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    • 5. 发明授权
    • Method for synthesizing 5-aminotetrazole
    • 合成5-氨基四唑的方法
    • US5451682A
    • 1995-09-19
    • US179559
    • 1994-01-10
    • Thomas K. HighsmithGary K. Lund
    • Thomas K. HighsmithGary K. Lund
    • C07D257/06
    • C07D257/06
    • A process of preparing 5-aminotetrazole ("5-AT") which proceeds at substantially neutral pH is disclosed. In the process, cyanamide or dicyandiamide and an azide salt are reacted at elevated temperature in the presence of an acid reagent. The acid reagent has a pK.sub.a in the range from about 3 to about 7. Large quantities of hydrazoic acid are not produced during the reaction. Upon completion of the reaction, the reaction mixture is acidified to a pH less than 3 to protonate the 5-AT. Several variations of the acidification step permit control of particle size and morphology. The precipitated particles are isolated to yield 5-AT.
    • 公开了以基本中性pH进行的制备5-氨基四唑(“5-AT”)的方法。 在此过程中,将氰胺或双氰胺和叠氮化物盐在升高的温度下在酸性试剂的存在下反应。 酸试剂的pKa在约3至约7的范围内。在反应期间不会产生大量的氢偶氮。 反应完成后,将反应混合物酸化至小于3的pH以质子化5-AT。 酸化步骤的几个变化允许控制粒度和形态。 分离出沉淀的颗粒,得到5-AT。
    • 6. 发明授权
    • Methods for synthesizing and processing bis-(1(2)H-tetrazol-5-yl)-amine
    • 合成和加工双 - (1(2)H-四唑-5-基) - 胺的方法
    • US5468866A
    • 1995-11-21
    • US177737
    • 1994-01-04
    • Thomas K. HighsmithRobert M. HajikRobert B. WardleGary K. LundReed J. Blau
    • Thomas K. HighsmithRobert M. HajikRobert B. WardleGary K. LundReed J. Blau
    • C07D257/06C07D403/12
    • C07D257/06
    • Methods of preparing bis-(1(2)H-tetrazol-5-yl)-amine (BTA) having improved physical and chemical characteristics are disclosed. In the process, a dicyanamide salt and an azide salt are reacted at high temperature in the presence of an acid reagent. Best yields are obtained when the reaction is allowed to proceed for approximately 48 hours. The dicyanamide salt is preferably present in a stoichiometric excess. The acid reagent has a pK.sub.a in the range from about 3 to about 9. The reaction mixture is acidified to a pH less than 3. Several variations of the acidification step permit control of particle size and morphology. Small, rounded particles are prepared by rapidly cooling the hot crude reaction product coincidentally with acidification. This is preferably accomplished by adding the hot crude reaction product directly to cold concentrated acid. The precipitated particles are isolated to yield BTA.
    • 公开了具有改善的物理和化学特性的双 - (1(2)H-四唑-5-基) - 胺(BTA)的制备方法。 在此过程中,二氰胺盐和叠氮盐在酸性试剂的存在下在高温下反应。 当允许反应进行约48小时时,获得最佳收率。 二氰胺盐优选以化学计量过量存在。 酸试剂的pKa在约3至约9的范围内。将反应混合物酸化至小于3的pH。酸化步骤的几个变化允许控制粒度和形态。 通过与酸化偶然地快速冷却热粗反应产物来制备小的圆形颗粒。 这优选通过将热粗反应产物直接加入到冷的浓酸中来完成。 分离沉淀的颗粒以产生BTA。
    • 7. 发明授权
    • Bitetrazoleamine gas generant compositions
    • 哌嗪胺气体发生剂组合物
    • US5682014A
    • 1997-10-28
    • US101396
    • 1993-08-02
    • Thomas K. HighsmithReed J. BlauGary K. Lund
    • Thomas K. HighsmithReed J. BlauGary K. Lund
    • B60R21/26C06B21/00C06B43/00C06D5/00C06D5/06C06B47/08
    • C06D5/06C06B21/0066C06B43/00
    • A solid composition for generating a nitrogen containing gas is provided. The composition includes an oxidizer and a non-azide fuel selected from a bitetrazoleamine or a derivative or a salt or complex thereof and mixtures thereof. The preferred bitetrazole-amine is bis-(1(2)H-tetrazol-5-yl)-amine, a metal salt, a salt with a nonmetallic cation of a high nitrogen content base or a complex thereof. The salts and complexes are generally metal salts and complexes. The metal can be a transition metal. Metals that have been found to be particularly useful include copper, boron, cobalt, zinc, potassium, sodium, and strontium. The oxidizer is generally a metal oxide or a metal hydroxide. The composition can include certain other components such as secondary oxidizers, burn rate modifiers, slag formers, and binders.
    • 提供了一种用于产生含氮气体的固体组合物。 组合物包括选自四唑胺或其衍生物或其盐或络合物的氧化剂和非叠氮化物燃料及其混合物。 优选的四唑 - 胺是双 - (1(2)H-四唑-5-基) - 胺,金属盐,与高氮含量碱的非金属阳离子或其络合物的盐。 盐和络合物通常是金属盐和络合物。 金属可以是过渡金属。 已发现特别有用的金属包括铜,硼,钴,锌,钾,钠和锶。 氧化剂通常是金属氧化物或金属氢氧化物。 组合物可以包括某些其它组分,例如二次氧化剂,燃烧速率改性剂,成矿剂和粘合剂。