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21. 发明授权

US4370204A Method for the purification of hexamethyldisiloxane 失效
标题翻译：六甲基二硅氧烷纯化方法
公开(公告)号：US4370204A
公开(公告)日：1983-01-25
申请号：US354466
申请日：1982-03-03
申请人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
IPC分类号： C07F7/20 , B01D3/36
CPC分类号： C07F7/20
摘要： Process for purifying hexamethyldisiloxane contaminated with toluene or other solvents that cannot be completely separated from the hexamethyldisiloxane by distillation, based on the discovery that hexamethyldisiloxane forms a previously unknown azeotrope with acetonitrile. This azeotrope has a heavier phase that is rich in acetonitrile and a lighter phase that is rich in hexamethyldisiloxane. These phases are mutually immiscible. The azeotrope starts to boil at 71.4.degree. C., which permits the hexamethyldisiloxane to be separated at relatively low temperatures from the impurities. The process involves one or more entrainment distillations in the presence of an excess of acetonitrile and the re-separation of the acetonitrile from the resulting lighter phase by distillation. Two further novel azeotropic systems, one consisting of hexamethyldisiloxane and toluene and the other of acetonitrile and toluene, are provided.
摘要翻译：基于六甲基二硅氧烷与乙腈形成先前未知的共沸物的发现，用于净化由甲苯或其它不能与六甲基二硅氧烷分离的其它溶剂的六甲基二硅氧烷的纯化方法。该共沸物具有富含乙腈的较重相和富含六甲基二硅氧烷的较轻相。这些阶段是互不混溶的。共沸物在71.4℃开始沸腾，这允许六甲基二硅氧烷在相对较低的温度下与杂质分离。该过程涉及在过量的乙腈存在下进行一次或多次夹带蒸馏，并通过蒸馏从所得更轻的相中重新分离乙腈。提供两个另外的新型共沸系统，一个由六甲基二硅氧烷和甲苯组成，另一个是乙腈和甲苯。

22. 发明授权

US4228092A Process for the preparation of organoalkoxysilanes 失效
标题翻译：制备有机烷氧基硅烷的方法
公开(公告)号：US4228092A
公开(公告)日：1980-10-14
申请号：US000605
申请日：1979-01-02
申请人： Hans-Joachim Kotzsch , Claus-Dietrich Seiler , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Claus-Dietrich Seiler , Hans-Joachim Vahlensieck
IPC分类号： C07F7/04 , C07F7/02 , C07F7/18
CPC分类号： C07F7/188 , C07F7/025
摘要： An improvement in a process for the esterification of a organochlorosilane by feeding alcohol into a chlorosilane maintained within a reaction zone without said alcohol contacting said chlorosilane in the gas phase wherein the esterification is performed stepwise with extraction of hydrogen chloride which has developed, the improvement which comprises employing in at least a final esterification step an organochlorosilane of the formulaH.sub.a R.sub.b SiCl.sub.4-a-bwhereinR represents an optionally halogen-substituted alkyl radical which can also contain an oxygen or sulfur atom in the chain, or a halogen or a NO.sub.2 group or a protected phenolic group containing aryl radical,a equals 0, 1, or 2,b equals 1 or 2, anda+b amounts to a maximum of 3,said final esterification step being performed with the addition of heat.
摘要翻译：通过将醇保持在反应区内的氯硅烷中而不使醇与气相中的氯代硅烷接触来改善有机氯代硅烷的酯化反应，其中通过萃取开发的氯化氢逐步进行酯化，其改进是包括在至少最终酯化步骤中使用式HaRbSiCl4-ab的有机氯硅烷，其中R表示任选的卤素取代的烷基，其还可以在链中含有氧或硫原子，或卤素或NO 2基团或被保护的含酚基的芳基，等于0,1或2，b等于1或2，a + b最多达3，所述最终酯化步骤是通过加热进行的。

23. 发明授权

US4049690A Method of preparing .beta.-chloroethyltrichlorosilane 失效
标题翻译：制备{62-氯乙基三氯硅烷的方法
公开(公告)号：US4049690A
公开(公告)日：1977-09-20
申请号：US636880
申请日：1975-12-02
申请人： Claus-Dieter Seiler , Hans-Joachim Vahlensieck
发明人： Claus-Dieter Seiler , Hans-Joachim Vahlensieck
IPC分类号： B01J27/00 , C07F7/12 , C07F7/08
CPC分类号： C07F7/127
摘要： An improved process for the hydrochlorination of vinyltrichlorosilane to prepare .beta.-chloroethyltrichlorosilane, which hydrochlorination is carried out by reacting the vinyltrichlorosilane with HCl in the presence of a Lewis catalyst, the improvement lying in carrying out the reaction at a temperature between 30.degree. and 65.degree. C, preferably at normal pressure.
摘要翻译：乙烯基三氯硅烷氢氯化以制备β-氯乙基三氯硅烷的改进方法，该氢氯化是通过在路易斯催化剂存在下使乙烯基三氯硅烷与HCl反应进行的，其中在30至65℃的温度下进行反应优选在常压下。

24. 发明授权

US4924021A Cyclic phenol organosilanes and method for their preparation 失效
标题翻译：环状苯酚有机硅烷及其制备方法
公开(公告)号：US4924021A
公开(公告)日：1990-05-08
申请号：US70258
申请日：1987-07-06
申请人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
IPC分类号： A01N55/00 , A01N55/10 , C07F7/04 , C07F7/14 , C07F7/18
CPC分类号： A01N55/00 , C07F7/045 , C07F7/14 , C07F7/1828
摘要： Disclosed are 2-silacoumaranes and their o-allylphenolsilane monoester precursors and methods for their preparation. The benzene ring of these new compounds may be substituted with halogen and/or alkyl or alkyl halogen moieties. The cyclization of monoester precursor to the desired end products is performed in the presence of catalysts. This cyclization can be performed without the isolation of the o-allyphenolsilane monoester by feeding by the cyclization reactor with the starting products for the preparation of this intermediate directly after they have reacted, or, if trichlorosilane is the starting product, directly after they have been mixed.Among other applications, the invention compounds are suitable for use as adhesion mediators and additives for coating compositions.
摘要翻译：公开了2-硅玉米烷及其O-烯丙基苯酚硅烷前体及其制备方法。这些新化合物的苯环可以被卤素和/或烷基或烷基卤素部分取代。在催化剂存在下，将单酯前体环化成所需的最终产物。这种环化可以在没有通过环化反应器进料的情况下进行，直接在它们已经反应后直接用于制备该中间体的起始产物，或者如果三氯硅烷是起始产物，则直接在它们已经被混合在其他应用中，本发明化合物适合用作涂料组合物的粘合介质和添加剂。

25. 发明授权

US4824979A Method for the preparation of partial esters and ortho esters of titanium, zirconium or hafnium 失效
标题翻译：钛，锆或铪的偏酯和原酸酯的制备方法
公开(公告)号：US4824979A
公开(公告)日：1989-04-25
申请号：US810514
申请日：1985-12-18
申请人： Hans-Joachim Kotzsch , Hans-Gunther Srebny , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Hans-Gunther Srebny , Hans-Joachim Vahlensieck
IPC分类号： C08F4/00 , C07F7/00 , C07F7/28 , C08F4/42 , C08F4/76 , C08G85/00
CPC分类号： C07F7/006
摘要： Disclosed is a new method for the preparation of metallic acid esters of titanium, zirconium or hafnium wherein a halide of the metal reacts with an organosilane ester, resulting in the formation of partial esters of the metallic acids. The degree of esterification of the metallic acid ester can be controlled based on the organosilane ester and it is possible to obtain complete esterification of the metal halides. The metallic acid partial esters prepared by the method are very pure, and can be separated selectively from the mixture in a simple manner. The metallic acid alkyl esters obtained can very easily be further esterified to the metallic acid tetraalkyl esters with the formation of very pure tetraalkyl esters.
摘要翻译：公开了一种制备钛，锆或铪的金属酸酯的新方法，其中金属的卤化物与有机硅烷酯反应，导致形成金属酸的偏酯。可以基于有机硅烷酯来控制金属酸酯的酯化程度，并且可以获得金属卤化物的完全酯化。通过该方法制备的金属酸偏酯是非常纯的，并且可以以简单的方式从混合物中选择性地分离。获得的金属酸性烷基酯可以非常容易地进一步酯化成金属酸四烷基酯，形成非常纯的四烷基酯。

26. 发明授权

US4609749A Method for the simultaneous preparation of carboxylic acid trimethylsilyl esters and silylated carboxylic acid amides 失效
标题翻译：同时制备羧酸三甲基甲硅烷基酯和甲硅烷基化羧酸酰胺的方法
公开(公告)号：US4609749A
公开(公告)日：1986-09-02
申请号：US800979
申请日：1985-11-22
申请人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
IPC分类号： B01J31/00 , C07B61/00 , C07F7/10 , C07F7/18
CPC分类号： C07F7/1896 , C07F7/10
摘要： Carboxylic acid trimethylsilyl esters (I) and trimethylsilyl carboxylic acid amides can be prepared simultaneously from the corresponding carboxylic acid anhydrides; the esters (I) and monocarboxylic acid trimethylsilyl amides are formed first and can then be recovered, or else the bis-trimethylsilyl carboxylic acid amides are formed by further transposition with trimethylchlorosilane in the presence of tertiary amines, and are separated from the carboxylic acid trimethylsilyl ester (I) and recovered.
摘要翻译：羧酸三甲基甲硅烷基酯（I）和三甲基甲硅烷基羧酸酰胺可以由相应的羧酸酐同时制备; 首先形成酯（I）和单羧酸三甲基甲硅烷基酰胺，然后可以回收，或者通过在叔胺存在下与三甲基氯硅烷进一步转置形成双三甲基甲硅烷基羧酸酰胺，并与羧酸三甲基甲硅烷基酯（I）并回收。

27. 发明授权

US4417067A Method of cleaving organosiloxanes 失效
标题翻译：裂解有机硅氧烷的方法
公开(公告)号：US4417067A
公开(公告)日：1983-11-22
申请号：US446756
申请日：1982-12-03
申请人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
IPC分类号： C07F7/12 , C07F7/08
CPC分类号： C07F7/123
摘要： The present invention relates to the cleavage of organosiloxanes with hydrogen chloride with the formation of organochlorosilanes. In accordance with the invention, this cleavage is performed at temperatures below 20.degree. C., and the dihydrates and trihydrates of the hydrogen chloride are formed. These settle as the specifically heavier, liquid phase and thus can easily be separated from the organochlorosilanes. The preferred temperature range in which the procedure of the invention is performed is between +10.degree. C. and -10.degree. C., while yields of as much as 99% of the desired organochlorosilane are obtained. The process can also be performed continuously.The inventive process is particularly useful because it can be used to convert contaminated organosiloxanes, such as used heat exchange or hydraulic oil materials, into useful products.
摘要翻译：本发明涉及在形成有机氯硅烷的情况下用氯化氢裂解有机硅氧烷。根据本发明，该切割在低于20℃的温度下进行，形成氯化氢的二水合物和三水合物。它们作为特别重的液相沉降，因此可以容易地与有机氯硅烷分离。进行本发明方法的优选温度范围为+10℃至-10℃，得到所需有机氯代硅烷的产率高达99％。该过程也可以连续执行。本发明的方法特别有用，因为它可以用于将受污染的有机硅氧烷，例如用过的热交换或液压油材料转化为有用的产品。

28. 发明授权

US4254270A Salt-like products of the addition of phenols onto amino organosilane esters and method for the preparation thereof 失效
标题翻译：将盐添加到氨基有机硅烷酯上的盐状产物及其制备方法
公开(公告)号：US4254270A
公开(公告)日：1981-03-03
申请号：US90715
申请日：1979-11-02
申请人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
IPC分类号： A01N55/00 , A01N55/10 , C07F7/18 , C07F7/10
CPC分类号： A01N55/00 , C07F7/182 , Y10S514/918
摘要： An adduct of phenol with an aminoorganosilane ester with salt-like charge-transfer-complex structure of the general formula ##STR1## wherein R represents an alkyl moiety of 1 to 8 carbon atoms or ethylene glycol or polyethylene glycol or propylene glycol or polypropylene glycol moieties terminally closed with a lower alkyl or acyl group;R' represent hydrogen or alkyl moieties having 1 to 20 carbon atoms optionally containing one or more ether bridges, a cycloalkyl moiety or an aryl moiety;R" represents alkyl with 1 to 8 carbon atoms;X represents halogen or C.sub.1-4 alkyl moieties or a nitro group;a being a value of 0 to 3;b a value of 0 to 5;c a value of 0 to 20; andn a value of 1 to 6; and a process for preparing the same.
摘要翻译：苯酚与具有通式为“IMAGE”的盐状电荷转移 - 复合结构的氨基有机硅烷酯的加合物，其中R表示1至8个碳原子的烷基部分或乙二醇或聚乙二醇或丙二醇或聚丙二醇部分用低级烷基或酰基末端封闭; R'表示氢或具有1至20个碳原子的烷基部分，任选地含有一个或多个醚桥，环烷基部分或芳基部分; R“表示具有1至8个碳原子的烷基; X表示卤素或C 1-4烷基部分或硝基; a为0到3的值; b值为0〜5; c值为0到20; n为1〜6的值。及其制备方法。

29. 发明授权

US4060536A Method of preparing N,N'-bis-trimethylsilylurea 失效
标题翻译：制备N，N {40-双 - 三甲基甲硅烷基脲的方法
公开(公告)号：US4060536A
公开(公告)日：1977-11-29
申请号：US746023
申请日：1976-11-30
申请人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
IPC分类号： C07F7/10 , B01J27/00 , B01J31/00 , C07B61/00 , C07D499/00 , C07D499/12
CPC分类号： C07D499/00
摘要： An improvement in a process for preparing N,N'-bis-trimethylsilylurea by reaction of urea with hexamethyldisilazane at an elevated temperature accompanied with ammonia evolution wherein the reaction is carried out in the presence of an acid catalyst.
摘要翻译：通过尿素与六甲基二硅氮烷反应制备N，N'-二 - 三甲基甲硅烷基脲的方法的改进，伴随氨释放，其中反应在酸催化剂存在下进行。

30. 发明授权

US4016188A Process for the preparation of low silanes and silane esters 失效
标题翻译：低硅烷和硅烷酯的制备方法
公开(公告)号：US4016188A
公开(公告)日：1977-04-05
申请号：US556994
申请日：1975-03-10
申请人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
发明人： Hans-Joachim Kotzsch , Hans-Joachim Vahlensieck
IPC分类号： C01B33/04 , C07F7/02 , C07F7/18 , C01B33/00 , C01B33/20
CPC分类号： C01B33/043 , C07F7/025
摘要： A process for preparing monosilane and low silane esters thereof which comprises contacting a hydrogen silane ester of the formula H.sub.x Si(OR).sub.4.sub.-x, wherein R represents an alkyl or alkoxyalkyl moiety and x is 1, 2 or 3, with a catalyst of an element of the first group and/or the second or third main or secondary group of the periodic system or iron or manganese or and organic nitrogen compound under distillation conditions and recovering a product having the formula H.sub.x.sub.+1 Si(OR).sub.4.sub.-x.sub.-1 and/or a product of the formula H.sub.x.sub.-1 Si(OR).sub.4.sub.-x.sub.+1.
摘要翻译：一种制备甲硅烷及其低硅烷酯的方法，其包括将式H x Si（OR）4-x的氢硅烷酯与其中R表示烷基或烷氧基烷基部分，x为1,2或3的氢硅烷酯与元素和/或周期系统的第二或第三主族或次基团或铁或锰或有机氮化合物在蒸馏条件下回收具有式Hx + 1Si（OR）4-x-1的产物和/或式Hx-1Si（OR）4-x + 1的产物。

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