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    • 4. 发明授权
    • Process for the preparation of acylated hexaazaisowurtzitane derivatives
    • 酰化六氮杂异纤锌矿型结构烷烃衍生物的制备方法
    • US6153749A
    • 2000-11-28
    • US214439
    • 1999-01-11
    • Tamotsu KodamaHaruyuki MinouraNobuhisa MiyakeSetsuo YamamatsuTsutomu Katsumata
    • Tamotsu KodamaHaruyuki MinouraNobuhisa MiyakeSetsuo YamamatsuTsutomu Katsumata
    • C07D487/18C07D487/22C07D259/00
    • C07D487/22
    • Disclosed is a method for producing an acyl group-containing hexaazaisowurtzitane derivative represented by the following formula (1),WA.sub.n H.sub.(6-n) (1)wherein n represents an integer of 4 or 6, each A independently represents an acyl group having 1 to 10 carbon atoms, H represents a hydrogen atom, and W represents a hexavalent hexaazaisowurtzitane residue represented by the following formula (2): ##STR1## which comprises: providing a composition system comprising a mixed solvent of a first solvent and a second solvent respectively having high and low dissolving abilities for the desired compound, wherein the mixed solvent has the desired compound dissolved therein; and removing the first solvent having a high dissolving ability from the composition system to thereby deposit crystals of the desired compound. The desired compound, which is useful as a precursor of high performance explosive additive, i.e., hexanitrohexaazaisowurtzitane, can be easily produced in high purity form in high yield and at low cost.
    • PCT No.PCT / JP97 / 03695 371日期1999年1月11日 102(e)1999年1月11日PCT PCT 1997年10月14日PCT公布。 第WO98 / 16529号公报 日期:1998年4月23日公开是制备由下式(1)表示的含酰基的六氮杂异纤锌矿型结构烷烃衍生物的方法WAnH(6-n)(1)其中n表示4或6的整数,A各自独立地表示 具有1至10个碳原子的酰基,H表示氢原子,W表示由下式(2)表示的六价六氮杂异纤锌矿型结构烷烃残基:其包括:提供包含第一溶剂和第二溶剂的混合溶剂的组合物体系 溶剂,分别具有所需化合物的高和低溶解能力,其中混合溶剂具有溶解在其中的所需化合物; 并从组合物体系中除去具有高溶解能力的第一溶剂,从而沉淀出所需化合物的晶体。 作为高性能炸药添加剂的前体,即六硝基六氮杂异纤锌矿型结构烷烃可以使用的所需化合物可以以高收率和低成本容易地以高纯度形式制备。
    • 5. 发明授权
    • Process for purification of polyether
    • 聚醚的纯化方法
    • US4677231A
    • 1987-06-30
    • US798249
    • 1985-11-08
    • Atsushi AoshimaSetsuo YamamatsuShoichiro Tonomura
    • Atsushi AoshimaSetsuo YamamatsuShoichiro Tonomura
    • C08G65/30C07C41/38C07C41/36
    • C08G65/30Y02P20/582
    • A process for purifying a polyalkylene ether, which comprises mixing a polyalkylene ether or a mixture of a polyalkylene ether and an organic solvent containing a heteropoly acid and/or its salt with at least one solvent for purification selected from hydrocarbons having 3 to 15 carbon atoms or halogenated hydrocarbons having 1 to 15 carbon atoms and separating by precipitation the phase composed mainly of the heteropoly acid and/or its salt, and a process wherein the polyalkylene ether or a mixture of a polyalkylene ether and an organic solvent containing a heteropoly acid and/or its salt is brought into contact with a solid adsorbent capable of adsorbing the heteropoly acid and/or its salt in the presence of at least one solvent for purification as described above, either further after the separation according to the process described above, or in the state unseparated.According to the present invention, the heteropoly acid and/or its salt dissolved in the polyalkylene ether or the mixture of the polyalkylene ether with the organic solvent can be removed efficiently in the form which can be reused. Further after the treatment with an adsorbent, the concentration of heteropoly acids in the polyalkylene ether can be reduced to extremely lower.
    • 一种纯化聚亚烷基醚的方法,其包括将聚亚烷基醚或含有杂多酸和/或其盐的有机溶剂的聚亚烷基醚或其混合物与选自具有3至15个碳原子的烃的至少一种纯化溶剂混合 或具有1至15个碳原子的卤代烃,并通过沉淀主要由杂多酸和/或其盐组成的相分离,以及其中聚亚烷基醚或聚亚烷基醚和含有杂多酸的有机溶剂的混合物和 /或其盐与固体吸附剂接触,所述固体吸附剂在至少一种如上所述的纯化溶剂存在下,可以在根据上述方法分离之后进一步吸附杂多酸和/或其盐,或 在状态未分离。 根据本发明,可以以可再利用的形式有效地除去溶解在聚亚烷基醚中的杂多酸和/或其盐或聚亚烷基醚与有机溶剂的混合物。 进一步用吸附剂处理后,聚亚烷基醚中杂多酸的浓度可以降低至极低。
    • 6. 发明授权
    • Method for acylating hexakis (arylmethyl) hexaazaisowurtzitane
    • 酰基化六(芳基甲基)六氮杂异纤锌矿型结构烷烃的方法
    • US06297373B1
    • 2001-10-02
    • US09508581
    • 2000-03-14
    • Tamotsu KodamaNaoko IshiharaHaruyuki MinouraNobuhisa MiyakeSetsuo Yamamatsu
    • Tamotsu KodamaNaoko IshiharaHaruyuki MinouraNobuhisa MiyakeSetsuo Yamamatsu
    • C07D48722
    • C07D487/22
    • A method for acylating a hexakis (arylmethyl) hexaazaisowurtzitane (WB6) by reductively removing the arylmethyl groups in the presence of an acylating agent, characterized by contacting a WB6 (a) with a heterogeneous system reduction catalyst (b) in the presence of an acylating agent (c) and a reducing agent (d) in a solvent (e) for the WB6 (a) to reductively remove the arylmethyl groups from the WB6 (a) and acylate the same, and by preventing the WB6 (a) and the catalyst (b) from being contacted with each other when at least either of the acylating agent (c) and the reducing agent (d) is not present. In this method, the decomposition of the WB6 skeleton, which readily occurs in the beginning of the acylation of the WB6 as a starting material, can be highly effectively inhibited. This method can hence stably produce a tetraacylhexaazaisowurtzitane derivative in a high yield and is industrially advantageous.
    • 一种通过在酰化剂存在下还原除去芳基甲基来酰化六(芳基甲基)六氮杂异纤锌矿型结构烷烃(WB6)的方法,其特征在于在酰化剂存在下使WB6(a)与异相体系还原催化剂(b)接触 用于WB6(a)的溶剂(e)中的试剂(c)和还原剂(d)从WB6(a)还原性除去芳基甲基并将其酰化,并通过防止WB6(a)和 当不存在酰化剂(c)和还原剂(d)中的至少任一种时,催化剂(b)彼此接触。 在该方法中,能够高效地抑制作为起始原料的WB6的酰化开始时容易发生的WB6骨架的分解。 因此,该方法可以高产率稳定地生产四酰基六氮杂异纤锌矿型结构烷烃衍生物,在工业上是有利的。
    • 7. 发明授权
    • Catalyst for use in producing carboxylic esters
    • 用于生产羧酸酯的催化剂
    • US6040472A
    • 2000-03-21
    • US945308
    • 1997-10-23
    • Setsuo YamamatsuTatsuo YamaguchiKoshiro Yokota
    • Setsuo YamamatsuTatsuo YamaguchiKoshiro Yokota
    • B01J21/14B01J23/62B01J29/44B01J29/48B01J35/00B01J37/00C07C67/39C07C69/74B01J31/00
    • C07C67/39B01J23/628B01J29/44B01J29/48B01J35/002B01J21/14B01J37/0045
    • Disclosed is a novel catalyst for use in producing a carboxylic ester from an aldehyde, an alcohol and molecular oxygen, which comprises a carrier having supported thereon Pd and Pb in a Pd/Pb atomic ratio (S) of 3/0.7.ltoreq.S.ltoreq.3/1.3, and which exhibits a maximum intensity peak at a diffraction angle (2.theta.) in the range of from 38.55.degree. to 38.70.degree. in a powder X-ray diffraction pattern thereof, wherein the peak is ascribed to the (111) crystal face diffraction of a Pd--Pb intermetallic compound. The catalyst can be efficiently produced by subjecting a catalyst precursor comprising a carrier having supported thereon a reducible Pd compound or a mixture of a reducible Pd compound and a reducible Pb compound to a reduction treatment in the presence of lead ions and at least one compound selected from a lower fatty acid, an alkali metal salt and an alkaline earth metal salt, or by subjecting a catalyst prepared by a conventional method, which comprises a carrier having supported thereon Pd or a mixture of Pd and Pb, to an activation treatment. By using the catalyst, the desired carboxylic ester can be produced with high selectivity, while suppressing the formation of by-products, even under high temperature and high aldehyde concentration conditions. Further, in the continuous production of a carboxylic ester using the catalyst, stabilization of the catalyst can be effectively performed, so that a desired carboxylic ester can be stably produced with high efficiency and in high yield for a prolonged period of time.
    • PCT No.PCT / JP96 / 02008 Sec。 371日期:1997年10月23日 102(e)1997年10月23日PCT PCT 1996年7月18日PCT公布。 公开号WO97 / 03751 日期1997年2月6日公开是一种用于从醛,醇和分子氧生产羧酸酯的新型催化剂,其包含负载Pd / Pb原子比(S)为3 / 0.7
    • 8. 再颁专利
    • Catalyst for use in producing carboxylic esters
    • 用于生产羧酸酯的催化剂
    • USRE38283E1
    • 2003-10-21
    • US10101252
    • 2002-03-20
    • Setsuo YamamatsuTatsuo YamaguchiKoshiro Yokota
    • Setsuo YamamatsuTatsuo YamaguchiKoshiro Yokota
    • C07C6974
    • C07C67/39B01J21/14B01J23/628B01J29/44B01J29/48B01J35/002B01J37/0045C07C69/54
    • Disclosed is a novel catalyst for use in producing a carboxylic ester from an aldehyde, an alcohol and molecular oxygen, which comprises a carrier having supported thereon Pd and Pb and a Pd/Pb atomic ratio (S) of 3/0.7≦S≦ from 3/0.7 to 3/1.3, and which exhibits a maximum intensity peak at a diffraction angle (2&thgr;) in the range of from 38.55° to 38.70° in a power X-ray diffraction pattern thereof, wherein the peak is ascribed to the (111) crystal face diffraction of a Pd—Pb intermetallic compound. The catalyst can be efficiently produced by subjecting a catalyst precursor comprising a carrier having supported thereon a reducible Pd compound or a mixture of a reducible Pd compound and a reducible Pb component to a reduction treatment in the presence of lead ions and at least one compound selected from a lower fatty acid, an alkali metal salt and an alkaline earth metal salt, or by subjecting a catalyst prepared by a conventional method, which comprises a carrier having supported thereon Pd or a mixture of Pd and Pb, to an activation treatment. By using the catalyst, the desired carboxylic ester can be produced with high selectivity, while suppressing the formation of by-products, even under high temperature and high aldehyde concentration conditions. Further, in the continuous production of a carboxylic ester using the catalyst, stabilization of the catalyst can be effectively performed, so that a desired carboxylic ester can be stably produced with high efficiency and in high yield for a prolonged period of time.