Method of producing thermoplastic elastomers having alternate
crystalline structure such as polyoxetane ABA or star block copolymers
by a block linking process
    1.
    发明授权
    Method of producing thermoplastic elastomers having alternate crystalline structure such as polyoxetane ABA or star block copolymers by a block linking process 失效
    具有交替结晶结构的热塑性弹性体如聚氧杂环丁烷ABA或通过嵌段连接方法的星形嵌段共聚物的方法

    公开(公告)号:US5516854A

    公开(公告)日:1996-05-14

    申请号:US559179

    申请日:1990-07-27

    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 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 comprising:providing monofunctional hydroxyl terminated A blocks which are crystalline at temperatures below about 60.degree. C. and separately providing di-, tri- or tetrafunctional hydroxyl terminated B blocks which are amorphous at temperatures above about -20.degree. C.,end-capping said A blocks by separately reacting said A blocks with a difunctional diisocyanate in which one isocyanate moiety is at least about five times as reactive with the terminal hydroxyl group of the A blocks as the other isocyanate moiety, whereby the more reactive isocyanate moiety tends to react with the terminal hydroxyl group of the A blocks, leaving the less reactive isocyanate moiety free and unreacted, andadding di-, tri- or tetrafunctional B block to the end-capped A blocks at approximately the stoichiometric ratios that they are intended to be present in the thermoplastic elastomer such that the free and unreacted isocyanate moiety on the end-capped A block reacts with a functional moiety of the B block to produce ABA or A.sub.n B thermoplastic elastomers.

    摘要翻译: 一种制备具有A嵌段和至少一个B嵌段的热塑性弹性体的方法,其中所述A嵌段在低于约60℃的温度下是结晶的,并且所述B嵌段在高于约-20℃的温度下是无定形的,所述A嵌段 各自为衍生自氧杂环丁烷及其衍生物和/或四氢呋喃及其衍生物的单体的聚醚,所述方法包括:提供在低于约60℃的温度下为结晶的单官能羟基封端的A嵌段,并分别提供二 - ,三 - 或四官能 羟基封端的B嵌段,其在高于约-20℃的温度下是无定形的,通过将所述A嵌段与双官能二异氰酸酯分开反应来封端所述A嵌段,其中一个异氰酸酯部分与末端羟基反应的至少约五倍 一组A嵌段作为另一异氰酸酯部分,由此更多的反应性异氰酸酯部分倾向于与A b的末端羟基反应 锁定,使较少反应性的异氰酸酯部分游离并未反应,并以其预期存在于热塑性弹性体中的化学计量比近似地将末端封端的A嵌段加入二官能,三官能或四官能团B嵌段, 并且封端的A嵌段上的未反应的异氰酸酯部分与B嵌段的官能部分反应以产生ABA或AnB热塑性弹性体。

    Gas generant compositions containing salts of 5-nitrobarbituric acid,
salts of nitroorotic acid, or 5-nitrouracil
    2.
    发明授权
    Gas generant compositions containing salts of 5-nitrobarbituric acid, salts of nitroorotic acid, or 5-nitrouracil 失效
    含有5-硝基巴比妥酸盐,硝基光油酸或5-硝基尿嘧啶盐的气体发生剂组合物

    公开(公告)号:US5015309A

    公开(公告)日:1991-05-14

    申请号:US347540

    申请日:1989-05-04

    CPC分类号: C06D5/06 C06B25/34

    摘要: Automotive airbag gas generant formulation providing alternative to commercially used formulations containing sodium azide. The composition comprises from about 25% to about 75% by weight of a heterocyclic compound having the following structure: ##STR1## wherein R is selected from hydrogen,--CO.sub.2 X, and--OXand X is a cation providing an anhydrous salt. The other principal ingredient of the composition is from about 25% to 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% to 2% 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.

    Hydrogenolysis of
2,4,6,8,10,12-Hexabenzyl-2,4,6,8,10,12-Hexaazatetracyclo�5.5.0.0.sup.5,9
.0.sup.3,11 !dodecane
    3.
    发明授权
    Hydrogenolysis of 2,4,6,8,10,12-Hexabenzyl-2,4,6,8,10,12-Hexaazatetracyclo�5.5.0.0.sup.5,9 .0.sup.3,11 !dodecane 失效
    2,4,6,8,10,12-六苄基-2,4,6,8,10,12-六氮杂四环[5.5.0.05,9.03,11]十二烷的氢解

    公开(公告)号:US5739325A

    公开(公告)日:1998-04-14

    申请号:US568451

    申请日:1995-12-07

    CPC分类号: C07D487/22

    摘要: A process for the hydrogenolysis of 2,4,6,8,10,12-hexabenzyl-2,4,6,8,10,12-hexaazatetracyclo�5.5.0.0.sup.5,9.0.sup.3,11 !dodecane ("HBIW") is disclosed. In the process, a quantity of HBIW, a cosolvent, and a bromine source are placed into a reaction vessel. Acetic anhydride and a palladium hydrogenolysis catalyst are rapidly added to the reaction vessel. The hydrogenolysis catalyst should be substantially free of water. The reaction vessel is purged of an atmosphere capable of reacting with hydrogen, and hydrogen is quickly introduced into the reaction vessel to convert the HBIW to tetraacetyldibenzylhexaazaisowurtzitane ("TADB"). The acetic anhydride is added immediately prior to hydrogen introduction so that the acetic anhydride does not have time to react with the HBIW to form an acetylated derivative prior to commencement of the desired hydrogenation reaction. The process requires very little palladium catalyst, preferably less than 10% wt/wt based on the HBIW substrate. The TADB, precipitated on the palladium hydrogenolysis catalyst, is subjected to a second hydrogenation step using a formic acid solvent in the presence of hydrogen to form tetraacetyldiformylhexaazaisowurtzitane ("TADF").

    摘要翻译: 公开了2,4,6,8,10,12-六苄基-2,4,6,8,10,12-六氮杂四环[5.5.0.05,9.03,11]十二烷(“HBIW”)的氢解方法 。 在此过程中,将一定数量的HBIW,共溶剂和溴源放入反应容器中。 将乙酸酐和钯氢解催化剂快速加入到反应容器中。 氢解催化剂应基本上不含水。 将反应容器吹扫出能够与氢反应的气氛,并将氢气快速地引入反应容器中,以将HBIW转化成四乙酰基二苄基六氮杂异纤锌矿型结构烷烃(“TADB”)。 在引入氢之前立即加入乙酸酐,使得乙酸酐在开始所需氢化反应之前没有时间与HBIW反应形成乙酰化衍生物。 该方法需要非常少的钯催化剂,优选基于HBIW底物小于10%wt / wt。 在钯氢解催化剂上沉淀的TADB在氢气存在下使用甲酸溶剂进行第二氢化步骤以形成四乙酰基全甲酰六氮杂异纤锌矿型结构烷烃(“TADF”)。

    Methods for controlled polymerization of energetic cyclic ethers using
alkylating salts
    4.
    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

    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。

    Synthesis of
4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.05,903,11]dode
cane
    5.
    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

    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。