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    • 1. 发明授权
    • Process for producing aromatic hydroxylic compound
    • 制备芳香族羟基化合物的方法
    • US5475157A
    • 1995-12-12
    • US256245
    • 1994-09-02
    • Shintaro ArakiHiroshi IwasakiHiroyasu OhnoIsao HashimotoTeruaki Mukaiyama
    • Shintaro ArakiHiroshi IwasakiHiroyasu OhnoIsao HashimotoTeruaki Mukaiyama
    • C07C37/08C07C45/53
    • C07C37/08Y02P20/52
    • There is disclosed a process for producing an aromatic hydroxylic compound by acid decomposition of a hydroperoxide having the general formula (I) ##STR1## wherein Ar represents an aromatic hydrocarbon group having a valence of n; and n represents an integer of 1 or 2, in the presence of an acid catalyst, thereby to provide an aromatic hydroxylic compound having the general formula (II)Ar--(OH)n (II)wherein Ar and n are the same as above defined, characterized in that tetrafluoroboric acid, hexafluorosilicic acid or hexafluorophosphoric acid is used as the acid catalyst. According to this process, the aromatic hydroxylic compound is obtained in a high yield while the by-production of hydroxyacetone is effectively suppressed. In paricular, a more effective suppression of by-production of hydroxyacetone and a higher yield of the target compound can be achieved by carrying out the acid decomposition reaction in two stages wherein the first stage of the reaction is carried out in the first reactor at a temperature of 50.degree.-95.degree. C., the resultant reaction mixture is sent to the second reactor, and the second stage of the reaction is then carried out in the second reactor at a temperature of 80.degree.-120.degree. C.
    • PCT No.PCT / JP93 / 01586 Sec。 371日期:1994年9月2日 102(e)1994年9月2日PCT 1993年11月1日PCT公布。 公开号WO94 / 10115 PCT 日本公报1994年5月11日。公开了通过酸分解具有通式(I)c的化合价n为n的烃基的氢过氧化物制备芳族羟基化合物的方法。 并且n表示1或2的整数,在酸催化剂的存在下,由此提供具有通式(II)的Ar-(OH)n(II)的芳族羟基化合物,其中Ar和n与上述相同 其特征在于使用四氟硼酸,六氟硅酸或六氟磷酸作为酸催化剂。 根据该方法,以高产率获得芳族羟基化合物,同时有效抑制羟基丙酮的副产物。 在这种情况下,可以通过在两个阶段中进行酸分解反应来实现对羟基丙酮的副产物的更有效抑制和目标化合物的较高产率,其中反应的第一阶段在第一反应器中以 温度为50-95℃,将所得反应混合物送至第二反应器,然后在第二反应器中在80-120℃的温度下进行第二阶段反应。
    • 4. 发明授权
    • Process for preparing N,O-dialkylhydroxylamine, its salts or
intermediates in their synthesis
    • 在其合成中制备N,O-二烷基羟胺,其盐或中间体的方法
    • US5510511A
    • 1996-04-23
    • US97225
    • 1993-07-27
    • Satoshi InokiMitsuyuki TakesueIsao HashimotoNoriaki KiharaKiyoaki Sugi
    • Satoshi InokiMitsuyuki TakesueIsao HashimotoNoriaki KiharaKiyoaki Sugi
    • C07C239/20C07C271/12C07C261/00
    • C07C271/12C07C239/20
    • A process for preparing N,O-dialkylhydroxycarbamic acid ester which comprises reacting hydroxylamine or its salt with dihydrocarbyl carbonate in the presence of a basic compound to prepare hydroxycarbamic acid ester and subsequently alkylating this compound with an alkylating agent; a process for recovering N,O-dialkylhydroxycarbamic acid ester which comprises azeotropically distilling the ester with water from a solution containing the ester; a process for preparing N,O-dialkylhydroxylamine which comprises hydrolyzing N,O-dialkylhydroxycarbamic acid ester in an aqueous solution or a hydrous solvent in the presence of an alkali; a process for purifying N,O-dialkylhydroxylamine hydrochloride which comprises adding aldehyde or ketone to a solution of N,O-dialkylhydroxylamine hydrochloride containing O-alkylhydroxylamine hydrochloride as impurities to convert the O-alkylhydroxylamine hydrochloride into O-alkyl aldoxime or O-alkyl ketoxime and subsequently separating the N,O-dialkylhydroxylamine hydrochloride from the reaction system; and a process for separating N,O-dialkylhydroxylamine hydrochloride which comprises (i) adding benzene or alkylated benzene to an aqueous solution containing N,O-dialkylhydroxylamine hydrochloride, azeotropically removing water or a hydrochloride solution, and, subsequently (ii)adding alcohol thereto to obtain N,O-dialkylhydroxylamine hydrochloride in the form of crystal.
    • 一种制备N,O-二烷基羟基氨基甲酸酯的方法,其包括使羟胺或其盐与二烃基碳酸酯在碱性化合物的存在下反应以制备羟基氨基甲酸酯,随后用烷基化剂烷基化该化合物; 一种回收N,O-二烷基羟基氨基甲酸酯的方法,该方法包括从含有酯的溶液中用水共沸蒸馏该酯; 一种制备N,O-二烷基羟胺的方法,其包括在碱存在下水溶液或含水溶剂中N,O-二烷基羟基氨基甲酸酯水解; 一种纯化N,O-二烷基羟胺盐酸盐的方法,其包括将醛或酮加入到含有O-烷基羟胺盐酸盐的N,O-二烷基羟胺盐酸盐的溶液中作为杂质,以将O-烷基羟胺盐酸盐转化为O-烷基羟基肟或O-烷基酮肟 随后从反应体系中分离出N,O-二烷基羟胺盐酸盐; 以及分离N,O-二烷基羟胺盐酸盐的方法,其包括(i)将苯或烷基化苯加入到含有N,O-二烷基羟胺盐酸盐的水溶液中,共沸除去水或盐酸盐溶液,随后(ii)向其中加入醇 得到晶体形式的N,O-二烷基羟胺盐酸盐。
    • 9. 发明授权
    • Vertical roller mill
    • 立式辊磨机
    • US4679739A
    • 1987-07-14
    • US745287
    • 1985-06-14
    • Isao HashimotoTosuke KinoshitaMasahiro UchidaSusumu Uchiyama
    • Isao HashimotoTosuke KinoshitaMasahiro UchidaSusumu Uchiyama
    • B02C15/00B02C15/04
    • B02C15/04B02C15/004
    • A roller mill according to this invention includes a base and a table supported on the base, the table being adapted to be rotated on a generally vertical axis. The table has an annular groove formed in its top surface, the groove having a semicircular cross section. At least one roller is supported by the base above the table, each roller being rotatable on an axis which intersects with the vertical axis of the table. Each roller has an arcuate peripheral portion which forms part of a circle of curvature in cross section. The roller and the table rotate on their respective axes, and they are adapted to compress and mill material in the groove betweem them, a clearance which receives the material being formed between the peripheral portion of the roller and the groove. The roller has a wider axial dimension on the side which is inward radially of the table from a radial plane of the roller, this plane passing through the center of the circle of the peripheral part of the roller, than the axial dimension on the outward side of the table.
    • 根据本发明的辊磨机包括底座和支撑在基座上的工作台,该工作台适于在大致垂直的轴线上旋转。 该工作台具有形成在其顶表面上的环形槽,该槽具有半圆形横截面。 至少一个辊子由桌子上方的基座支撑,每个辊子可在与桌子的垂直轴线相交的轴线上旋转。 每个辊具有弓形周边部分,其形成横截面为曲率圆的一部分。 辊子和工作台在其各自的轴线上旋转,并且它们适于压缩和磨碎它们之间的槽中的材料,该间隙容纳形成在辊的周边部分和槽之间的材料。 滚子在从滚子的径向平面向内径向延伸的一侧具有较宽的轴向尺寸,该平面通过滚子周边部分圆的中心,而不是在外侧的轴向尺寸 的表。
    • 10. 发明授权
    • Process for preparation of aromatic hydroperoxides
    • 芳香族氢过氧化物的制备方法
    • US4267387A
    • 1981-05-12
    • US85587
    • 1979-10-17
    • Ichiro ImaiIsao HashimotoKeiji SuzukiHiroaki Nakagawa
    • Ichiro ImaiIsao HashimotoKeiji SuzukiHiroaki Nakagawa
    • C07C67/00C07C407/00C07C409/08C07C179/035
    • C07C409/08C07C407/00
    • An improved process for the preparation of an aromatic hydroperoxide by oxidizing a hydroxyalkyl-substituted aromatic compound having at least one hydroxyalkyl group directly bonded to an aromatic ring carbon of the aromatic compound and being represented by the formula ##STR1## wherein R.sub.1 and R.sub.2 each are a lower alkyl group, with hydrogen peroxide in the presence of an acid catalyst in a heterogeneous system of a water-immiscible inert aromatic hydrocarbon solvent at a reaction temperature of up to about 70.degree. C. while removing by-product water as an azeotrope with the aromatic hydrocarbon solvent in the oxidation system; characterized in that said oxidation is carried out while feeding a vapor of a water-immiscible inert aromatic hydrocarbon solvent having a temperature higher than the reaction temperature but not exceeding about 90.degree. C. into a liquid phase of the oxidation system.
    • 通过氧化具有至少一个羟基烷基的羟烷基取代的芳族化合物来制备芳香族氢过氧化物的改进方法,所述羟烷基取代的芳族化合物直接与芳香族化合物的芳香环碳键合,并且由式(I)表示,其中R 1和R 2各自为 低级烷基与过氧化氢在酸性催化剂存在下在水不混溶惰性芳烃溶剂的异相体系中反应温度高达约70℃,同时除去副产物水作为共沸物, 氧化体系中的芳烃溶剂; 其特征在于,在将温度高于反应温度但不超过约90℃的与水不混溶的惰性芳族烃溶剂的蒸气进料到氧化系统的液相中的同时进行所述氧化。