Method of making monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C07D-403/12
C06B-043/00
출원번호
US-0506717
(2012-05-11)
등록번호
US-RE44721
(2014-01-21)
발명자
/ 주소
Hordos, Deborah L.
Burns, Sean P.
출원인 / 주소
TK Holdings Inc.
대리인 / 주소
L.C. Begin & Associates, PLLC
인용정보
피인용 횟수 :
0인용 특허 :
6
초록▼
A method of forming monoammonium salt of 5,5′-bis-1H-tetrazole (BTA-1NH3) is presented comprising the steps of charging a mixing vessel with a solution of free BTA acid and distilled water, adding ammonium hydroxide in excess to obtain a pH of at least 9.5 and mixing the solution, and adding sulfuri
A method of forming monoammonium salt of 5,5′-bis-1H-tetrazole (BTA-1NH3) is presented comprising the steps of charging a mixing vessel with a solution of free BTA acid and distilled water, adding ammonium hydroxide in excess to obtain a pH of at least 9.5 and mixing the solution, and adding sulfuric acid cooled to 10-20 degrees Celsius to obtain a pH of at least 4.5 and mixing the solution. A gas generator 10 containing a gas generant 12 containing the BTA-1NH3 formed in accordance with the present invention is also presented. Gas generating systems 180 such as vehicle occupant protection systems 180, containing the gas generator 10, are also provided.
대표청구항▼
1. A method of forming the monoammonium salt of 5,5′-bis-1H-tetrazolebis-(1(2)H-tetrazol-5-yl)-amine comprising the steps of: charging a mixing vessel with a solution of free 5,5′-bis-1H-tetraolebis-(1(2)H-tetrazol-5-yl)-amine acid and distilled water;ammoniating the solution to obtain a pH of at le
1. A method of forming the monoammonium salt of 5,5′-bis-1H-tetrazolebis-(1(2)H-tetrazol-5-yl)-amine comprising the steps of: charging a mixing vessel with a solution of free 5,5′-bis-1H-tetraolebis-(1(2)H-tetrazol-5-yl)-amine acid and distilled water;ammoniating the solution to obtain a pH of at least 9.5 and mixing the solution; andacidifying the solution while cooling the solution to 5-20 degrees Celsius, to obtain a pH of at least 4.5 and precipitate a solid. 2. The method of claim 1 wherein the ammoniating step comprises adding ammonium hydroxide while heating the solution to about 65-70 C. 3. The method of claim 1 wherein the acidifying step comprises adding 33% sulfuric acid solution to the solution. 4. A solid formed from the method of claim 1. 5. A gas generator device (10) for gas generation, said gas generator containing the solid formed from the method of claim 1. 6. A vehicle occupant protection system containing the solid formed from the method of claim 1. 7. A gas generating composition containing: a fuel containing monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine; andan oxidizer selected from nonmetal and metal nitrate salts, nitrite salts, chlorate salts, metal and nonmetal perchlorate salts, oxides, and mixtures thereof,wherein the monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine is provided in amorphous-shaped crystals, said crystals having no defined regular shape. 8. The gas generating composition of claim 7 further comprising an additive selected from silicone compounds, elemental silicon, silicon dioxide, fused silica, silicones, silicates, natural minerals, lubricants, and mixtures thereof. 9. The gas generating composition of claim 7 wherein said nonmetal and metal nitrate salts are selected from basic metal nitrates, ammonium nitrate, phase-stabilized ammonium nitrate, potassium nitrate, and strontium nitrate. 10. The gas generating composition of claim 7 wherein said nitrite salts are selected from potassium nitrite, said chlorate salts are selected from potassium chlorate, said metal and nonmetal perchlorate salts are selected from potassium perchlorate and ammonium perchlorate, said oxides are selected from iron oxide and copper oxide, and, said basic nitrate salts are selected from basic copper nitrate and basic iron nitrate. 11. The gas generating composition of claim 7 wherein said fuel is provided at about 10 to 50 weight percent of the gas generating composition, and, said oxidizer is provided at about 0.1 to 80 weight percent of the gas generating composition. 12. The gas generating composition of claim 7 wherein said fuel is provided at about 20-35 weight percent of the gas generating composition. 13. The gas generating composition of claim 7 wherein said oxidizer is provided at about 10-70 weight percent of the gas generating composition. 14. The gas generating composition of claim 7 further comprising a secondary fuel selected from anhydrous acid of bis-(1(2)H-tetrazol-5-yl)-amine, acid monohydrate of bis-(1(2)H-tetrazol-5-yl-amine, metal salts of bis-(1(2)H-tetrazol-5-yl)-amine comprising the potassium, sodium, strontium, copper, boron, zinc salts of bis-(1(2)H-tetrazol-5-yl)-amine, and complexes thereof; azoles comprising 5-aminotetrazole; metal salts of azoles comprising potassium 5-aminotetrazole; nonmetal salts of azoles comprising mono- or di-ammonium salt of 5,5′-bis-1H-tetrazole; nitrate salts of azoles comprising 5-aminotetrazole nitrate; nitramine derivatives of azoles comprising 5-nitraminotetrazole; metal salts of nitramine derivatives of azoles comprising dipotassium 5-nitraminotetrazole; nonmetal salts of nitramine derivatives of azoles comprising mono- or di-ammonium 5-nitraminotetrazole and; guanidines comprising dicyandiamide; salts of guanidines comprising guanidine nitrate; nitro derivatives of guanidines comprising nitroguanidine; azoamides comprising azodicarbonamide; nitrate salts of azoamides comprising azodicarbonamidine dinitrate; and mixtures thereof. 15. The gas generating composition of claim 8 wherein said additive is selected from the group comprising polydimethylsiloxane, potassium silicates, talc, clay, graphite powder, graphite fibers, magnesium stearate, boron nitride, molybdenum sulfide, and mixtures thereof. 16. The gas generating composition of claim 7 further comprising a binder selected from the group of binders comprising cellulose derivatives comprising cellulose acetate, cellulose acetate butyrate, carboxymethylcellulose, salts of carboxymethyl cellulose, and carboxymethyl cellulose acetate butyrate; polyalkene carbonates comprising polypropylene carbonate and polyethylene carbonate; and mixtures thereof. 17. The gas generating composition of claim 14 wherein said fuel and secondary fuel when combined are provided at about 0.1 to 80 weight percent of the gas generating composition. 18. The gas generating composition of claim 14 wherein said fuel and secondary fuel when combined are provided at about 10 to 70 weight percent of the gas generating composition. 19. A gas generating composition comprising monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine and phase stabilized ammonium nitrate, wherein the monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine is provided in amorphous-shaped crystals that contain no defined regular shape. 20. The gas generating composition of claim 19 wherein said monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine is provided at about 27 weight percent and said phase stabilized ammonium nitrate is provided at about 73 weight percent, said weight percents taken with regard to the total gas generating composition. 21. A gas generating composition containing: a fuel containing monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine; andan oxidizer selected from nonmetal and metal nitrate salts, nitrite salts, chlorate salts, metal and nonmetal perchlorate salts, oxides, and mixtures thereof,wherein the monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine is provided in amorphous-shaped crystals, said crystals having no defined regular shape, andwherein said gas generating composition is made by the method comprising the steps of charging a mixing vessel with a solution of free bis-(1(2)H-tetrazol-5-yl)-amine acid and distilled water;ammoniating the solution to obtain a pH of at least 9.5 and mixing the solution; andacidifying the solution while cooling the solution to 5-20 degrees Celsius, to obtain a pH of at least 4.5 and precipitate a solid. 22. A gas generating composition comprising monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine and phase stabilized ammonium nitrate, wherein the monoammonium salt of bis-(1(2)H-tetrazol-5-yl)-amine is provided in amorphous-shaped crystals that contain no defined regular shape, and wherein said gas generating composition is made by the method comprising the steps of charging a mixing vessel with a solution of free bis-(1(2)H-tetrazol-5-yl)-amine acid and distilled water;ammoniating the solution to obtain a pH of at least 9.5 and mixing the solution; andacidifying the solution while cooling the solution to 5-20 degrees Celsius, to obtain a pH of at least 4.5 and precipitate a solid.
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이 특허에 인용된 특허 (6)
Khandhadia Paresh S. ; Burns Sean P. ; Williams Graylon K., High gas yield non-azide gas generants.
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