Process for 4-sulfonamidolphenyl hydrazines
    1.
    发明授权
    Process for 4-sulfonamidolphenyl hydrazines 失效
    4-磺酰氨基苯基肼的方法

    公开(公告)号:US6011177A

    公开(公告)日:2000-01-04

    申请号:US978965

    申请日:1997-11-26

    IPC分类号: C07C303/40 C07C311/39

    CPC分类号: C07C303/40

    摘要: 4-Sulfonamidophenyl hydrazines are prepared by reaction between the hydrazine, optionally substituted, and the corresponding 4-substituted benzenesulfonamides, where the 4-substitution is an appropriate leaving group, in the presence of water and the absence of dimethyl sulfoxide as a solvent. The result is a product of unusually high purity.

    摘要翻译: 通过在任选取代的肼和相应的4-取代的苯磺酰胺(其中4-取代是合适的离去基团)在水和不存在二甲基亚砜作为溶剂的条件下反应来制备4-磺酰胺基苯肼。 结果是异常高纯度的产品。

    Large scale batch process for diazomethane
    2.
    发明授权
    Large scale batch process for diazomethane 失效
    重氮甲烷的大规模批量处理

    公开(公告)号:US5817778A

    公开(公告)日:1998-10-06

    申请号:US970035

    申请日:1997-11-13

    CPC分类号: C07C245/16

    摘要: Diazomethane is prepared in a batch process on a scale of at least 50 gram-moles per batch, from an N-methyl-N-nitroso amine in an organic solvent and an inorganic base in an aqueous solution by the use of a phase transfer catalyst and by controlling the choice of solvent, reagent concentrations, addition rate and reaction temperature to cause codistillation of the product and the organic solvent in such a manner that the concentration of diazomethane in both liquid and vapor phases are controlled within limits that will prevent detonation of the diazomethane.

    摘要翻译: 重氮甲烷以分批方法制备,每批至少50克摩尔的量级,由有机溶剂中的N-甲基-N-亚硝基胺和水溶液中的无机碱通过使用相转移催化剂 并通过控制溶剂的选择,试剂浓度,加入速率和反应温度来引起产物和有机溶剂的共蒸馏,使液相和汽相中重氮甲烷的浓度控制在防止爆炸的范围内 重氮甲烷。

    Continuous process for diazomethane from an n-methyl-n-nitrosoamine and
from methylurea through n-methyl-n-nitrosourea
    3.
    发明授权
    Continuous process for diazomethane from an n-methyl-n-nitrosoamine and from methylurea through n-methyl-n-nitrosourea 失效
    从正甲基 - 正 - 亚硝基胺和甲基脲到正甲基 - 正 - 亚硝基脲的重氮甲烷的连续方法

    公开(公告)号:US5854405A

    公开(公告)日:1998-12-29

    申请号:US969993

    申请日:1997-11-13

    IPC分类号: C07C245/16 C07C245/12

    CPC分类号: C07C245/16

    摘要: Diazomethane is produced in a continuous process with little or no explosion hazard, by dissolving an N-methyl-N-nitroso amine in a mixture of a water-miscible organic solvent that dissolves the N-methyl-N-nitroso amine and a water-immiscible organic solvent that dissolves diazomethane, and combining a stream of this solution with a stream of an aqueous inorganic base, allowing the aqueous and organic phases to settle after a suitable residence time, and phase separating the phases, all on a continuous basis. When using N-methyl-N-nitrosourea as the amine, the diazomethane process is preceded by a continuous nitrosation process involving combining aqueous solutions of methyl urea and a nitrite salt with an organic solution of a mineral or organic acid, the solvent in the organic solution being a mixture of the two organic solvents referred to above, allowing the aqueous and organic phases to settle after a suitable residence time, and phase separating the phases, all on a continuous basis. The resulting organic phase is continuously fed to the diazomethane stages described above.

    摘要翻译: 通过将N-甲基-N-亚硝基胺溶解在溶解N-甲基-N-亚硝基胺的水混溶性有机溶剂和水溶性有机溶剂的混合物中,以几乎没有或没有爆炸危险的连续方法生产重氮甲烷, 溶解重氮甲烷的不混溶的有机溶剂,并将该溶液的流与无机碱水溶液混合,使水相和有机相在合适的停留时间后沉降,并相分离所有相。 当使用N-甲基-N-亚硝基脲作为胺时,重氮甲烷工艺之前是连续的亚硝化方法,其中包括将甲基脲和亚硝酸盐的水溶液与有机溶液或无机酸有机溶液结合,有机溶剂 溶液是上述两种有机溶剂的混合物,允许水相和有机相在合适的停留时间后沉降,并且相分离所有相,全部在连续的基础上。 将所得有机相连续进料至上述重氮甲烷级。

    3-Azidomethyl-3-nitratomethyloxetane
    5.
    发明授权
    3-Azidomethyl-3-nitratomethyloxetane 失效
    3-叠氮基甲基-3-硝基甲基氧杂环丁烷

    公开(公告)号:US5489700A

    公开(公告)日:1996-02-06

    申请号:US469329

    申请日:1995-06-05

    CPC分类号: C08G65/22 C07D305/06

    摘要: 3-Azidomethyl-3-nitratomethyloxetane, a novel oxetane compound, is used as a monomer for the formation of homopolymers and copolymers with other known energetic oxetane monomers. The polyethers of the present invention can be subsequently cured to form elastomers suitable for use as energetic binders in propellant formulations or the like.

    摘要翻译: 3-叠氮基甲基-3-硝基甲基氧杂环丁烷是新型的氧杂环丁烷化合物,用作与其它已知的能量大的氧杂环丁烷单体形成均聚物和共聚物的单体。 本发明的聚醚可随后固化以形成适合用作推进剂配方等中的高能粘合剂的弹性体。

    Polymerization of energetic, cyclic ether monomers using boron
trifluoride tetrahydrofuranate
    6.
    发明授权
    Polymerization of energetic, cyclic ether monomers using boron trifluoride tetrahydrofuranate 失效
    使用三氟化硼四氢化物聚合能量较高的环醚单体

    公开(公告)号:US5468841A

    公开(公告)日:1995-11-21

    申请号:US226919

    申请日:1994-04-13

    IPC分类号: C08G65/22

    CPC分类号: C08G65/22

    摘要: The present invention provides an improved method of carrying out cationic polymerization of cyclic ether monomers substituted with high-energy, electron-withdrawing pendant groups (e.g., BAMO and NMMO). Such cyclic ether monomers are polymerized with an initiator precursor (i.e., an alcohol) and boron trifluoride tetrahydrofuranate (BF.sub.3 .cndot.THF). It has been discovered that when boron trifluoride tetrahydrofuranate is used as a catalyst in the cationic polymerization of cyclic ether monomers substituted with high-energy, electron-withdrawing pendant groups (e.g., BAMO and NMMO), polymers are produced that have improved functionality and low poly-dispersity. The polymers formed using the method of the present invention are useful for forming cross-linked elastomers which, in turn, are useful for forming elastomeric binders for high-energy compositions, such as propellants, explosives, gasifiers or the like.

    摘要翻译: 本发明提供了用高能吸电子侧基(例如BAMO和NMMO)取代的环醚单体进行阳离子聚合的改进方法。 这种环醚单体与引发剂前体(即醇)和三氟化硼四氢硼酸酯(BF 3,THF)聚合。 已经发现,当用高能吸电子侧基(例如BAMO和NMMO)取代的环醚单体的阳离子聚合中使用四氟化硼作为催化剂时,产生具有改进的官能度和低的聚合物 多分散性 使用本发明的方法形成的聚合物可用于形成交联的弹性体,其又可用于形成用于高能组合物的弹性体粘合剂,例如推进剂,爆炸物,气化器等。

    Polyfluorinated, branched-chain diols and diisocyanantes and fluorinated
polyurethanes prepared therefrom
    7.
    发明授权
    Polyfluorinated, branched-chain diols and diisocyanantes and fluorinated polyurethanes prepared therefrom 失效
    由其制备的多氟,支链二醇和二异氰酸酯和氟化聚氨酯

    公开(公告)号:US5204441A

    公开(公告)日:1993-04-20

    申请号:US491972

    申请日:1990-03-12

    摘要: Branched-chain diols and a method of forming them by reacting 1,4-diiodoperfluorobutane and perfluoropropylene to obtain branched-chain diiodide adducts thereof, reacting the diiodide adducts with ethylene to obtain I--CH.sub.2 CH.sub.2 --R--CH.sub.2 CH.sub.2 --I, wherein R is a branched-chain perfluoroalkyl radical, and hydrolysing the iodo groups to alcohols to obtain HO--CH.sub.2 CH.sub.2 --R--CH.sub.2 CH.sub.2 --OH. These diols can be reacted with branched-chain diisocyanates to form polyurethanes of better processability and lower glass transition temperatures than polyurethanes prepared from linear fluorinated monomers.

    摘要翻译: 支链二醇和通过1,4-二碘全氟丁烷和全氟丙烯反应形成它们的方法,得到其支链二碘化物加合物,使二碘化物加合物与乙烯反应,得到I-CH 2 CH 2 -R-CH 2 CH 2 -I,其中R为 支链全氟烷基,并将碘基水解成醇,得到HO-CH 2 CH 2 -R-CH 2 CH 2 -OH。 这些二醇可以与支链二异氰酸酯反应形成与由线性氟化单体制备的聚氨酯相比具有更好加工性和较低玻璃化转变温度的聚氨酯。

    1,3-diethynyladamantane and methods of polymerization thereof
    8.
    发明授权
    1,3-diethynyladamantane and methods of polymerization thereof 失效
    1,3-二乙炔基金刚烷及其聚合方法

    公开(公告)号:US4918158A

    公开(公告)日:1990-04-17

    申请号:US887219

    申请日:1986-07-21

    IPC分类号: C07C1/30 C07C13/615 C07C17/32

    摘要: 1,3-Diethynyladamantane and a method of forming same by brominating adamantane to yield 1,3-dibromoadamantane, subjecting vinyl bromide to Friedel-Crafts alkylation with the 1,3-dibromoadamantane to form 1,3-bis(2,2-dibromoethyl)adamantane and subjecting the 1,3-bis(2,2-dibromoethyl)adamantane to dehydrohalogenation to yield the 1,3-diethynyladamantane. 1,3-Diethynyladamantane can be polymerized to produce strong, thermally stable resins suitable for advanced aerospace structural applications, as matrices for carbon-carbon systems and as electrical insulators. It can also be copolymerized with 1-ethynyladamantane to yield similarly useful resins.

    摘要翻译: 1,3-丁二炔基金刚烷及其形成方法,通过溴化金刚烷得到1,3-二溴金刚烷,用1,3-二溴金刚烷对溴化乙烯进行Friedel-Crafts烷基化,形成1,3-双(2,2-二溴乙基 )金刚烷,并使1,3-双(2,2-二溴乙基)金刚烷脱卤化氢,得到1,3-二乙炔基金刚烷。 1,3-二乙炔基金刚烷可以被聚合以产生适合于先进航空航天结构应用的强的,热稳定的树脂,作为碳 - 碳体系和电绝缘体的基质。 它也可以与1-乙炔基金刚烷共聚以产生类似有用的树脂。

    Fluorinated thermoset polyurethane elastomers prepared from polyether prepolymers formed from mono-substituted fluorinated oxetane monomers
    9.
    发明授权
    Fluorinated thermoset polyurethane elastomers prepared from polyether prepolymers formed from mono-substituted fluorinated oxetane monomers 有权
    由由单取代的氟代氧杂环丁烷单体形成的聚醚预聚物制备的氟化热固性聚氨酯弹性体

    公开(公告)号:US07354985B2

    公开(公告)日:2008-04-08

    申请号:US10678663

    申请日:2003-10-03

    IPC分类号: C08G18/28 C07D305/00

    摘要: This application is directed to novel fluorinated polymers and prepolymers derived from mono-substituted oxetane monomers having fluorinated alkoxymethylene side-chains and the method of making these compositions. The mono-substituted fluorinated oxetane monomers having fluorinated alkoxymethylene side-chains are prepared in high yield by the reaction of a fluorinated alkoxides with either 3-halomethyl-3-methyloxetane premonomers or aryl sulfonate derivative of 3-hydroxymethyl-3-methyloxetane premonomers. Preparation of a mono-substituted 3-bromomethyl-3-methyloxetane premonomer via a simple, high yield process amenable to commercial scaleup is also disclosed. The fluorinated oxetane monomers of this invention can be readily homo/co-polymerized in the presence of a Lewis acid and polyhydroxy compounds to obtain hydroxy-terminated polyether prepolymers having fluorinated alkoxymethylene side chains. Additionally, the fluorinated oxetane monomers can be copolymerized with non-fluorinated monomers such as tetrahydrofuran to give polyether prepolymers with improved hydrocarbon compatibility. These prepolymers are polydisperse and exhibit number average molecular weights from 5,000 to about 50,000. These prepolymers are amorphous oils with primary hydroxy end-groups and thus function efficiently as the soft block for the synthesis of a variety of thermoset/thermoplastic elastomers and plastics having the characteristics of very low surface energy, high hydrophobicity, low glasss transition temperature and low coefficient of friction. The polyurethanes derived from the prepolymers of this invention are elastomeric and, in addition to the above characteristics, exhibit high moisture resistance, high tear strength and excellent adhesion to a variety of substrates.

    摘要翻译: 本申请涉及由具有氟化烷氧基亚甲基侧链的单取代的氧杂环丁烷单体衍生的新的氟化聚合物和预聚物以及制备这些组合物的方法。 具有氟化烷氧基亚甲基侧链的单取代氟化氧杂环丁烷单体通过氟化烷氧化物与3-卤代甲基-3-甲基氧杂环丁烷预先单体或3-羟甲基-3-甲基氧杂环丁烷预先单体的芳基磺酸酯衍生物的反应以高收率制备。 还公开了通过易于商业化的简单高产率工艺制备单取代的3-溴甲基-3-甲基环氧乙烷预先单体。 本发明的氟化氧杂环丁烷单体可以在路易斯酸和多羟基化合物的存在下容易地均相/共聚,得到具有氟化烷氧基亚甲基侧链的羟基封端的聚醚预聚物。 此外,氟化氧杂环丁烷单体可以与非氟化单体如四氢呋喃共聚,得到具有改进的烃相容性的聚醚预聚物。 这些预聚物是多分散体,其数均分子量为5,000至约50,000。 这些预聚物是具有初级羟基端基的无定形油,因此作为用于合成各种具有非常低的表面能,高疏水性,低玻璃化转变温度和低的特性的各种热固性/热塑性弹性体和塑料的软块有效地起作用 摩擦系数。 衍生自本发明的预聚物的聚氨酯是弹性体的,并且除了上述特征之外,还显示出高耐湿性,高撕裂强度和对各种基材的优异粘合性。