CN116789506A - Gas generating composition for automobile safety belt pretensioner and preparation method thereof - Google Patents
Gas generating composition for automobile safety belt pretensioner and preparation method thereof Download PDFInfo
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- CN116789506A CN116789506A CN202310797375.4A CN202310797375A CN116789506A CN 116789506 A CN116789506 A CN 116789506A CN 202310797375 A CN202310797375 A CN 202310797375A CN 116789506 A CN116789506 A CN 116789506A
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- generating composition
- gas generating
- belt pretensioner
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- nitroguanidine
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- 239000000203 mixture Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003814 drug Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000012216 screening Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 239000008187 granular material Substances 0.000 claims description 44
- IDCPFAYURAQKDZ-UHFFFAOYSA-N 1-nitroguanidine Chemical compound NC(=N)N[N+]([O-])=O IDCPFAYURAQKDZ-UHFFFAOYSA-N 0.000 claims description 33
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- NDEMNVPZDAFUKN-UHFFFAOYSA-N guanidine;nitric acid Chemical compound NC(N)=N.O[N+]([O-])=O.O[N+]([O-])=O NDEMNVPZDAFUKN-UHFFFAOYSA-N 0.000 claims description 21
- ULRPISSMEBPJLN-UHFFFAOYSA-N 2h-tetrazol-5-amine Chemical compound NC1=NN=NN1 ULRPISSMEBPJLN-UHFFFAOYSA-N 0.000 claims description 19
- 239000007800 oxidant agent Substances 0.000 claims description 18
- AXZAYXJCENRGIM-UHFFFAOYSA-J dipotassium;tetrabromoplatinum(2-) Chemical compound [K+].[K+].[Br-].[Br-].[Br-].[Br-].[Pt+2] AXZAYXJCENRGIM-UHFFFAOYSA-J 0.000 claims description 17
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 15
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 15
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 15
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical group OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 15
- 239000000853 adhesive Substances 0.000 claims description 14
- 230000001070 adhesive effect Effects 0.000 claims description 14
- 230000001590 oxidative effect Effects 0.000 claims description 14
- 229910001487 potassium perchlorate Inorganic materials 0.000 claims description 13
- 235000010333 potassium nitrate Nutrition 0.000 claims description 12
- 239000004323 potassium nitrate Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011863 silicon-based powder Substances 0.000 claims description 9
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 7
- 238000004806 packaging method and process Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- ZRALSGWEFCBTJO-UHFFFAOYSA-N guanidine group Chemical group NC(=N)N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 3
- 229910001963 alkali metal nitrate Inorganic materials 0.000 claims description 3
- 229910001485 alkali metal perchlorate Inorganic materials 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 239000001913 cellulose Substances 0.000 claims description 3
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 3
- 125000005587 carbonate group Chemical group 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 239000008188 pellet Substances 0.000 claims 1
- 238000004898 kneading Methods 0.000 abstract description 16
- 239000007789 gas Substances 0.000 description 32
- 239000000047 product Substances 0.000 description 11
- 238000002485 combustion reaction Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- PVGBHEUCHKGFQP-UHFFFAOYSA-N sodium;n-[5-amino-2-(4-aminophenyl)sulfonylphenyl]sulfonylacetamide Chemical compound [Na+].CC(=O)NS(=O)(=O)C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 PVGBHEUCHKGFQP-UHFFFAOYSA-N 0.000 description 1
- -1 specifically Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- 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
- C06B31/08—Compositions containing an inorganic nitrogen-oxygen salt the salt being an alkali metal or an alkaline earth metal nitrate with a metal oxygen-halogen salt, e.g. inorganic chlorate, inorganic perchlorate
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0066—Shaping the mixture by granulation, e.g. flaking
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0075—Shaping the mixture by extrusion
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Air Bags (AREA)
Abstract
The invention discloses a gas generating composition for an automobile safety belt pretensioner, which comprises the following components in percentage by mass: the invention has the characteristics of low hygroscopicity while meeting the requirement of output function, and the sum of the mass percentages of the components is 100 percent. The invention also discloses a preparation method of the gas-generating composition for the automobile safety belt pretensioner, which comprises the steps of weighing raw materials according to mass percent, taking water as a solvent, kneading, extruding, granulating, screening and drying the raw materials to obtain the gas-generating composition for the automobile safety belt pretensioner, namely a gas-generating medicine.
Description
Technical Field
The invention belongs to the technical field of pyrotechnic compositions for civil initiating explosive devices, relates to a gas generating composition for an automobile safety belt pretensioner, and further relates to a preparation method of the gas generating composition for the automobile safety belt pretensioner.
Background
When an automobile collides, a miniature gas generator (hereinafter referred to as MGG) in the safety belt pretensioner is ignited to generate high-temperature high-pressure gas, the gas acts, the safety is tightened, the passenger is restrained on the seat rapidly, and the passenger is prevented from being injured due to inertia forward tilting or sliding. Unlike the gas generating composition for an airbag, the gas generating composition for the MGG has less gas generating amount, fast burning speed, no filter or coolant in the combustion chamber, and high temperature and high pressure gas directly acts towards a ratchet wheel or other mechanisms.
At present, the gas-generating fuel for MGG is changed from nitrocellulose homogeneous powder to heterogeneous gas-generating composition.
The gas-generating composition forming process is divided into two types, namely sheet forming and extrusion forming, and a tabletting process is adopted in foreign countries, and the product comprises the following components: small size, high consistency of size and weight, low crushing force (less than about 10N), low hygroscopicity, and the like. The method is influenced by various factors such as raw materials, equipment and the like, is common in domestic extrusion molding technology, has large difference between output functions of products and foreign products, and is directly expressed as obvious difference of P-t curve forms of a closed explosive device.
Disclosure of Invention
The invention aims to provide a gas generating composition for an automobile safety belt pretensioner, which meets the output function requirement and has the characteristic of low hygroscopicity.
It is another object of the present invention to provide a method for preparing a gas generating composition for an automotive seat belt pretensioner, for preparing a gas generating composition for an automotive seat belt pretensioner.
The first technical scheme adopted by the invention is that the gas generating composition for the automobile safety belt pretensioner comprises the following components in percentage by mass: 40-55% of combustible agent, 40-55% of oxidant, 5-7% of adhesive and 0-5% of auxiliary component, wherein the sum of the mass percentages of the components is 100%;
the combustible agent is guanidine or azole organic matter, the oxidant is alkali metal nitrate and perchlorate, the adhesive is water-soluble cellulose material, and the auxiliary component is carbonate, simple substance or metal oxide.
The invention is also characterized in that:
the combustible agent comprises any two of guanidine nitrate, nitroguanidine and 5-aminotetrazole.
When the combustible agent is guanidine nitrate and nitroguanidine, the mass ratio of guanidine nitrate to nitroguanidine is 1:1 to 1:3, a step of;
when the combustible agent is guanidine nitrate and 5-aminotetrazole, the mass ratio of the guanidine nitrate to the 5-aminotetrazole is 1:1 to 1:2;
when the combustible agent is nitroguanidine and 5-aminotetrazole, the mass ratio of the nitroguanidine to the 5-aminotetrazole is 3:1 to 7:1.
the oxidizing agent comprises potassium nitrate and potassium perchlorate.
The mass ratio of the potassium nitrate to the potassium perchlorate in the oxidant is 1:1 to 1:3.
the binder is hydroxypropyl methylcellulose.
The auxiliary components comprise one or more of lithium carbonate, potassium carbonate, silicon powder and ferric oxide.
The second technical scheme adopted by the invention is that the preparation method of the gas generating composition for the automobile safety belt pretensioner comprises the following steps:
weighing the following raw materials in percentage by mass: 40-55% of combustible agent, 40-55% of oxidant, 5-7% of adhesive and 0-5% of auxiliary component, wherein the sum of the mass percentages of the components is 100%, water is taken as solvent, and the raw materials are prepared through the procedures of kneading, extruding, granulating, screening and drying.
The present invention is also characterized in that,
drying extruded strip materials in the shade before granulating to enable the extruded strip materials to reach a semi-dry state; or directly granulating while extrusion molding, drying the medicinal granules in the shade to make the medicinal granules reach a semi-dry state, and then screening.
The drying is specifically that the medicine particles are dried for 0.5 to 2 hours at a low temperature of between room temperature and 40 ℃; and then drying at a high temperature of between 70 and 105 ℃ until the water content in the medicine granules is not more than 0.4 percent of the total mass of the medicine granules, and sealing and packaging the dried medicine granules after drying.
The beneficial effects of the invention are as follows:
the invention is used for the gas-generating composition of the car safety belt pretensioner, make up the combustion reaction main body with the double-component combustible agent and double-component oxidizing agent, regard water-soluble adhesive as the shaping material, add the auxiliary ingredient according to the ignitability and output requirement; the final effect is evaluated according to the approach degree of the P-t curve form after ignition in the closed explosion device and the curve of the comparison sample, so that the output function requirement is met, and the MGG is assembled, and in addition, the MGG has relatively low hygroscopicity so as to improve the process condition management of the MGG.
The preparation method of the gas generating composition for the automobile safety belt pretensioner is used for preparing the gas generating composition, and has the advantages of simple operation steps, environment-friendly production process and low dust.
Drawings
FIG. 1 is a graph of P-t function test for various examples and comparative sample A;
FIG. 2 is a graph of P-t function test for various examples and comparative sample B;
fig. 3 is a graph of moisture absorption curves for different types of gas generating compositions with viscosity binders.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention relates to a gas generating composition for an automobile safety belt pretensioner, which comprises the following components in percentage by mass: 40-55% of combustible agent, 40-55% of oxidant, 5-7% of adhesive and 0-5% of auxiliary component, and the sum of the mass percentages of the components is 100%.
The combustible agent is guanidine or azole organic substance used as gas-generating fuel, the granularity of the combustible agent is less than 15 μm, more preferably less than 10 μm, and specifically, the combustible agent comprises any two of guanidine nitrate, nitroguanidine and 5-aminotetrazole.
When the combustible agent comprises guanidine nitrate and nitroguanidine, the mass ratio of guanidine nitrate to nitroguanidine is 1:1 to 1:3, a step of; when the combustible agent comprises Guanidine Nitrate (GN) and 5-aminotetrazole (5 AT), the mass ratio of guanidine nitrate to 5-aminotetrazole is 1:1 to 1:2; when the combustible agent comprises Nitroguanidine (NQ) and 5-aminotetrazole (5 AT), the mass ratio of the nitroguanidine to the 5-aminotetrazole is 3:1 to 7:1, a step of;
5-aminotetrazole (5 AT) is selected as an anhydrous raw material; the crystal form of the Nitroguanidine (NQ) is selected to be the best in sphere, the short column shape is inferior, the needle-shaped product is inferior, the influence of the needle-shaped crystal form material on the burning speed is obvious, the burning speed is fast and the consistency is poor in the gas production composition, the microstructure density of the gas production composition products of the needle-shaped and long needle-shaped products is poor, the micropore structure is increased to be hygroscopic, and from the safety point of view, the wet Nitroguanidine (NQ) with the water content of more than 20% is selected, so that the process preparation is complicated, the moisture of the material is detected on the line side, and the total amount and the solvent amount are calculated. In the kneading process, a one-shot mode is preferably used when wet Nitroguanidine (NQ) is used, and the wet Nitroguanidine (NQ) is added and kneaded simultaneously with the binder and the solvent; when dry nitroguanidine is used, it is preferable to knead the binder with water first and then to feed and knead the nitroguanidine separately in a plurality of amounts.
The oxidant is alkali metal nitrate and perchlorate, and is used as main oxygen supply source, the granularity of the oxidant is not more than 25 mu m and more preferably less than 10 mu m, specifically, the oxidant comprises potassium nitrate (KN) and potassium perchlorate (KP), and the mass ratio of the potassium nitrate to the potassium perchlorate in the oxidant is 1:1 to 1:3, a step of;
potassium perchlorate (KP) has a strong gas supply capability, and when the proportion of the composition increases, the combustion speed increases rapidly, and the combustion pressure is relatively high, so that the harmful components in the combustion gas increase correspondingly, and in addition, the ignition energy requirement is high because the performance is stable; the melting point of potassium nitrate (KN) is relatively low, chemical reaction can be initiated by low ignition energy, the proportion of harmful products in combustion products is low, and the disadvantage is that the oxygen supply capability is slightly inferior to that of potassium perchlorate (KP), and the combustion speed is slowly improved; in summary, potassium nitrate (KN) and potassium perchlorate (KP) are used in combination to balance oxygen supply capacity, reaction rate, ignition capacity and end product.
The adhesive is a water-soluble cellulose material, specifically, the adhesive is hydroxypropyl methylcellulose, preferably high-viscosity hydroxypropyl methylcellulose (HPMC), preferably has a mass concentration of 1% and a viscosity of not less than 4000 mPa.s and higher, and the use of the high-viscosity adhesive is beneficial to reducing the mass percentage in the formula, has a large adjustment margin for the formula design, and has better manufacturability of the high-viscosity raw material, relatively compact product and further beneficial to improving the hygroscopicity.
The auxiliary components are carbonate, simple substance or metal oxide, can be used singly or in combination as components for regulating output functions, and are used in most combinations, and specifically, the auxiliary components comprise one or more of lithium carbonate, potassium carbonate, silicon powder and ferric oxide;
lithium carbonate (Li) 2 CO 3 ) Or potassium carbonate (K) 2 CO 3 ) Firstly, the combustion temperature is reduced, secondly, the trace acid components in the raw materials are balanced, the aging performance is optimized, the granularity is smaller than 10 mu m, preferably smaller than 5 mu m, and the mass percent is 0% -3%; silicon powder (Si) can improve the ignition performance and color of the gas-generating composition, the granularity is below 5 mu m, and the mass percentage of the silicon powder is 0-3%; ferric oxide (Fe) 2 O 3 ) Can promote combustion and color, improve the combustion speed, and has granularity smaller than 10 mu m, and the mass percent is 0-0.5%.
The finished product of the gas generating composition is in the shape of cylindrical small particles, and can be provided with single holes or multiple holes or solid.
The invention relates to a preparation method of an MGG gas-generating composition, which comprises the following steps:
weighing the following raw materials in percentage by mass: the composition for producing MGG gas is prepared by taking water accounting for 10-25% of the total mass of the raw materials as a solvent, kneading, extruding, granulating (the ratio of the length to the diameter of the medicine particles is 0.7:1-2.5:1, preferably 1:1), screening and drying the raw materials.
The method is implemented according to the following steps:
step 1, weighing raw materials according to mass percentage, sequentially adding water, an adhesive, a combustible agent, functional additional components and an oxidant, respectively kneading, and feeding the combustible agent and the oxidant for multiple times according to the proportion so as to fully mix, wherein if necessary, a water circulation system is used for cooling or heating the materials to keep the materials at a proper temperature, so that a wet and soft dough-shaped material with certain viscosity and toughness is obtained;
step 2, adopting a press or an extruder, selecting a die, extruding the material into a strip shape, and drying in the shade at room temperature and under the condition that the relative humidity is not lower than 50% before granulating to enable the material to reach a semi-dry state; or, directly granulating while extruding the long strip-shaped material, drying the medicine granules in the shade to enable the medicine granules to reach a semi-dry state, and then screening, wherein the screened medicine granules are cylindrical solid small granules or hollow small granules with a plurality of cores, the diameter of the medicine granules is 0.9-2.2 mm, the length of the medicine granules is 0.6-3.0 mm, and the ratio of the length to the diameter of the medicine granules is 0.7:1 to 2.5:1, preferably 1:1 (the length-diameter ratio is 1:1, the assembly manufacturability is good, and the length-diameter ratio is adjusted according to the combustion performance requirement);
step 3, drying the screened medicine particles at a low temperature of between room temperature and 40 ℃ for 0.5 to 2 hours; and then drying at a high temperature of 70-105 ℃ until the water content in the medicine granules is not more than 0.4% of the total mass of the medicine granules, drying, and sealing and packaging the dried medicine granules.
Example 1
The embodiment provides a preparation method of a gas generating composition for an automobile safety belt pretensioner, which is used for preparing an MGG gas generating composition and is specifically implemented according to the following steps:
step 1, setting the total feeding amount as 100 parts, 20 parts of deionized water or distilled water, taking 6 parts of hydroxypropyl methylcellulose (HPMC), kneading, sequentially adding 30 parts of dry Nitroguanidine (NQ) and 18 parts of Guanidine Nitrate (GN) respectively into two parts, respectively feeding and kneading, and mixing 0.2 part of lithium carbonate (Li 2 CO 3 ) 1 part of silicon powder (Si) is put into a kneader and kneaded, and then 15 parts of potassium nitrate (KN) and 30 parts of potassium perchlorate (KP) are respectively put into the kneader in two parts and kneaded to obtain a dough-like material;
the kneader is preferably of a sandwich structure, and cold water can be used for indirect cooling in order to prevent the material from being excessively high in temperature; when the material temperature is low and the equipment load is too large, warm water is adopted to indirectly heat
Step 2, adopting a press or an extruder, selecting a die with the aperture of 1.6mm, extruding the material into a strip shape, and drying in the shade under the conditions that the room temperature and the relative humidity are not lower than 50 percent to enable the material to reach a semi-dry state (not sticky after being pressed); or directly granulating while extrusion forming, drying the medicinal granules in the shade to make the medicinal granules reach a semi-dry state, and then screening to obtain cylindrical solid small granules or hollow small granules with a plurality of cores;
step 3, drying the screened medicine granules at a low temperature of between room temperature and 40 ℃ for 0.5h; then drying at 90 deg.C until the water content is not more than 0.4% of the total mass of the granule, oven drying, and sealing and packaging.
Example 2
The embodiment provides a preparation method of a gas generating composition for an automobile safety belt pretensioner, which is implemented according to the following steps:
step 1, detecting the water content of wet nitroguanidine in advance, calculating the dosage of the wet nitroguanidine and the free water quantity in the wet nitroguanidine, setting the total dosage as 100 parts, 20 parts of deionized water or distilled water, taking 6 parts of hydroxypropyl methylcellulose (HPMC), 30 parts of nitroguanidine (the amount converted into dry NQ according to the water content) and 0.2 part of lithium carbonate (Li 2 CO 3 ) 1 part of silicon powder (Si) is put into a kneader for one time and kneaded, then 18 parts of Guanidine Nitrate (GN), 15 parts of potassium nitrate (KN) and 30 parts of potassium perchlorate (KP) are respectively divided into two parts for respective feeding and kneading, and finally a dough-shaped material is obtained;
step 2, adopting a press or an extruder, selecting a die with the aperture of 1.6mm, extruding the material into a strip shape, and drying in the shade under the conditions of room temperature and relative humidity not lower than 50% to enable the material to reach a semi-dry state (not sticky after being pressed); or directly granulating while extrusion molding, drying the medicine granules in the shade to make the medicine granules reach a semi-dry state, and then screening to obtain cylindrical solid small granules or hollow small granules with a plurality of cores;
step 3, drying the screened medicine granules at a low temperature of between room temperature and 40 ℃ for 0.5h; then drying at 90 deg.C until the water content is not more than 0.4% of the total mass of the granule, and sealing and packaging.
Example 3
The embodiment provides a preparation method of a gas generating composition for an automobile safety belt pretensioner, which is implemented according to the following steps:
step 1, setting the total feeding amount as 100 parts, 20 parts of deionized water or distilled water, taking 6 parts of hydroxypropyl methylcellulose (HPMC), kneading, sequentially adding 40 parts of Nitroguanidine (NQ), respectively feeding in two parts, kneading, taking 6 parts of 5-aminotetrazole, kneading, respectively feeding and kneading 0.2 part of lithium carbonate, 2 parts of silicon powder and 0.1 part of ferric oxide at one time, respectively feeding in two parts of 16 parts of potassium nitrate and 30 parts of potassium perchlorate, and kneading to obtain a dough-like material;
step 2, adopting a press or an extruder, selecting a die with the aperture of 1.2mm, extruding the material into a strip shape, and drying in the shade under the conditions of room temperature and relative humidity not lower than 50% to enable the material to reach a semi-dry state (not sticky after being pressed); or directly granulating while extruding, drying the medicinal granules in the shade to semi-dry state, and screening to obtain cylindrical solid small granules or hollow small granules with a plurality of cores;
step 3, drying the screened medicine granules at a low temperature of between room temperature and 40 ℃ for 0.5h; then drying at 90 deg.C until the water content is not more than 0.4% of the total mass of the granule, and sealing and packaging.
Example 4
The embodiment provides a preparation method of a gas generating composition for an automobile safety belt pretensioner, which is implemented according to the following steps:
step 1, setting the total feeding amount as 100 parts, 20 parts of deionized water or distilled water, taking 6 parts of adhesive (sodium carboxymethylcellulose, medium-viscosity and high-viscosity HPMC respectively), feeding 0.5 part of silicon powder and 0.2 part of ferric oxide at one time, kneading, taking 20 parts of 5-aminotetrazole, feeding and kneading twice, and taking 20 parts of guanidine nitrate, 15 parts of potassium nitrate and 37 parts of potassium perchlorate, feeding and kneading twice respectively to obtain a dough-shaped material;
step 2, adopting a press or an extruder, selecting a die with the aperture of 1.4mm, extruding into a strip shape, and drying in the shade under the conditions that the room temperature and the relative humidity are not lower than 50 percent to enable the die to be in a semi-dry state (not sticky after being pressed); or directly granulating the extruded strip-shaped material, drying the medicine granules in the shade to enable the medicine granules to reach a semi-dry state, and then screening to obtain cylindrical solid small granules or hollow small granules with a plurality of cores;
step 3, drying the screened medicine granules at a low temperature of between room temperature and 40 ℃ for 0.5h; then drying at 90 deg.C until the water content is not more than 0.4% of the total mass of the granule, and sealing and packaging.
Moisture absorption verification control:
as in example 4, sodium carboxymethyl cellulose, and medium viscosity hydroxypropyl methylcellulose were used as the binder.
The gas-generating compositions prepared in examples 1 and 3 were assembled into MGG, and P-t function test was performed in a 10mL sealed exploder to compare the curve morphology between peak pressures of 30% -70%.
Moisture absorption test method:
1) The test chamber is kept in a relatively constant temperature and humidity state, the space is relatively closed, the comparison test condition of the invention is that the ambient temperature is 25 ℃, the relative humidity is not lower than 65%, the gas generating composition occupies more than 2/3 of the height of the container, and the gas generating composition is open.
2) Comparative formulation of the gas generating composition is shown in example 4, the binder was CMCNa, medium viscosity HPMC, high viscosity HPMC, respectively.
3) The gas-generating composition was exposed to air and absorbed moisture for 120min, each time sampled from the surface layer, tested by an infrared moisture meter, and the sampling time and the test result were recorded, and a time-moisture trend chart was made, as shown in fig. 3.
3) The gas-generating composition was exposed to air and absorbed moisture for 120min, each time sampled from the surface layer, tested by an infrared moisture meter, and the sampling time and the test result were recorded, and a time-moisture trend chart was made, as shown in fig. 3.
The relevant data are shown in Table 1, the comparison results of the scheme and the output function are shown in FIGS. 1-2, and the comparison of hygroscopicity is shown in FIG. 3.
TABLE 1
As can be seen from the above comparative tests, the output performance of the MGG gas-generating composition prepared by the present invention is comparable to that of foreign tabletted products, and the use of a high tack adhesive in the preparation method of the present invention is advantageous for improving the moisture absorption resistance of the gas-generating composition.
Claims (10)
1. The gas generating composition for the automobile safety belt pretensioner is characterized by comprising the following components in percentage by mass: 40-55% of combustible agent, 40-55% of oxidant, 5-7% of adhesive and 0-5% of auxiliary component, wherein the sum of the mass percentages of the components is 100%;
the combustible agent is guanidine or azole organic matter, the oxidant is alkali metal nitrate and perchlorate, the adhesive is water-soluble cellulose material, and the auxiliary component is carbonate, simple substance or metal oxide.
2. The gas generating composition for an automobile seat belt pretensioner according to claim 1, wherein the flammable agent is any two of guanidine nitrate, nitroguanidine, 5-aminotetrazole.
3. The gas generating composition for an automobile seat belt pretensioner according to claim 2, wherein when the combustible agent is guanidine nitrate and nitroguanidine, the mass ratio of guanidine nitrate to nitroguanidine is 1:1 to 1:3, a step of; when the combustible agent is guanidine nitrate and 5-aminotetrazole, the mass ratio of the guanidine nitrate to the 5-aminotetrazole is 1:1 to 1:2; when the combustible agent is nitroguanidine and 5-aminotetrazole, the mass ratio of the nitroguanidine to the 5-aminotetrazole is 3:1 to 7:1.
4. the gas generating composition for an automotive seat belt pretensioner according to claim 1, wherein the oxidizing agent includes potassium nitrate and potassium perchlorate.
5. The gas generating composition for an automobile seat belt pretensioner according to claim 4, wherein a mass ratio of potassium nitrate to potassium perchlorate in the oxidizing agent is 1:1 to 1:3.
6. the gas generating composition for an automotive seat belt pretensioner according to claim 1, wherein the binder is hydroxypropyl methylcellulose.
7. The gas generating composition for an automotive seat belt pretensioner according to claim 1, wherein the auxiliary component includes one or more of lithium carbonate, potassium carbonate, silicon powder, and ferric oxide.
8. A process for the preparation of a gas generating composition for use in an automotive seat belt pretensioner for the preparation of a gas generating composition according to claim 1, characterized by specifically:
weighing the following raw materials in percentage by mass: the gas-producing composition for the automobile safety belt pretensioner is prepared by the steps of mixing, extruding, granulating, screening and drying the raw materials by taking water as a solvent, wherein the total mass percentage of the raw materials is 100%, the combustible agent is 40-55%, the oxidant is 40-55%, the adhesive is 5-7%, the auxiliary components are 0-5%.
9. The method for producing a gas generating composition for an automobile seat belt pretensioner according to claim 8, wherein the extruded elongated material is required to be dried in the shade to be in a semi-dry state before dicing; or directly granulating while extrusion molding, drying the medicinal granules in the shade to make the medicinal granules reach a semi-dry state, and then screening.
10. The method for producing a gas generating composition for an automobile safety belt pretensioner according to claim 8, wherein the drying is specifically that the pellets are dried at a low temperature of from room temperature to 40 ℃ for 0.5h to 2h; and then drying at 70-105 ℃ until the water content in the medicine granules is not more than 0.4% of the total mass of the medicine granules, and sealing and packaging the dried medicine granules.
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