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    Methods for controlled polymerization of energetic cyclic ethers using alkylating salts
    23.
    发明授权
    Methods for controlled polymerization of energetic cyclic ethers using alkylating salts 失效
    使用烷基化盐控制聚合能量环醚的方法

    公开(公告)号：US6100375A

    公开(公告)日：2000-08-08

    申请号：US233219

    申请日：1994-04-26

    申请人： Robert B. Wardle ,  W. Wayne Edwards

    发明人： Robert B. Wardle ,  W. Wayne Edwards

    IPC分类号： C08G65/10 ,  C08G65/18 ,  C08G65/22 ,  C08F6/00 ,  C08G59/00

    CPC分类号： C08G65/18 ,  C08G65/105 ,  C08G65/22

    摘要： Energetic polymers and methods for their synthesis are provided. The polymers are preferably produced from cyclic ether monomers having 4 or 5 member rings. The cyclic ether monomers preferably include energetic functional groups such that a polymer formed from the monomer is itself energetic. Polymerization is catalyzed by a combination of alkylating salt and alcohol. The preferred salts are triethoxonium salts with anions such as hexafluorophosphate, hexachloroantimonate, and tetrafluoroborate. It is found that by employing the combination of selected triethoxonium salts and selected alcohols that it is possible to produce an energetic polymer with predetermined functionality and molecular weight. The salt is found to scavenge water in the reaction mixture, thus increasing control over the functionality of the final product. The salt-alcohol combination also rapidly initiates polymerization and allows higher molecular weights to be achieved. This is particularly important in that one limitation previously experienced in polymerization of the types of monomers used in this invention was an inability to achieve rapid and complete polymerization.

    摘要翻译： 提供了能量聚合物及其合成方法。 聚合物优选由具有4或5个成员环的环醚单体制备。 环醚单体优选包括能量官能团，使得由单体形成的聚合物本身是能量的。 聚合由烷基化盐和醇的组合催化。 优选的盐是具有阴离子如六氟磷酸盐，六氯锑酸盐和四氟硼酸盐的三乙氧基铵盐。 发现通过使用选择的三乙氧基铵盐和选择的醇的组合，可以产生具有预定官能度和分子量的能量聚合物。 发现盐在反应混合物中清除水，从而增加对最终产品的功能的控制。 盐 - 醇组合也快速引发聚合，并且可以实现更高的分子量。 这是特别重要的，因为以前在本发明中使用的单体类型的聚合中经历的一个限制是不能实现快速和完全的聚合。

    Process of crystallizing 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12,-hexaazatetracyclo �5.5.0.0.5,903,11!- dodecane
    24.
    发明授权
    Process of crystallizing 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12,-hexaazatetracyclo �5.5.0.0.5,903,11!- dodecane 失效
    结晶2,4,6,8,10,12-六硝基-2,4,6,8,10,12-六氮杂四环[5.5.0.0,5,903,11] - 十二烷的方法

    公开(公告)号：US5874574A

    公开(公告)日：1999-02-23

    申请号：US991432

    申请日：1997-12-16

    申请人： Harold Eugene Johnston ,  Robert B. Wardle

    发明人： Harold Eugene Johnston ,  Robert B. Wardle

    IPC分类号： C07D487/22 ,  C07D257/02

    CPC分类号： C07D487/22

    摘要： A process of crystallizing CL-20 is disclosed. In the process, a wet CL-20 solvent/CL-20 solution is dried by azeotropic distillation of a CL-20 solvent/water azeotrope. Removal of water from the CL-20 solution permits crystallization of high density CL-20. A low density, CL-20 non-solvent is added to the resulting dry CL-20 solvent/CL-20 solution to cause precipitation of .epsilon.-polymorph CL-20. The CL-20 crystals are separated from the non-solvent and the solvent by adding sufficient water to displace the non-solvent and the solvent from the surface of the CL-20 crystals. In this fashion, the .epsilon.-polymorph CL-20 is made wet for later handling, packaging, and shipping.

    摘要翻译： 公开了一种结晶CL-20的方法。 在此过程中，通过CL-20溶剂/水共沸物的共沸蒸馏干燥湿CL-20溶剂/ CL-20溶液。 从CL-20溶液中去除水可以使高密度CL-20结晶。 向所得干CL-20溶剂/ CL-20溶液中加入低密度CL-20非溶剂，引起ε-多晶型物CL-20的沉淀。 通过加入足够的水以从CL-20晶体的表面置换非溶剂和溶剂，将CL-20晶体与非溶剂和溶剂分离。 以这种方式，将ε-多晶型物CL-20制成湿润用于后续处理，包装和运输。

    Synthesis of bis(2,2-dinitropropyl)acetal (BDNPA)
    25.
    发明授权
    Synthesis of bis(2,2-dinitropropyl)acetal (BDNPA) 失效
    双（2,2-二硝基丙基）缩醛（BDNPA）的合成

    公开(公告)号：US5648556A

    公开(公告)日：1997-07-15

    申请号：US339138

    申请日：1994-11-14

    申请人： R. Scott Hamilton ,  Robert B. Wardle

    发明人： R. Scott Hamilton ,  Robert B. Wardle

    IPC分类号： C07C201/12 ,  C07B61/00 ,  C07C205/29 ,  C07C41/50 ,  C07C43/30

    CPC分类号： C07C201/12

    摘要： A nonsolvent process of synthesizing bis(2,2-dinitropropyl)acetal (BDNPA) is disclosed. In the process, 2,2-dinitropropanol (DNPOH) is reacted at low temperature with an acetaldehyde source in the presence of an acid catalyst, such as a Lewis acid catalyst or protic acid catalyst. To inhibit by product formation, the reaction temperature is maintained from about -30.degree. C. to 30.degree. C. Upon completion of the reaction, the reaction solution is quenched with water and washed with an aqueous hydroxide solution. The hydroxide concentration should be sufficient to neutralize any acid formed during the quenching step and to solubilize unreacted 2,2-dinitropropanol as well as other aqueous soluble byproducts in the reaction solution. The BDNPA product is extracted with methyl tert-butyl ether (MTBE) or equivalent solvent. The organic solvent is evaporated to yield usable BDNPA product. The resulting yield is at least 50% based on the starting quantity of 2,2-dinitropropanol.

    摘要翻译： 公开了合成双（2,2-二硝基丙基）缩醛（BDNPA）的非溶剂方法。 在此过程中，在酸催化剂如路易斯酸催化剂或质子酸催化剂存在下，将2,2-二硝基丙醇（DNPOH）在低温下与乙醛源反应。 为了抑制产物形成，将反应温度保持在约-30℃至30℃。反应完成后，将反应溶液用水淬灭并用氢氧化钠水溶液洗涤。 氢氧化物浓度应足以中和淬灭步骤中形成的任何酸，并将未反应的2,2-二硝基丙醇以及其他水溶性副产物溶解在反应溶液中。 用甲基叔丁基醚（MTBE）或等效溶剂萃取BDNPA产物。 将有机溶剂蒸发，得到可用的BDNPA产物。 基于2,2-二硝基丙醇的起始量，所得产率为至少50％。

    High solids rocket motor propellants using diepoxy curing agents
    26.
    发明授权
    High solids rocket motor propellants using diepoxy curing agents 失效
    使用二环氧固化剂的高固体火箭发动机推进剂

    公开(公告)号：US5554820A

    公开(公告)日：1996-09-10

    申请号：US406573

    申请日：1995-03-20

    申请人： Robert B. Wardle ,  R. Scott Hamilton

    发明人： Robert B. Wardle ,  R. Scott Hamilton

    IPC分类号： C06B45/10

    CPC分类号： C06B45/10

    摘要： A PBAN-based solid rocket motor propellant which includes more than 85% or more solids is provided. Propellants of this nature are possible using the combination of diepoxide curing agents and PBAN as a binder. The curing agents include diepoxides having 4 to about 10 carbon atoms. It has been observed that when a diepoxide curing agent is substituted for conventional curing agents, viscosities are significantly reduced, thus enabling the addition of higher percentages of solids in the propellant formulation. Total solids loading of over 85% are achievable while maintaining end-of-mix viscosities within acceptable ranges.

    摘要翻译： 提供了一种包含超过85％或更多固体的PBAN固体火箭发动机推进剂。 这种性质的推进剂可以使用二环氧化物固化剂和PBAN作为粘合剂的组合。 固化剂包括具有4至约10个碳原子的二环氧化物。 已经观察到，当二环氧化物固化剂代替常规固化剂时，粘度显着降低，因此能够在推进剂制剂中添加更高百分比的固体。 总固体含量超过85％是可以实现的，同时保持混合后的粘度在可接受的范围内。

    Synthesis of 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.05,903,11]dode cane
    27.
    发明授权
    Synthesis of 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.05,903,11]dode cane 失效
    合成4,10-二硝基-2,6,8,12-四氧杂-4,10-二氮杂四环[5.5.0.05,903,11]十二烷

    公开(公告)号：US5498711A

    公开(公告)日：1996-03-12

    申请号：US101458

    申请日：1993-08-02

    申请人： Thomas K. Highsmith ,  W. Wayne Edwards ,  Robert B. Wardle

    发明人： Thomas K. Highsmith ,  W. Wayne Edwards ,  Robert B. Wardle

    IPC分类号： C06B25/34 ,  C06B45/10 ,  C07D498/22

    CPC分类号： C07D498/22 ,  C06B25/34 ,  C06B45/10 ,  C06B45/105

    摘要： 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.0.sup.5,9 0.sup.3,11 ]dodecane is synthesized by reacting a diacyl-2,3,5,6-tetraoxypiperazine or tetraoxadiazaisowurtzitane derivative, a strong acid, and a nitrate source, such that an exothermic reaction occurs which proceeds at a temperature above ambient temperature. The reaction product is precipitated by cooling. It may be purified by washing with methanol and/or sodium bicarbonate and by simmering in nitric acid.

    摘要翻译： 4,10-二硝基-2,6,8,12-四氧杂-4,10-二氮杂四环[5.5.0.05,903,11]癸烷是通过二酰基-2,3,5,6-四氧哌嗪或四氧杂二氮杂异纤锌矿型结构烷烃 衍生物，强酸和硝酸盐源，使得发生在高于环境温度的温度下进行的放热反应。 反应产物通过冷却沉淀。 它可以通过用甲醇和/或碳酸氢钠洗涤并通过在硝酸中煨来进行纯化。

    Gas generating compositions containing nitrotriazalone
    28.
    发明授权
    Gas generating compositions containing nitrotriazalone 失效
    包含硝基三唑的气体发生组合物

    公开(公告)号：US4931112A

    公开(公告)日：1990-06-05

    申请号：US439464

    申请日：1989-11-20

    申请人： Robert B. Wardle ,  Jerald C. Hinshaw ,  Robert M. Hajik

    发明人： Robert B. Wardle ,  Jerald C. Hinshaw ,  Robert M. Hajik

    IPC分类号： B60R21/26 ,  C06B25/00 ,  C06D5/00 ,  C06D5/06

    CPC分类号： C06B25/00 ,  C06D5/06

    摘要： Automotive airbag gas generant formulation providing an alternative to commercially used formulations containing sodium azide. The composition contains from about 25% to about 75% by weight of 5-nitro-1,2,4-trizal-3-one (usually known as nitrotriazolone). The other principal ingredient of the composition is from about 25% to about 75% by weight of an anhydrous oxidizing salt having a cation selected from metals of Group I-A of the Periodic Table (except sodium), calcium, strontium, or barium, and an anion which is essentially free of carbon, hydrogen, or halogens. From about 0.1% to about 5% of a binder can be added, if necessary. An automotive airbag inflator containing the composition and a method for generating gas comprising the step of igniting the composition stated above are also disclosed.

    Method of producing thermoplastic elastomers having alternate crystalline structure for use as binders in high-energy compositions
    29.
    发明授权
    Method of producing thermoplastic elastomers having alternate crystalline structure for use as binders in high-energy compositions 失效
    制备具有交替晶体结构的热塑性弹性体的方法，用作高能组合物中的粘合剂

    公开(公告)号：US4806613A

    公开(公告)日：1989-02-21

    申请号：US174665

    申请日：1988-03-29

    申请人： Robert B. Wardle

    发明人： Robert B. Wardle

    IPC分类号： C06B45/10 ,  C08G18/10 ,  C08G18/12 ,  C08G18/48 ,  C08G18/50 ,  C08G18/67 ,  C08G18/72 ,  C08G18/75 ,  C08G18/76 ,  C08G65/16 ,  C08G65/18 ,  C08G65/20 ,  C08G65/22

    CPC分类号： C08G18/7621 ,  C08G18/12 ,  C08G18/48 ,  C08G18/4854 ,  C08G18/4858 ,  C08G18/5003 ,  C08G18/5021 ,  C08G18/6795 ,  C08G18/755 ,  C08G2250/00

    摘要： A method of preparing a thermoplastic elastomer having A blocks and at least one B block, wherein said A blocks are crystalline at temperatures below about 60.degree. C. and said B block(s) is amorphous at temperatures above about -20.degree. C., said A blocks each being polyethers derived from monomers of oxetane and its derivatives and/or tetrahydrofuran and its derivatives, the method comprisingproviding hydroxyl terminated A blocks which are crystalline at temperatures below about 60.degree. C. and separately providing hydroxyl terminated B blocks which are amorphous at temperatures above about -20.degree. C.,end-capping said A blocks and said B blocks by separately reacting each of said A blocks and B blocks with a diisocyanate in which one isocyanate moiety is at least about five times as reactive with the terminal hydroxyl groups of each of the blocks as the other isocyanate moiety, whereby the more reactive isocyanate moiety tends to react with terminal hydroxyl groups of the blocks, leaving the less reactive isocyanate moiety free and unreacted,mixing said end-capped A blocks and said end-capped B blocks together at approximately the stoichiometric ratios that they are intended to be present in the thermoplastic elastomer, andreacting said mixture with a linking compound having two isocyanate-reactive groups which are sufficiently unhindered to react with the free isocyanate groups of said end-capped polymer.