21/02—Occupant safety arrangements or fittings, e.g. crash pads
- B60R21/16—Inflatable occupant restraints or confinements designed to inflate upon impact or impending impact, e.g. air bags
- B60R21/26—Inflatable occupant restraints or confinements designed to inflate upon impact or impending impact, e.g. air bags characterised by the inflation fluid source or means to control inflation fluid flow
- B60R2021/26064—Inflatable occupant restraints or confinements designed to inflate upon impact or impending impact, e.g. air bags characterised by the inflation fluid source or means to control inflation fluid flow characterised by auto-ignition means
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- Air Bags (AREA)
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Abstract
Hair brushThe invention relates to an automatic ignition medicament composition, a preparation method and application thereof, wherein the automatic ignition medicament composition comprises the following components in percentage by mass: NTO (3-nitro-1, 2, 4-triazole-5-ketone) 45-65%; sodium nitrate (NaNO)3)25 to 45 percent; 4.5 to 15.5 percent of guanidine nitrate; 0.1 to 10 percent of graphite; according to the automatic ignition powder provided by the invention, guanidine nitrate is subjected to wet mixing granulation by adopting a specific preparation process and then is mixed with NTO, sodium nitrate and graphite to prepare the automatic ignition powder with excellent performance, the automatic ignition powder composition has good long heat storage stability, is suitable for the long-time service life of an automobile, can realize instant ignition of the automatic ignition powder, realizes reliable ignition, remarkably improves the ignition performance, and meets the requirements of an air bag for protecting drivers and passengers.
Description
Technical Field
The invention relates to an automatic ignition medicament composition, a preparation method and application thereof, in particular to an automatic ignition medicament composition with decomposition temperature and explosion point lower than that of gas-producing medicaments and a preparation method thereof, belonging to the technical field of automobile safety airbag gas generators.
Background
As is well known, with the development of highways and the improvement of automobile performance, automobiles are driven at higher and higher speeds, so that traffic accidents of the automobiles are more frequent, and an airbag system which is an important component of passive safety of the automobiles is particularly important. A very important component of an airbag system is a gas generator, which functions to generate a sufficient volume of gas to supply the airbag at a sufficiently fast rate and in a short time. Automotive airbags are one or more inflators installed within the passenger or seat area of an automobile and within the interior trim of an automobile to protect critical areas of the driver and passengers from impact and to mitigate injuries from impacts. The safety air bag system consists of a sensor, a controller, a gas generator, an air bag and the like.
The automobile safety air bag has the following action principle: when the automobile is collided, firstly, the sensor receives the impact signal, the signal is transmitted to the central control unit, and after the signal is calculated by the computer of the central control unit, the computer outputs an electric signal as long as the specified threshold value is reached. The electric igniter in the gas generator is detonated and ignites the gas-generating agent after receiving the starting signal to generate a large amount of gas, the gas enters the air bag after being filtered and cooled, so that the air bag breaks through the cover cap to expand and unfold quickly in a very short time, and a buffer air cushion is formed between a driver or a passenger and the automotive interior, thereby effectively protecting the head and the chest of a human body and preventing the head and the chest from being injured or reducing the injury degree. However, under the condition of a sudden temperature rise caused by an external high-temperature environment, the pyrotechnic material of the gas generator is abnormally combusted, the strength of the shell is reduced, violent reaction and even explosion can occur, and the shell fragments are ejected, so that greater danger is brought to drivers and passengers. In order to avoid this and ensure the safety, materials with an auto-ignition function are newly added, which can be automatically ignited according to the rise of the ambient temperature without the assistance of a mechanical or electronic ignition device, namely, without starting a gas generator squib, so as to detonate the gas generator, remove the pyrotechnic materials in the gas generator and relieve the danger. Therefore, the decomposition temperature of the autoignition charge is lower than that of the gas generant charge and the ignition charge.
The life of an automobile is generally 10 to 15 years, and a pyrotechnic charge applied to an automobile airbag inflator should maintain stable performance during the time, and an automatic ignition charge should have a long life as one of pyrotechnic charges in the inflator.
At present, the automatic ignition powder on the market is mainly 5-aminotetrazole or nitroguanidine, basic copper nitrate, nitrate or chlorate is mainly used as an oxidant, or nitrocotton medicaments are directly used. Because 5-aminotetrazole medicaments are poor in thermal stability and easy to absorb moisture, and nitroguanidine, nitrocotton, chlorate and other raw materials are sensitive, wherein the nitrocotton has the greatest defect of poor thermal stability and complete decomposition in extreme cases. Therefore, this type of autoignition powder has a large risk factor in the production process and poor long-term storage stability.
Therefore, it is necessary to optimize the automatic ignition charge in the airbag inflator, which not only effectively protects the life safety of the passengers in traffic accidents, but also reduces the huge loss of the automobile manufacturers due to the abnormal ignition of the inflator.
For example, US6453816B2 contains mainly explosive such as calcium-bitetrazole-amine, NTO, 5-aminotetrazole, nitrate, nitroguanidine and bitetrazole amine, oxidant such as zinc peroxide, ammonium nitrate, potassium nitrate, strontium nitrate, potassium perchlorate and the like, and reductant such as titanium powder. The patent uses dry granulation and uses extrusion for tablet production and granulation production, with certain risks in the process handling, especially during the tabletting and granulation processes, and in addition the patent does not perform a very good film release. Therefore, several common autoignition agents for the airbag inflator have defects.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides an automatic ignition agent composition and a preparation method thereof, wherein the automatic ignition agent composition has good long heat storage stability and is suitable for the long-time service life of an automobile, namely, the automatic ignition agent composition can realize instant ignition, realizes reliable ignition, obviously improves the ignition performance and meets the requirements of an air bag for protecting a driver and passengers.
It is another object of the present invention to provide a use of the autoignition composition.
It is a further object of the present invention to provide an automotive airbag inflator.
The above purpose of the invention is mainly realized by the following technical scheme:
an automatic ignition medicament composition comprises the following components in percentage by mass:
the automatic ignition medicament composition comprises the following components in percentage by mass:
in the above automatic ignition agent composition, the particle size D90 of guanidine nitrate is not more than 20 μm.
In the above automatic ignition agent composition, the particle diameter D90 of the graphite is not more than 15 μm.
In the above automatic ignition agent composition, the sodium nitrate is finely ground by a vibration mill, and 60 mesh screen underflow is taken.
In the above automatic ignition charge composition, the sum of the water contents of the components of the automatic ignition charge composition is not more than 1% of the total mass of the components.
In the above automatic ignition agent composition, the mixture of the components is formed into particles having a water content of less than 0.5% before compression molding.
In the automatic ignition medicament composition, the automatic ignition medicament composition is of a circular sheet structure, and the diameter of the circular sheet structure is 3-15 mm; the thickness of the circular sheet structure is 1-5 mm; the mass of each round sheet-like structure is 0.01-2 g.
In the automatic ignition agent composition, the ignition agent composition is of a granular structure, and the grain diameter is 8-20 meshes.
In the above automatic ignition pharmaceutical composition, the guanidine nitrate is a material obtained by wet granulating a raw material guanidine nitrate, or a material obtained by wet granulating, drying, tabletting and granulating a raw material guanidine nitrate.
In the above automatic ignition agent composition, the guanidine nitrate is obtained from a raw material guanidine nitrate by a treatment method comprising:
(1) adding water into the raw material guanidine nitrate for wet mixing, wherein the water adding amount is 3% -12% of the total mass of the guanidine nitrate, and mixing to obtain a first material;
(2) granulating the first material through a 20-mesh screen to obtain a second material;
(3) and drying the second material until the water content is less than 0.5 percent of the total mass of the second material, and taking the materials below a 20-mesh screen and above a 100-mesh screen to obtain the needed guanidine nitrate.
In the above-mentioned automatic ignition charge composition, in use, the automatic ignition charge composition is mixed with an ignition charge and a gas generant charge together or used alone; or the autoignition charge composition may be separately placed in a heat sensitive region of the inflator housing to ensure reliable triggering of the autoignition charge upon external heating.
A preparation method of an automatic ignition medicament composition adopts a wet granulation mode to prepare the automatic ignition medicament composition.
A preparation method of an automatic ignition medicament composition specifically comprises the following steps:
(1) mixing 3-nitro-1, 2, 4-triazole-5-ketone, sodium nitrate, guanidine nitrate and graphite to obtain a first material;
(2) adding water into the first material for wet mixing to obtain a second material, wherein the water adding amount is 3-15% of the total mass of the first material;
(3) passing the second material through a screen with 10-40 meshes to obtain a third material;
(4) drying the third material until the water content is less than 0.5 percent of the total mass of the third material, and passing through a screen with 10-40 meshes again to obtain a fourth material;
(5) and carrying out material molding on the fourth material.
In the above method for preparing an automatic ignition agent composition, the guanidine nitrate used in the step (1) is obtained from a raw material guanidine nitrate by a treatment method comprising:
(1) adding water into the raw material guanidine nitrate for wet mixing, wherein the water adding amount is 3% -12% of the total mass of the guanidine nitrate, and mixing to obtain a first material;
(2) granulating the first material through a 20-mesh screen to obtain a second material;
(3) and drying the second material until the water content is less than 0.5 percent of the total mass of the second material, and taking the materials below a 20-mesh screen and above a 100-mesh screen to obtain the needed guanidine nitrate.
In the preparation method of the automatic ignition medicament composition, in the step (1), the 3-nitro-1, 2, 4-triazole-5-one, the sodium nitrate, the guanidine nitrate and the graphite are mixed in a mixing device to obtain a first material, and the mixing time is less than or equal to 40 min; the mixing device is a multi-motion mixer or an acoustic resonance mixer.
In the above method for preparing the automatic ignition agent composition, the time for wet mixing in the step (2) is 2min to 15 min; the wet mixing equipment is a kneader or a mixer.
In the above method for preparing the self-igniting pharmaceutical composition, the fourth material is molded by a rotary tablet press in the step (5).
In the preparation method of the automatic ignition medicament composition, the material in the step (5) is molded to obtain a circular sheet structure, and the diameter of the circular sheet structure is 3-15 mm; the thickness of the circular sheet structure is 1-5 mm; the mass of each round sheet-like structure is 0.01-2 g.
In the preparation method of the automatic ignition medicament composition, the material in the step (5) is molded to obtain a granular structure, and the grain diameter of the granular structure is 8-20 meshes; the granular structure is obtained by sieving after the flake structure is granulated.
An automatic ignition medicament composition is prepared by the preparation method.
The application of an automatic ignition medicament composition is provided, and the automatic ignition medicament composition is used for an automobile safety airbag gas generator.
The gas generator for the automobile safety airbag adopts the automatic ignition medicament composition as an automatic ignition medicament.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides a preparation method of a compound containing NTO (3-nitro-1, 2, 4-triazole-5-ketone) and sodium nitrate (NaNO)3) The novel automatic ignition medicament composition comprises guanidine nitrate and graphite, has low decomposition temperature of 150-180 ℃, is lower than the gas generating agent of the safety airbag, ensures the reliable ignition of the automatic ignition medicament during working, has good long heat storage stability, and is suitable for the long-time service life of automobiles.
(2) The invention relates to a composition for an ignition medicament, which comprises NTO (3-nitro-1, 2, 4-triazole-5-ketone) and sodium nitrate (NaNO)3) The automatic ignition medicament composition has excellent performance and obvious effect, and the automatic ignition medicament composition ignites violently and instantly when igniting a gas generating agent, thereby remarkably improving the ignition performance.
(3) The automatic ignition medicament composition provided by the invention contains graphite as a process aid, and through the research on the proportion of the graphite in the formula and the addition process, the graphite can be weighed and mixed with other components, and can also be added before compression, so that the composition tablet does not stick to a die in the tablet compression process, and the tablet can well keep the original luster and form after compression, has no pits on the surface and no burrs
(4) The automatic ignition medicament composition provided by the invention adopts a wet pressing process, guanidine nitrate is subjected to wet mixing granulation or guanidine nitrate is subjected to wet mixing granulation and granulation firstly, and then is subjected to wet mixing granulation and pressing with other components, so that the problem of difficulty of automatic ignition medicament is solved, the automatic ignition medicament can be instantly ignited, reliable ignition is realized, the ignition performance is obviously improved, and the requirements of safety airbags for protecting drivers and passengers are met.
(5) The automatic ignition medicament composition provided by the invention adopts a wet granulation and reshaping method, and has the advantages of good safety, less accident potential, stable pressing process, capability of meeting the requirements of modern production on similar ignition medicaments and good ignition performance.
(6) Before the ignition medicament composition is formed, the ignition medicament composition is granulated by a wet granulation method, so that the process is simpler, the cost is lower, the energy consumption is low, the process is more flexible, and the equipment investment is low.
(7) A large number of tests show that the automatic ignition powder composition can reliably ignite the gas generating agent; the decomposition temperature of the ignition powder composition is about 155 ℃, and the detonation heat of the ignition powder composition is 3436.4J/g; the test pressure of the friction sensitivity of the composition is 1.75MPa, the test angle is 75 degrees, the explosion percentage is 0 percent, the impact sensitivity is 68 percent under the test conditions of 98N drop hammer and 10cm drop height, the explosion percentage of the test medicament is 68 percent, and the static sensitivity V is50Is 7683V, E50345mJ, which belongs to a low-sensitivity medicine.
(8) The automatic ignition powder has flexible use mode, can be mixed with the ignition powder and the gas production powder together, or separated from the ignition powder and the gas production powder, or is independently placed in a heat sensitive area of a gas generator shell, so that the automatic ignition powder is reliably triggered under the condition of external heating, and the controlled ignition of the gas production powder is ensured.
Drawings
FIG. 1 is a surface morphology of an autoignition tablet in comparative example 1 of the present invention;
FIG. 2 is a surface morphology of an autoignition tablet in example 1 of the present invention;
FIG. 3 is a graph showing the external pressure comparison before and after the thermal aging of the autoignition charge in example 3 in accordance with the present invention;
FIG. 4 is an average curve of external pressure before and after thermal aging of an autoignition charge in example 3 in accordance with the present invention;
FIG. 5 shows the experimental placement of the generators of examples 1 to 3 of the present invention;
FIG. 6 shows the temperature measurement positions of the generators in examples 1 to 3 of the present invention;
FIG. 7 is a comparison of the generators before and after the forward test of the slow heat/auto-ignition test in example 3 of the present invention;
FIG. 8 is a comparison of the generators before and after the reverse test of the slow heat/auto-ignition test in example 3 of the present invention;
FIG. 9 is a comparison of the generators before and after the slow heat/auto-ignition test side test in example 3 of the invention.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
the automatic ignition medicament composition comprises the following components in percentage by mass:
in the self-ignition medicinal composition, the following components are preferably used in percentage by mass: NTO (3-nitro-1, 2, 4-triazole-5-ketone) 50% -60%; 30-40% of sodium nitrate (NaNO 3); 5 to 15 percent of guanidine nitrate; 0.1 to 5 percent of graphite.
The particle size D90 of the guanidine nitrate raw material is not more than 20 μm; the guanidine nitrate is a material obtained by performing wet granulation on a raw material guanidine nitrate, and can also be a material obtained by performing wet granulation, drying, tabletting and granulation on the raw material guanidine nitrate; the particle size D90 of the graphite is not more than 15 μm; the sodium nitrate is obtained by grinding through a vibration mill and taking 60-mesh screen underflow;
the sum of the water contents of the components of the autoignition medicament composition is not more than 1 percent of the total mass of the components.
The above mixture of components is made into particles with water content less than 0.5% before compression molding.
The automatic ignition medicament composition can be in a circular sheet structure, and the diameter of the circular sheet structure is 3-15 mm; the thickness of the circular sheet structure is 1-5 mm; the mass of each round sheet-like structure is 0.01-2 g.
The self-igniting chemical composition may have a granular structure and a particle size of 8 to 20 mesh.
The invention adopts a wet granulation mode to prepare the automatic ignition medicament composition, and the specific preparation method comprises the following steps:
(1) mixing NTO (3-nitro-1, 2, 4-triazole-5-ketone) and sodium nitrate (NaNO)3) Mixing guanidine nitrate and graphite to obtain a first material; the first material can be obtained by mixing in a mixing device, and the mixing time is less than or equal to 40 min; the mixing device may employ a multiple motion mixer or an acoustic resonance mixer.
(2) Adding water into the first material for wet mixing to obtain a second material, wherein the water adding amount is 3-15% of the total mass of the first material; the time of wet mixing is 2min to 15 min; the wet mixing equipment is a kneader or a mixer.
(3) Passing the second material through a screen with 10-40 meshes to obtain a third material;
(4) drying the third material until the water content is less than 0.5% of the total mass of the third material, and passing through a 10-40-mesh screen again to obtain a fourth material;
(5) and forming the fourth material by a rotary tablet press.
The guanidine nitrate adopted in the step (1) is obtained from a raw material guanidine nitrate by the following treatment method:
(a) adding water into the raw material guanidine nitrate for wet mixing, wherein the water adding amount is 3% -12% of the total mass of the guanidine nitrate, and mixing to obtain a first material;
(b) and granulating the first material through a 20-mesh screen to obtain a second material. Alternatively, the first material may be granulated by passing through a 20-mesh sieve, and the second material may be obtained by taking the material below the 20-mesh sieve and above the 100-mesh sieve.
(c) And drying the second material until the water content is less than 0.5 percent of the total mass of the second material, and taking the materials below a 20-mesh screen and above a 100-mesh screen to obtain the needed guanidine nitrate.
Forming the material in the step (5) to obtain a circular sheet structure or a granular structure, wherein the diameter of the circular sheet structure is 3-15 mm; the thickness of the circular sheet structure is 1-5 mm; the mass of each round sheet-like structure is 0.01-2 g. Or obtaining a granular structure, wherein the grain diameter of the granular structure is 12-20 meshes; the granular structure is obtained by granulating and sieving a flaky structure.
The automatic ignition medicament composition prepared by the invention is mainly used for an automobile safety airbag gas generator.
The invention also provides a gas generator which uses the automatic ignition medicament composition with reliable ignition performance as an automatic ignition medicament.
The automatic ignition powder of the invention is placed in two modes: one is to mix the autoignition charge with the ignition charge and the gas generant charge or separate from the ignition charge and the gas generant charge, and the other is to place the autoignition charge in a thermally sensitive region of the gasifier shell to ensure reliable triggering of the autoignition charge upon external heating, thereby ensuring controlled ignition of the gas generant charge.
Comparative example 1 (without deinking agent C)
The automatic ignition medicament composition comprises the following components in percentage by mass:
54% of NTO (3-nitro-1, 2, 4-triazole-5-ketone);
sodium nitrate (NaNO)3) 34％；
12% of guanidine nitrate;
the components are weighed and then pressed into round pieces with the diameter of 5mm and the thickness of 2.4-2.9 mm by a wet granulation and rotary tablet press. The preparation method comprises the following steps: mixing NTO (3-nitro-1, 2, 4-triazole-5-ketone) and sodium nitrate (NaNO)3) Mixing guanidine nitrate by a ribbon mixer to obtain a first material; adding 10 percent (mass percentage content) of distilled water into the first material, carrying out wet kneading for 5min to obtain a second material, and passing the second material through a 10-mesh screen to obtain a third material; drying the third material until the water content is less than 0.5 percent of the total mass of the third material, and passing through a 20-mesh screen again to obtain a fourth material; will be firstAnd forming the materials by a rotary tablet press to obtain the circular sheet structure.
As shown in figure 1, the self-igniting powder without deinking agent has sticking mold on the surface of the tablet, which can not well maintain the original luster and shape, and pits and burrs on the surface.
Example 1
The automatic ignition medicament composition comprises the following components in percentage by mass:
the components are weighed and then pressed into round pieces with the diameter of 5mm and the thickness of 2.3-2.9 mm by a wet granulation and rotary tablet press. The preparation method comprises the following steps: mixing NTO (3-nitro-1, 2, 4-triazole-5-ketone) and sodium nitrate (NaNO)3) Mixing guanidine nitrate and graphite through a ribbon mixer to obtain a first material; adding 10 percent (mass percentage content) of distilled water into the first material, carrying out wet kneading for 5min to obtain a second material, and passing the second material through a 10-mesh screen to obtain a third material; drying the third material until the water content is less than 0.5 percent of the total mass of the third material, and passing through a 20-mesh screen again to obtain a fourth material; and (5) carrying out material forming on the fourth material through a rotary tablet press to obtain a circular sheet structure.
FIG. 2 is a surface morphology of a tablet of the autoignition dose composition in accordance with example 1 of the present invention; in the comparative example, graphite is added as a mold release agent, so that the surface of the tablet is not adhered to a mold, the tablet can well keep the original luster and form, and the surface of the tablet is free from pits and burrs.
Example 2
The automatic ignition medicament composition comprises the following components in percentage by mass:
the components are weighed and pressed into straight pieces by a wet granulation and rotary tablet pressA wafer with the diameter of 8mm and the thickness of 2.4-2.6 mm. The preparation method comprises the following steps: mixing NTO (3-nitro-1, 2, 4-triazole-5-ketone) and sodium nitrate (NaNO)3) Mixing guanidine nitrate and graphite through a ribbon mixer to obtain a first material; adding 8 percent (mass percentage content) of distilled water into the first material, carrying out wet kneading for 8min to obtain a second material, and passing the second material through a 10-mesh screen to obtain a third material; drying the third material until the water content is less than 0.5 percent of the total mass of the third material, and passing through a 20-mesh screen again to obtain a fourth material; and (5) carrying out material forming on the fourth material through a rotary tablet press to obtain a circular sheet structure.
Example 3
The automatic ignition medicament composition comprises the following components in percentage by mass:
the components are weighed and then pressed into round pieces with the diameter of 6.4mm and the thickness of 3.4-3.8 mm by a wet granulation and rotary tablet press. The preparation method comprises the following steps: mixing NTO (3-nitro-1, 2, 4-triazole-5-ketone) and sodium nitrate (NaNO)3) Mixing guanidine nitrate and graphite through a ribbon mixer to obtain a first material; adding 5 percent (mass percentage content) of distilled water into the first material, carrying out wet kneading for 10min to obtain a second material, and passing the second material through a 10-mesh screen to obtain a third material; drying the third material until the water content is less than 0.5 percent of the total mass of the third material, and passing through a 20-mesh screen again to obtain a fourth material; and (5) carrying out material forming on the fourth material through a rotary tablet press to obtain a circular sheet structure.
The autoignition agents prepared in examples 1 to 3 were subjected to a performance test:
(1) burst heat test
Testing an instrument: the vacuum bomb precision temperature-regulating type automatic calorimeter RF-C7000(TJ) Z.
And (3) testing conditions are as follows: under vacuum, the sample amount was 4 g/time, and the measurement was performed in parallel twice.
And (4) testing standard: according to the constant temperature method of the composite solid propellant detonation heat test method, which is standard QJ 1359-88 of Ministry of industry of aerospace of the people's republic of China. The results are shown in Table 1.
Table 1 table of the properties of the autoignition charge in examples 1 to 3 of the present invention
The autoignition powder prepared in examples 1 to 3 was analyzed for detonation heat testing.
(2) Automatic ignition charge DSC-TG characterization
Thermal stability analysis was performed on the autoignition agents of examples 1 to 3
Testing an instrument: german Steed resistant STA449F3 super high temperature synchronous thermal analyzer,
according to the standard: standard number Q/G4A-2002 thermal decomposition temperature test method for composite solid propellant at institute of fourth institute of aerospace science and technology group
And (3) testing conditions are as follows: temperature range: -150 ℃ to +700 ℃; the heating rate is 10 ℃/min, the atmosphere is N2, and the flow rate of N2 is 60 ml/min; the initial decomposition temperature and exothermic decomposition peak temperature of the auto-ignition powder at a temperature rise rate of 10 ℃/min were tested.
DSC-TG test analysis was performed for the automatic ignition agents of examples 1 to 3.
The test records are shown in table 1 above.
(3) High temperature long term storage stability test of autoignition powder
According to the standard: USCAR
The test method comprises the following steps: the automatic ignition powder is placed at the temperature of 107 ℃ for 408 hours, the DSC-TG and the weight of the powder are tested before and after the experiment, and the DSC-TG and the weight loss of the powder after long-time high-temperature aging are analyzed to measure the long heat storage stability of the powder. The test results are shown in table 1 above.
The autoignition agents of examples 1 to 3 were analyzed for high temperature long term storage stability test.
(4) According to the standard: USCAR 5.2.4.5 Slow heating/auto-ignition test
Testing equipment: transformer, electric heater, temperature display, test barrel, thermocouple and stopwatch
The test method comprises the following steps:
the test placement position and the temperature measurement position include forward, reverse, and lateral.
FIG. 5 is a schematic diagram showing the experimental placement positions of the generators in examples 1 to 3 of the present invention; wherein fig. 5a, 5b, 5c are respectively the forward, reverse and lateral directions of the trial placement position.
FIG. 6 is a diagram showing the measurement positions of the temperature of the generator in examples 1 to 3 of the present invention. Wherein fig. 6a, 6b, 6c are respectively the forward, reverse and lateral directions of the temperature measurement position.
The slow heat/auto-ignition test analysis was performed on the auto-ignition charge example 3.
As can be seen from the results in Table 2, the generator has a complete structure after the test, and meets the requirements of the USCAR 5.2.4.5 slow heating/auto-ignition test.
Table 2 USCAR 5.2.4.5 slow heating/auto-ignition test table in example 3 of the invention
Fig. 7 is a graph comparing the generators after the forward test of the slow heating/auto-ignition test in example 3 of the present invention, wherein fig. 7a is a front view of the generators after the test, and fig. 7b is a back view of the generators after the test.
Fig. 8 is a comparative graph of a slow heat/auto-ignition test reverse test generator of example 3 of the present invention, wherein fig. 8a is a front view of the test generator and fig. 8b is a back view of the test generator.
Fig. 9 is a comparison of the slow heat/auto-ignition test side test generator of example 3 of the present invention, wherein fig. 9a is a front view and fig. 9b is a back view of the test generator.
(5) Comparison of external pressure Performance before and after thermal aging of Generator
According to the standard: USCAR
Testing equipment: tank (60L pressure vessel)
And (3) testing conditions are as follows: the heat aging temperature is 107 ℃, the total time is 408h (17 days),
the test method comprises the following steps: the autoignition powder of example 3 was charged into a generator equipped with 18 ignition powder and gas generant powder in total, 9 were subjected to conventional tests, and 9 generators were placed in an oil bath oven and subjected to thermal cycling at 107 ℃ for 408 hours, after which the generator was subjected to normal temperature (23 ℃), high temperature (85 ℃) and low temperature (-40 ℃) and subjected to 3-shot heat preservation for 4 hours, respectively, and then subjected to Tank test.
FIG. 3 is a graph showing the external pressure before and after heat aging; FIG. 4 shows the average curve of external pressure before and after heat aging.
From the curve, the gas generator filled with the automatic ignition powder of the invention meets the requirements of all properties outside the generator after 408 hours at the temperature of 107 ℃, and the external pressure performance is equivalent before and after thermal aging.
As can be seen from the test results shown in tables 1 and 2, the automatic ignition powder provided by the invention has the advantages that the initial decomposition temperature is lower and is 150-180 ℃, the heat release amount is large, the long-term storage thermal stability is good, the total time is 408 hours at 107 ℃, the DSC-TG data is equivalent to the data before aging, the weight loss is reduced by less than 2%, the automatic ignition powder is suitable for being used in a gas generator, the basic thermal temperature qualitative is ensured, the gas explosion danger can not be randomly ignited at the lower temperature, the gas generator can be automatically ignited when the external environment temperature is abnormally increased, the explosion danger of the gas generator at the high temperature is avoided, the long-term storage thermal stability is better, and the automatic ignition powder is suitable for the long-term service life of an automobile.
The above description is only for the best mode of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Those skilled in the art will appreciate that the invention may be practiced without these specific details.
Claims (22)
1. An auto-ignition charge composition characterized by: comprises the following components in percentage by mass:
the guanidine nitrate is a material obtained by carrying out wet granulation on a raw material guanidine nitrate, and the material below a 20-mesh screen and above a 100-mesh screen are taken; or the guanidine nitrate is subjected to wet granulation, drying, tabletting and granulation to obtain a material, and the material below a 20-mesh screen and the material above a 100-mesh screen are taken.
2. The auto-ignition charge composition of claim 1, wherein: comprises the following components in percentage by mass:
3. the automatic ignition agent composition according to claim 1 or 2, wherein: the particle size D90 of the raw material guanidine nitrate is not more than 20 mu m.
4. The automatic ignition agent composition according to claim 1 or 2, wherein: the particle size D90 of the graphite is not more than 15 μm.
5. The automatic ignition agent composition according to claim 1 or 2, wherein: the sodium nitrate is ground by a vibration mill, and 60-mesh screen underflow is taken.
6. The automatic ignition agent composition according to claim 1 or 2, wherein: the sum of the water contents of the components of the automatic ignition medicament composition is not more than 1 percent of the total mass of the components.
7. The automatic ignition agent composition according to claim 1 or 2, wherein: the mixture of the components is made into particles with water content less than 0.5% before compression molding.
8. The automatic ignition agent composition according to claim 1 or 2, wherein: the automatic ignition medicament composition is of a circular sheet structure, and the diameter of the circular sheet structure is 3-15 mm; the thickness of the circular sheet structure is 1-5 mm; the mass of each round sheet-like structure is 0.01-2 g.
9. The automatic ignition agent composition according to claim 1 or 2, wherein: the ignition medicament composition is of a granular structure, and the grain diameter is 8-20 meshes.
10. The auto-ignition charge composition of claim 1, wherein: the guanidine nitrate is obtained from a raw material guanidine nitrate by the following treatment method:
(1) adding water into the raw material guanidine nitrate for wet mixing, wherein the water adding amount is 3% -12% of the total mass of the guanidine nitrate, and mixing to obtain a first material;
(2) granulating the first material through a 20-mesh screen to obtain a second material;
(3) and drying the second material until the water content is less than 0.5 percent of the total mass of the second material, and taking the materials below a 20-mesh screen and above a 100-mesh screen to obtain the needed guanidine nitrate.
11. The automatic ignition agent composition according to claim 1 or 2, wherein: when in use, the automatic ignition medicament composition is mixed with the ignition powder and the gas generating powder or is used independently; or the autoignition charge composition may be separately placed in a heat sensitive region of the inflator housing to ensure reliable triggering of the autoignition charge upon external heating.
12. The method for preparing an autoignition primer composition according to claim 1 or 2, wherein: the automatic ignition medicament composition is prepared by adopting a wet granulation mode.
13. The method of preparing an autoignition primer composition according to claim 12, wherein: the method specifically comprises the following steps:
(1) mixing 3-nitro-1, 2, 4-triazole-5-ketone, sodium nitrate, guanidine nitrate and graphite to obtain a first material;
(2) adding water into the first material for wet mixing to obtain a second material, wherein the water adding amount is 3-15% of the total mass of the first material;
(3) passing the second material through a screen with 10-40 meshes to obtain a third material;
(4) drying the third material until the water content is less than 0.5 percent of the total mass of the third material, and passing through a screen with 10-40 meshes again to obtain a fourth material;
(5) and carrying out material molding on the fourth material.
14. The method of preparing an autoignition primer composition according to claim 13, wherein: the guanidine nitrate adopted in the step (1) is obtained from a raw material guanidine nitrate by the following treatment method:
(1) adding water into the raw material guanidine nitrate for wet mixing, wherein the water adding amount is 3% -12% of the total mass of the guanidine nitrate, and mixing to obtain a first material;
(2) granulating the first material through a 20-mesh screen to obtain a second material;
(3) and drying the second material until the water content is less than 0.5 percent of the total mass of the second material, and taking the materials below a 20-mesh screen and above a 100-mesh screen to obtain the needed guanidine nitrate.
15. The method of preparing an autoignition primer composition according to claim 13, wherein: in the step (1), 3-nitro-1, 2, 4-triazole-5-ketone, sodium nitrate, guanidine nitrate and graphite are mixed in a mixing device to obtain a first material, wherein the mixing time is less than or equal to 40 min; the mixing device is a multi-motion mixer or an acoustic resonance mixer.
16. The method of preparing an autoignition primer composition according to claim 13, wherein: the time for wet mixing in the step (2) is 2-15 min; the wet mixing equipment is a kneader or a mixer.
17. The method of preparing an autoignition primer composition according to claim 13, wherein: and (5) molding the fourth material by a rotary tablet press.
18. The method of preparing an autoignition primer composition according to claim 13, wherein: forming the material in the step (5) to obtain a circular sheet structure, wherein the diameter of the circular sheet structure is 3-15 mm; the thickness of the circular sheet structure is 1-5 mm; the mass of each round sheet-like structure is 0.01-2 g.
19. The method of preparing an autoignition primer composition according to claim 13, wherein: the material in the step (5) is molded to obtain a granular structure, and the particle size of the granular structure is 8-20 meshes; the granular structure is obtained by sieving after the flake structure is granulated.
20. An auto-ignition charge composition characterized by: the preparation method of any one of claims 12 to 19.
21. Use of the self-igniting pharmaceutical composition according to any one of claims 1 to 11, wherein: the automatic ignition medicament composition is used for an automobile safety airbag gas generator.
22. Automobile air bag gas generator, its characterized in that: the use of the self-igniting pharmaceutical composition according to any one of claims 1 to 11.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811457864.0A CN109438150B (en) | 2018-11-30 | 2018-11-30 | Automatic ignition medicament composition, preparation method, application and gas generator |
| PCT/CN2019/091614 WO2020107869A1 (en) | 2018-11-30 | 2019-06-18 | Automatic ignition agent composition, preparation method, application and gas generator |
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| CN201811457864.0A CN109438150B (en) | 2018-11-30 | 2018-11-30 | Automatic ignition medicament composition, preparation method, application and gas generator |
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| CN109438150B (en) * | 2018-11-30 | 2021-07-13 | 湖北航鹏化学动力科技有限责任公司 | Automatic ignition medicament composition, preparation method, application and gas generator |
| CN109733557A (en) * | 2019-03-18 | 2019-05-10 | 宁波振华救生设备有限公司 | A kind of low burn temperature atm number controllably slowly produces the gas generator of gas |
| CN114031474B (en) * | 2021-12-24 | 2022-09-02 | 湖北航天化学技术研究所 | Oxygen candle ignition powder and preparation method thereof |
| CN117252100B (en) * | 2023-09-22 | 2024-05-03 | 安徽理工大学 | Airbag performance optimization method and system based on medicament combustion test |
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| JP4131486B2 (en) * | 1999-07-09 | 2008-08-13 | 日本化薬株式会社 | Auto-igniting enhancer composition |
| WO2004048296A1 (en) * | 2002-11-22 | 2004-06-10 | Nippon Kayaku Kabushiki Kaisha | Gas generating agent, process for production thereof, and gas generators for air bags |
| FR2866022B1 (en) * | 2004-02-10 | 2006-07-28 | Snpe Materiaux Energetiques | GAS GENERATING PYROTECHNIC COMPOSITION FOR MOTOR VEHICLE SAFETY |
| CN101466653A (en) * | 2006-04-19 | 2009-06-24 | 日本化药株式会社 | Explosive composition, explosive composition molded body, and their production methods |
| CN108218648B (en) * | 2017-12-20 | 2019-07-12 | 湖北航鹏化学动力科技有限责任公司 | A kind of gas generator |
| CN109438150B (en) * | 2018-11-30 | 2021-07-13 | 湖北航鹏化学动力科技有限责任公司 | Automatic ignition medicament composition, preparation method, application and gas generator |
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