WO2007012348A1 - Gas generating composition for automotive use manufactured by pellet formation - Google Patents
Gas generating composition for automotive use manufactured by pellet formation Download PDFInfo
- Publication number
- WO2007012348A1 WO2007012348A1 PCT/EP2005/053637 EP2005053637W WO2007012348A1 WO 2007012348 A1 WO2007012348 A1 WO 2007012348A1 EP 2005053637 W EP2005053637 W EP 2005053637W WO 2007012348 A1 WO2007012348 A1 WO 2007012348A1
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- WO
- WIPO (PCT)
- Prior art keywords
- gas generating
- generating composition
- composition according
- composition
- previous
- Prior art date
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Classifications
-
- 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
- C06B21/0041—Shaping the mixture by compression
-
- 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
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/007—Ballistic modifiers, burning rate catalysts, burning rate depressing agents, e.g. for gas generating
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
- C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
- C06D5/06—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of two or more solids
Definitions
- the present invention refers to gas generating compositions for filling a vehicle occupant protection device, such as an airbag.
- the compositions of the invention have a reduced pressure exponent, high clean gas generation performance and can be easily processed by means of pellet formation without requiring binders.
- a vehicle occupant protection device such as an airbag, generally comprises a housing, a gas generating material inside said housing, a starter so that the gas generating material can combust, and means for leading the gas to the airbag.
- the starter makes the gas generating composition combust, producing an inflated gas volume. This gas is led to the airbag which expands, protecting the vehicle occupant.
- Pellet formation of the gas generating material in automatic mechanical presses is the most cost-effective industrial manufacturing process due to the rates of output obtained and the easy process control. However the process has the drawback of showing difficulties when components with certain particle sizes are used.
- a solution to this problem is the use of binders. However, their use reduces the rate of output and frequently forces working with mixtures under heat.
- compositions containing azides, composite propellants or nitramide propellants have been used, among other components, in gas generating compositions used up until now. These compounds have drawbacks in terms of toxicity of the generated gases, long-term stability or low burning rates.
- Dinitramide-based propellants have been developed to solve these problems .
- Dinitramides have the general formula X + [N (NO 2 ) 2 ] ' , where X+ is the cationic counterion. These compounds have high burning rates and do not produce reaction products that can be toxic. In this sense, dinitramides have been used as propellants, for example in US patents 5,498,303 and 5,324,075.
- a dinitramide has particularly been disclosed that produces an especially satisfactory result. It is guanylurea dinitramide (C 2 N 7 H 7 O 5 , hereinafter GUDN) .
- This compound has the following advantages:
- the problem to be resolved by the present invention is to provide gas generating compositions having reduced pressure exponents while at the same time maintaining processing features allowing them to be processed by pellet formation without requiring binders .
- compositions of the invention show an improved performance against aging when their humidity content is less than 0.2%.
- the invention is aimed at an improved gas generating composition
- GUDN a mixture of potassium nitrate (NO 3 K) and basic copper nitrate
- a gas generating composition is thus obtained which has the previously mentioned advantages derived from the presence of GUDN, especially a burning rate substantially independent of the particle size, but in which the combustion temperature and dependence of the burning rate on pressure have been substantially reduced as a result of the incorporation of an effective amount of at least one pressure exponent reducing additive (not a binder) .
- the invention is aimed at a process for producing said gas generating compositions, comprising the step of drying the composition until having a humidity content of less than 0.2%. This process facilitates the production of gas generating compositions having a smaller pressure exponent.
- the invention refers to the use of said composition in vehicle occupant protection devices such as airbags .
- Figure 1 shows the dependence of the burning rate on pressure for compositions with different GUDN particle sizes.
- Figure 2 shows the dependence of the burning rate on pressure for compositions with different MgO contents.
- Figure 3 shows the dependence of the burning rate on the % of MgO added to the composition at a given pressure (22 MPa) .
- Figures 4a and 4b show the dependence of the burning rate on pressure for different compositions which have been subjected to aging tests under different relative humidity conditions.
- the composition comprises as a fuel component the guanylurea dinitramide (GUDN) .
- the percentage of GUDN used in the preferred embodiment is about 50-70% by weight of the total composition or less.
- a mixture of potassium nitrate (NO 3 K) and basic copper nitrate (NO S ) 2 CU-SCU(OH) 2 is used as an oxidizer.
- the latter has the property of reducing the combustion temperature and reducing the pressure exponent.
- the sum of these two oxidizers is about 25-35% of the mixture or less.
- MgO is added in the preferred embodiment to reduce the dependence of the burning rate on pressure. All the indicated percentages are by weight unless otherwise specified.
- potassium perchlorate is added in the preferred embodiment to favor CO 2 production, reducing CO production.
- between 0%-l% of zinc or magnesium stearate is added to reduce the humidity absorption capacity of the composition.
- the first of the two is preferably added since its melting point is 130 0 C compared to 87 0 C for magnesium stearate.
- the humidity content of the composition is less than 0.2% in order to improve its performance against aging.
- the addition of zinc stearate reduces the humidity absorption capacity such that in order to have good aging results, the H2O content of the pellets must be less than 0.2%, which corresponds to pellet aging at a relative humidity of 0% (dryness) .
- compositions of the invention have a burning rate of about 20 mm/s at 22 MPa and pressure exponents
- the manufacturing process corresponds to the general scheme:
- the press used is preferably a double-acting automatic feed rotary press, the entire process being carried out under controlled environmental conditions.
Abstract
A gas generating composition for an inflatable vehicle occupant protection device in pellet form comprising a fuel component that is guanylurea dinitramide, an oxidizer that is a mixture of potassium nitrate (NO3K) and basic copper nitrate (NO3)2Cu 3Cu(OH)2 and an effective amount of at least one composition pressure exponent modifying compound such as MgO at a concentration of about 2 to 6%. The invention also refers to a process for obtaining said composition.
Description
GAS GENERATING COMPOSITION FOR AUTOMOTIVE USE MANUFACTURED BY
PELLET FORMATION
FIELD OF THE INVENTION The present invention refers to gas generating compositions for filling a vehicle occupant protection device, such as an airbag. The compositions of the invention have a reduced pressure exponent, high clean gas generation performance and can be easily processed by means of pellet formation without requiring binders.
BACKGROUND OF THE INVENTION
A vehicle occupant protection device, such as an airbag, generally comprises a housing, a gas generating material inside said housing, a starter so that the gas generating material can combust, and means for leading the gas to the airbag. When the vehicle experiences a collision, the starter makes the gas generating composition combust, producing an inflated gas volume. This gas is led to the airbag which expands, protecting the vehicle occupant. Pellet formation of the gas generating material in automatic mechanical presses is the most cost-effective industrial manufacturing process due to the rates of output obtained and the easy process control. However the process has the drawback of showing difficulties when components with certain particle sizes are used. A solution to this problem is the use of binders. However, their use reduces the rate of output and frequently forces working with mixtures under heat.
Compositions containing azides, composite propellants or nitramide propellants have been used, among other components, in gas generating compositions used up until now. These compounds have drawbacks in terms of toxicity of the generated gases, long-term stability or low burning rates.
Dinitramide-based propellants have been developed to solve these problems . Dinitramides have the general formula X+[N (NO2) 2] ', where X+ is the cationic counterion. These compounds have high burning rates and do not produce reaction products that can be toxic. In this sense, dinitramides have
been used as propellants, for example in US patents 5,498,303 and 5,324,075. A dinitramide has particularly been disclosed that produces an especially satisfactory result. It is guanylurea dinitramide (C2N7H7O5, hereinafter GUDN) . This compound has the following advantages:
- it produces low molecular weight non-toxic gases, and
- it has low sensitivity to impact and friction; However it also has some drawbacks: it has a relatively high combustion temperature within guanidine fuel components, and it has a high and strongly pressure-dependent burning rate .
A case of this type is disclosed in international publication WO98/55428, which has given rise, among others, to European patent EP 1,007,496. Although several methods of obtaining GUDN are disclosed in this document, no specific gas generating compositions are disclosed, nor is their processing for gas generators for automotive use disclosed.
Another document of this type is US patent 6,117,255, disclosing a gas generating composition comprising GUDN as a fuel component, together with oxidizers and binders. However, due to the lack of using lubricants or burning rate modifiers, these compositions produce very high pressure exponents, that is, the burning rate is highly dependent on pressure, and furthermore the use of binders makes formation in mechanical presses difficult, reducing the rate of output. SUMMARY OF THE INVENTION
Accordingly, the problem to be resolved by the present invention is to provide gas generating compositions having reduced pressure exponents while at the same time maintaining processing features allowing them to be processed by pellet formation without requiring binders .
The solution is based on the fact that the inventors have found that when GUDN is used as a fuel, the composition burning rate is virtually independent of the particle size used.
Therefore it is possible to use those particle sizes facilitating pellet formation without needing to use binders
which make their processing difficult. This factor in combination with the addition of at least one compound reducing the gas exponent of the composition, particularly MgO, provides gas generating compositions having reduced pressure exponents while at the same time maintaining processing features allowing them to be processed by pellet formation without requiring binders. It must be understood that MgO as a pressure exponent reducer is given only as an example and that any other compound or compounds could be used as long as they perform the function of reducing the composition pressure exponent.
It has further been found that the compositions of the invention show an improved performance against aging when their humidity content is less than 0.2%.
Therefore in a first aspect, the invention is aimed at an improved gas generating composition comprising GUDN and a mixture of potassium nitrate (NO3K) and basic copper nitrate
(NO3) 2* 3Cu (OH) 2. A gas generating composition is thus obtained which has the previously mentioned advantages derived from the presence of GUDN, especially a burning rate substantially independent of the particle size, but in which the combustion temperature and dependence of the burning rate on pressure have been substantially reduced as a result of the incorporation of an effective amount of at least one pressure exponent reducing additive (not a binder) . In a second aspect the invention is aimed at a process for producing said gas generating compositions, comprising the step of drying the composition until having a humidity content of less than 0.2%. This process facilitates the production of gas generating compositions having a smaller pressure exponent. In a third aspect the invention refers to the use of said composition in vehicle occupant protection devices such as airbags . BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 shows the dependence of the burning rate on pressure for compositions with different GUDN particle sizes.
Figure 2 shows the dependence of the burning rate on pressure for compositions with different MgO contents.
Figure 3 shows the dependence of the burning rate on the % of MgO added to the composition at a given pressure (22 MPa) .
Figures 4a and 4b show the dependence of the burning rate on pressure for different compositions which have been subjected to aging tests under different relative humidity conditions.
DETAILED DESCRIPTION OF THE INVENTION
In the preferred embodiment of the invention, the composition comprises as a fuel component the guanylurea dinitramide (GUDN) . The percentage of GUDN used in the preferred embodiment is about 50-70% by weight of the total composition or less. Furthermore, a mixture of potassium nitrate (NO3K) and basic copper nitrate (NOS)2CU-SCU(OH)2 is used as an oxidizer.
The latter has the property of reducing the combustion temperature and reducing the pressure exponent. In the preferred embodiment the sum of these two oxidizers is about 25-35% of the mixture or less. Finally, between 3-6% of MgO is added in the preferred embodiment to reduce the dependence of the burning rate on pressure. All the indicated percentages are by weight unless otherwise specified. Between 0% and 6% of potassium perchlorate is added in the preferred embodiment to favor CO2 production, reducing CO production.
In yet another preferred embodiment about 7% of Fe3O4 is added to improve the oxygen balance and facilitate pellet formation.
In yet another preferred embodiment between 0%-l% of zinc or magnesium stearate is added to reduce the humidity absorption capacity of the composition. The first of the two is preferably added since its melting point is 1300C compared to 870C for magnesium stearate.
And in an additional preferred embodiment the humidity content of the composition is less than 0.2% in order to improve its performance against aging.
EXAMPLES EXAMPLE 1
A series of tests were performed in order to determine the dependence of the burning rate on the GUDN particle size in the
composition. The following formulation, hereinafter called "basic formulation", was tested, incorporating GUDN batches of different particle sizes: GUDN/KNO3/Cu (NO3) 2 -Cu (OH) 2/Fe304/Mg0 in the ratios of 56/23/10/7/0-6.
The results are shown in Table 1 and Figure 1.
Table 1
It can be observed how the burning rate is virtually independent of the GUDN particle size, whereas in the absence of other additional components, there is certain dependence on the pressure. This makes it possible to use the particle sizes that are most favorable for pellet formation without the particle size having a significant effect on the burning rate. EXAMPLE 2 The effect of the amount of MgO in the formulation on the burning rate of the composition was determined in another series of tests. To that end the basic formulation was again used to start from, to which different MgO concentrations were added. The results are shown in Figure 2. It can be concluded from these results that the addition of MgO in concentrations in the range of 4-6% slightly reduces the dependence of the burning rate on pressure. This effect is more clearly observed in Figure 3. This figure shows the influence of added MgO concentration on the burning rate at a certain pressure (specifically at 22 MPa) . It can be observed that when the MgO concentration is increased initially, the burning rate notably decreases until reaching an area of greater stability at MgO concentrations in the order of 4%-6%. EXAMPLE 3 Compositions which were subjected to aging tests under
conditions of different relative humidity were then tested. The results are shown in Figures 4a and 4b.
In a first series of tests the dependence of the burning rate on pressure was studied for different samples of the basic composition which had been aged under different conditions of relative humidity (under dryness or under 40%, 60% or 80% relative humidity) (Figure 4a) . It is observed that when the pellets have been aged under conditions of increasing relative humidity, the burning rate exponentially increases under all pressures.
In a second series of tests samples of the same basic composition to which 0.3% zinc stearate was added were tested under the same conditions (Figure 4b) . The increasing humidity of the pellets continues giving rise to an increase in the burning rate of the composition, although with a smaller pressure exponent in all cases.
Therefore, it is observed that the addition of zinc stearate reduces the humidity absorption capacity such that in order to have good aging results, the H2O content of the pellets must be less than 0.2%, which corresponds to pellet aging at a relative humidity of 0% (dryness) .
In summary, the compositions of the invention have a burning rate of about 20 mm/s at 22 MPa and pressure exponents
(n) of less than one, that is, it shows very high performances while at the same time they can be processed by pellet formation with a high rate of output.
The manufacturing process corresponds to the general scheme:
DRYING AND MIXING
SIEVING RAW → AND →
MATERIALS HOMOGENIZING
FIRST SECOND
→ GRANULATION → COMPRESSION → COMPRESSION STEP STEP
ending with a step for drying the pellets to a degree of
humidity of less than 0.2%.
The press used is preferably a double-acting automatic feed rotary press, the entire process being carried out under controlled environmental conditions.
Claims
1.- A gas generating composition for an inflatable vehicle occupant protection device, comprising a fuel component that is guanylurea dinitramide and an oxidizer, characterized in that the oxidizer is a mixture of potassium nitrate (NO3K) and basic copper nitrate (NO3) 2Cu • 3Cu (OH) 2, and in that it further comprises an effective amount of at least one composition pressure exponent modifying compound.
2.- A gas generating composition according to claim 1, characterized in that the pressure exponent modifying compound is MgO at a concentration of about 2 to 6% of MgO.
3.- A gas generating composition according to claims 1 or 2, characterized in that the guanylurea dinitramide comprises 50- 70% by weight of the total composition.
4.- A gas generating composition according to claims 1 to 3, characterized in that the mixture of potassium nitrate (NO3K) and basic copper nitrate (NO3) 2Cu- 3Cu (OH) 2 is about 25%-35% by weight of the total composition.
5.- A gas generating composition according to any of the previous claims, characterized in that it further comprises 0-6% of potassium perchlorate in order to reduce carbon monoxide emission .
6.- A gas generating composition according to any of the previous claims, characterized in that it further comprises 0-1% of zinc stearate in order to reduce the humidity absorption capacity of the composition.
7.- A gas generating composition according to any of the previous claims, characterized in that it further comprises about 7% of Fe3O4 in order to improve the oxygen balance and pellet formation ease.
8.- A gas generating composition according to any of the previous claims, characterized in that the humidity content is less than 0.2%.
9.- A gas generating composition according to any of the previous claims, characterized in that it is in pellet form.
10.- A process of obtaining a gas generating composition for an inflatable vehicle occupant protection device according to any of claims 1 to 8, characterized in that it comprises the step of drying the composition to a humidity content value of less than 0.2%.
11.- A process of obtaining a gas generating composition according to claim 9, characterized in that the pressing is carried out in automatic feed and automatic extraction mechanical rotary presses.
12.- A process of obtaining a gas generating composition according to any of claims 9 or 10, characterized in that said composition is in pellet form.
13.- Use of a gas generating compound according to any of claims 1 to 8 for inflating an inflatable vehicle occupant protection device such as an airbag.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/EP2005/053637 WO2007012348A1 (en) | 2005-07-26 | 2005-07-26 | Gas generating composition for automotive use manufactured by pellet formation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/EP2005/053637 WO2007012348A1 (en) | 2005-07-26 | 2005-07-26 | Gas generating composition for automotive use manufactured by pellet formation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2007012348A1 true WO2007012348A1 (en) | 2007-02-01 |
Family
ID=36582019
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/EP2005/053637 WO2007012348A1 (en) | 2005-07-26 | 2005-07-26 | Gas generating composition for automotive use manufactured by pellet formation |
Country Status (1)
| Country | Link |
|---|---|
| WO (1) | WO2007012348A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2346797A1 (en) * | 2008-11-12 | 2011-07-27 | Autoliv ASP, INC. | Gas generating compositions having glass fibers |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0659711A2 (en) * | 1993-12-10 | 1995-06-28 | Morton International, Inc. | Processing aids for gas generants |
| US5500059A (en) * | 1993-08-02 | 1996-03-19 | Thiokol Corporation | Anhydrous 5-aminotetrazole gas generant compositions and methods of preparation |
| WO1998055428A1 (en) * | 1997-05-21 | 1998-12-10 | Försvarets Forskningsanstalt | New chemical compound, explosive containing the compound and use of the compound in gas generators |
| EP1006096A1 (en) * | 1998-12-02 | 2000-06-07 | TRW Airbag Systems GmbH & Co. KG | Non-azide gas generating composition |
| US6117255A (en) * | 1998-07-28 | 2000-09-12 | Trw Inc. | Gas generating composition comprising guanylurea dinitramide |
| US6132537A (en) * | 1998-04-08 | 2000-10-17 | Trw Airbag Systems Gmbh & Co. Kg | Azide-free gas-producing composition |
| US6143102A (en) * | 1999-05-06 | 2000-11-07 | Autoliv Asp, Inc. | Burn rate-enhanced basic copper nitrate-containing gas generant compositions and methods |
| US6176950B1 (en) * | 1999-05-17 | 2001-01-23 | James C. Wood | Ammonium nitrate and paraffinic material based gas generating propellants |
| US20020079031A1 (en) * | 2000-12-22 | 2002-06-27 | Snpe | Gas-generating pyrotechnic compositions with a hydrocarbonaceous binder and continuous manufacturing process |
| EP1342705A1 (en) * | 2000-10-10 | 2003-09-10 | Nippon Kayaku Kabushiki Kaisha | Gas-generating agent composition and gas generator employing the same |
-
2005
- 2005-07-26 WO PCT/EP2005/053637 patent/WO2007012348A1/en not_active Application Discontinuation
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5500059A (en) * | 1993-08-02 | 1996-03-19 | Thiokol Corporation | Anhydrous 5-aminotetrazole gas generant compositions and methods of preparation |
| EP0659711A2 (en) * | 1993-12-10 | 1995-06-28 | Morton International, Inc. | Processing aids for gas generants |
| WO1998055428A1 (en) * | 1997-05-21 | 1998-12-10 | Försvarets Forskningsanstalt | New chemical compound, explosive containing the compound and use of the compound in gas generators |
| US6132537A (en) * | 1998-04-08 | 2000-10-17 | Trw Airbag Systems Gmbh & Co. Kg | Azide-free gas-producing composition |
| US6117255A (en) * | 1998-07-28 | 2000-09-12 | Trw Inc. | Gas generating composition comprising guanylurea dinitramide |
| EP1006096A1 (en) * | 1998-12-02 | 2000-06-07 | TRW Airbag Systems GmbH & Co. KG | Non-azide gas generating composition |
| US6143102A (en) * | 1999-05-06 | 2000-11-07 | Autoliv Asp, Inc. | Burn rate-enhanced basic copper nitrate-containing gas generant compositions and methods |
| US6176950B1 (en) * | 1999-05-17 | 2001-01-23 | James C. Wood | Ammonium nitrate and paraffinic material based gas generating propellants |
| EP1342705A1 (en) * | 2000-10-10 | 2003-09-10 | Nippon Kayaku Kabushiki Kaisha | Gas-generating agent composition and gas generator employing the same |
| US20020079031A1 (en) * | 2000-12-22 | 2002-06-27 | Snpe | Gas-generating pyrotechnic compositions with a hydrocarbonaceous binder and continuous manufacturing process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2346797A1 (en) * | 2008-11-12 | 2011-07-27 | Autoliv ASP, INC. | Gas generating compositions having glass fibers |
| EP2346797A4 (en) * | 2008-11-12 | 2013-12-18 | Autoliv Asp Inc | Gas generating compositions having glass fibers |
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