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1. 发明授权

US4397791A Process for reacting alcohols and/or phenols with phosphorus pentasulfide 失效
标题翻译：醇和/或酚与五硫化二磷反应的方法
公开(公告)号：US4397791A
公开(公告)日：1983-08-09
申请号：US243613
申请日：1981-03-13
申请人： Werner Krause , Jurgen Grosse , Werner Klose
发明人： Werner Krause , Jurgen Grosse , Werner Klose
IPC分类号： C07F9/165 , B01J31/00 , B01J31/02 , C07B61/00 , C07F9/17 , C07F9/18
CPC分类号： C07F9/17 , C07F9/18
摘要： The invention relates to a process wherein an alcohol and/or phenol is reacted with phosphorus pentasulfide in the presence of a catalyst which is selected from(a) phosphonium salts of the general formula: ##STR1## (b) ammonium salts of the general formula: ##STR2## (c) phosphine oxides of the general formula: ##STR3## (d) phosphine sulfides of the general formula: ##STR4## (e) phosphinic acid derivatives of the general formula: ##STR5## In formulae I through V, the substituents R.sub.1, R.sub.2, R.sub.3 and R.sub.4 each stand for identical or different alkyl-, aryl-, alkaryl- or aralkyl- groups having from 1 to 22 carbon atoms. A stands for an inorganic or organic acid, and X and Y, respectively, stand for both oxygen and sulfur, and M stands for a monovalent metal or oxygen.
摘要翻译：本发明涉及一种方法，其中醇和/或苯酚与五硫化二磷在催化剂存在下反应，所述催化剂选自（a）通式鏻的盐：（b）一般的铵盐 II（c）以下通式的氧化膦：（a）下列通式的膦硫化物：（e）下列通式的次膦酸衍生物：式I至V中，取代基R 1，R 2，R 3和R 4各自代表具有1至22个碳原子的相同或不同的烷基 - ，芳基 - ，烷芳基 - 或芳烷基 - 基团。 A代表无机或有机酸，X和Y分别代表氧和硫，M代表一价金属或氧。

2. 发明授权

US4834960A Process for purifying phosphorous acid 失效
标题翻译：纯化亚磷酸的方法
公开(公告)号：US4834960A
公开(公告)日：1989-05-30
申请号：US182871
申请日：1988-04-18
申请人： Jurgen Grosse , Gunther Schimmel , Bernhard Hofmann
发明人： Jurgen Grosse , Gunther Schimmel , Bernhard Hofmann
IPC分类号： C01B25/163
CPC分类号： C01B25/163
摘要： The purification of phosphorous acid which is formed in halogenations of hydrocarbon derivatives using phosphorus trihalides is carried out in the context of preparing phosphorous acid in a reaction zone by reacting a mixture of phosphorus trichloride and water which has been finely divided by means of steam at temperatures between 150.degree. and 200.degree. C. in the gas phase. In this process, the liquid reaction product drains into a concentrating evaporation zone which has a downstream first separation zone. Inert gas is introduced to the lower part of the first separation zone. A melt is withdrawn from the first separation zone into a crystallizing zone. The waste gases from the reaction zone are treated with a washing liquid in a second separation zone before being passed into the atmosphere. The washing liquid used is an aqueous solution of never-purified phosphorous acid, which can have been prepurified by hydrolysis and stripping.
摘要翻译：通过使用三卤化磷在烃衍生物的卤化中形成的亚磷酸的纯化是在反应区中通过使三氯化磷和水分混合物在蒸气中分解的温度反应在反应区中进行的在气相中为150〜200℃。在该方法中，液体反应产物排入具有下游第一分离区的浓缩蒸发区。惰性气体被引入第一分离区的下部。将熔体从第一分离区取出成结晶区。来自反应区的废气在通入大气中之前用洗涤液在第二分离区中处理。所使用的洗涤液是未经纯化的亚磷酸的水溶液，其可以通过水解和汽提进行预净化。

3. 发明授权

US4728443A Textile softening detergent composition 失效
标题翻译：纺织软化洗涤剂组合物
公开(公告)号：US4728443A
公开(公告)日：1988-03-01
申请号：US725376
申请日：1985-04-22
申请人： Hans-Peter Rieck , Jurgen Grosse , Werner Gohla
发明人： Hans-Peter Rieck , Jurgen Grosse , Werner Gohla
IPC分类号： C11D3/12 , D06M11/00
CPC分类号： C11D3/1273 , C11D3/124
摘要： A textile softening detergent composition contains from 5 to 70 wgt % surfactant, from 0.5 to 50 wgt % builder, from 1 to 20 wgt % crystalline laminated silicic acid and/or a corresponding alkali metal silicate and standard detergent aids. It is characterized in that the crystalline laminated silicic acid or its alkali metal salt of the general formulaM.sub.2 Si.sub.x O.sub.2x+1 .multidot.y H.sub.2 Oin which x stands for a number larger than 7.0, M stands for sodium, potassium or hydrogen, and y stands for a number of from 0 to 25, shows one or more reflexes unassignable to quartz, tridymite and cristobalite in the X-ray diffraction diagram in the range of the d-values of 3.0-4.0.multidot.10.sup.-8 cm. Process for rinsing textiles using the crystalline laminated silic acid or its alkali metal salts as a textile softening agent.
摘要翻译：织物软化洗涤剂组合物含有5-70重量％表面活性剂，0.5-50重量％助洗剂，1-20重量％结晶层状硅酸和/或相应的碱金属硅酸盐和标准洗涤助剂。其特征在于结晶层状硅酸或其通式为M2SixO2x + 1xyH2O的碱金属盐，其中x表示大于7.0的数，M表示钠，钾或氢，y表示数从0到25，在d值为3.0-4.0x10-8 cm的范围内，在X射线衍射图中显示了对石英，鳞石英和方英石不可分的一种或多种反射。使用结晶层状硅酸或其碱金属盐作为织物软化剂漂洗纺织品的方法。

4. 发明授权

US4371509A Oxidizing phosphorus compounds with chlorosulfonic acid 失效
标题翻译：用氯磺酸氧化磷化合物
公开(公告)号：US4371509A
公开(公告)日：1983-02-01
申请号：US299678
申请日：1981-09-08
申请人： Jurgen Grosse
发明人： Jurgen Grosse
IPC分类号： C01B25/10 , C07F9/12 , C07F9/14 , C07F9/143 , C07F9/20 , C07F9/206 , C07F9/34 , C07F9/42 , C07F9/53 , C07F9/6574 , C07F9/09 , C07F9/28
CPC分类号： C07F9/65742 , C01B25/10 , C07F9/12 , C07F9/14 , C07F9/20 , C07F9/34 , C07F9/42 , C07F9/53
摘要： The invention relates to a process for oxidizing organic phosphorus compounds of the general formula (I)R.sub.3-n PX.sub.n (I)in which R stands for an organic radical, X stands for halogen and n stands for 0, 1, 2 or 3, to obtain compounds of the general formula (II)R.sub.3-n P(O)X.sub.n (II)in which R, X and n have the meanings given above. To this end, chlorosulfonic acid is used as oxidant and the oxidation is effected in homogeneous liquid phase.
摘要翻译：本发明涉及一种氧化通式（Ⅰ）R3-nPXn（Ⅰ）的有机磷化合物的方法，其中R代表有机基团，X代表卤素，n代表0,1,2或3，获得其中R，X和n具有上述含义的通式（II）的化合物R3-nP（O）Xn（II）。为此，使用氯磺酸作为氧化剂，氧化是在均相液相中进行的。

5. 发明授权

US4749758A Process for the preparation of copolymers of vinylphosphonic acid and (meth) acrylic acid in aqueous solution 失效
标题翻译：乙烯基膦酸和（甲基）丙烯酸在水溶液中的共聚物的制备方法
公开(公告)号：US4749758A
公开(公告)日：1988-06-07
申请号：US858568
申请日：1986-04-24
申请人： Walter Dursch , Jurgen Grosse , Werner Gohla , Friedrich Engelhardt , Ulrich Riegel
发明人： Walter Dursch , Jurgen Grosse , Werner Gohla , Friedrich Engelhardt , Ulrich Riegel
IPC分类号： C08F2/00 , C08F4/32 , C08F30/00 , C08F30/02 , C08F220/06 , C08F230/02 , C11D3/37
CPC分类号： C08F230/02 , C11D3/3784
摘要： Process for the preparation of polymers of vinylphosphonic acid in water with the aid of catalysts which form free radicals, which comprises heating vinylphosphonic acid and (meth)acrylic acid to temperatures of 40.degree. to 120.degree. C. in water in the presence of 1 to 5.5% by weight of aliphatic peroxy esters and/or diacyl peroxides which dissociate by half in one hour at temperatures below 122.degree. C., the total amount of vinylphosphonic acid being taken together with up to 30% by weight, based on the total amount of monomer, of (meth)acrylic acid and the remainder of the (meth)acrylic acid being added in the course of the reaction.The copolymers are suitable for use in detergent and cleaning agents.
摘要翻译：借助于形成自由基的催化剂制备乙烯基膦酸在水中的聚合物的方法，该催化剂包括将乙烯基膦酸和（甲基）丙烯酸在40℃至120℃的温度下在1〜 5.5％（重量）脂肪族过氧酯和/或二酰基过氧化物，其在低于122℃的温度下在1小时内解离了一半，乙烯基膦酸的总量基于总量达到30重量％的单体，（甲基）丙烯酸，其余的（甲基）丙烯酸是在反应过程中加入的。该共聚物适用于洗涤剂和清洁剂。

6. 发明授权

US4473509A Process for making phosphonic anhydrides 失效
标题翻译：制备膦酸酐的方法
公开(公告)号：US4473509A
公开(公告)日：1984-09-25
申请号：US442103
申请日：1982-11-16
申请人： Jurgen Grosse , Werner Pieper
发明人： Jurgen Grosse , Werner Pieper
IPC分类号： C07F9/38 , C07F9/40 , C07F9/28
CPC分类号： C07F9/3895
摘要： The disclosure relates to a process for making phosphonic anhydrides of general formula (I)(RPO.sub.2).sub.n.H.sub.2 O (I)in which R stands for an alkyl or aryl radical having from 1 to 6 carbon atoms and n stands for a value between 2 and 20. To this end, the disclosure provides for a compound of general formula (II) ##STR1## in which R has the meaning given above to be oxidized with concentrated sulfuric acid under inert gas and in the presence of a diluent at a temperature between 0.degree. and 100.degree. C., the compound of general formula (II) and sulfuric acid being used in a molar ratio of about 1:1.
摘要翻译：本公开涉及制备通式（I）（RPO 2）n·H 2 O（I）的膦酸酐的方法，其中R表示具有1至6个碳原子的烷基或芳基，n表示2 为此，本公开内容提供了通式（II）的化合物（II），其中R具有上述给出的含义，以在惰性气体下和在稀释剂存在下用浓硫酸氧化在0℃至100℃的温度下，通式（II）的化合物和硫酸的摩尔比为约1:1。

7. 发明授权

US5158752A Plant for producing ammonium polyphosphate 失效
标题翻译：生产聚磷酸铵的工厂
公开(公告)号：US5158752A
公开(公告)日：1992-10-27
申请号：US657532
申请日：1991-02-19
申请人： Thomas Staffel , Gunther Schimmel , Horst Buhl , Jurgen Grosse
发明人： Thomas Staffel , Gunther Schimmel , Horst Buhl , Jurgen Grosse
IPC分类号： C01B15/16 , C01B25/40 , C05B13/06
CPC分类号： C01B25/405 , C05B13/06
摘要： A plant for producing chain-type ammonium polyphosphate from ammonium orthophosphate and phosphorus pentoxide in the presence of gaseous ammonia comprises a reactor having rotatable mixing, kneading and comminuting tools in its interior and a feed pipe for the solid starting materials, an introduction pipe for ammonia, a gas discharge pipe and a discharge line for the reaction product, all of which are flow-connected to the interior of the reactor. The discharge line of the reactor is also connected for material flow to a mixing apparatus. A discharge device, which is controlled by the power consumption of the drive motor of the reactor, is arranged in the discharge line.
摘要翻译：一种在气态氨存在下由正磷酸铵和五氧化磷生产链式多磷酸铵的设备包括一个在其内部具有可旋转的混合，捏合和粉碎工具的反应器，以及用于固体原料的进料管，用于氨的引入管，气体排出管和反应产物的排出管线，所有这些都与反应器的内部流通。反应器的排出管线也连接用于物料流到混合装置。排出装置，其由反应堆的驱动电动机的功率消耗来控制，排放在排出管线中。

8. 发明授权

US4427603A Process for making phosphonic acid ester chlorides 失效
标题翻译：制备膦酸酯氯化物的方法
公开(公告)号：US4427603A
公开(公告)日：1984-01-24
申请号：US379304
申请日：1982-05-18
申请人： Jurgen Grosse , Werner Pieper
发明人： Jurgen Grosse , Werner Pieper
IPC分类号： C07F9/42 , C07F9/14
CPC分类号： C07F9/425
摘要： The disclosure relates to a process for making phosphonic acid ester chlorides of the general formula (I)R--P(O) ClOR' (I)in which R stands for an alkyl group with 1 to 6 carbon atoms or an aryl group and R' stands for an alkyl group with 1 to 20 carbon atoms or an aryl group. More particularly, a compound of general formula (II)R--PCl.sub.2 (II)is reacted with a sulfuric acid monoester of general formula (III)R'--O--SO.sub.3 H (III)R and R' in formulae (II) and (III) having the meanings given above; the reactants are used in about equimolar proportions and the reaction is effected at a temperature of from -20.degree. C. to 50.degree. C. After termination of the reaction, the phosphonic acid ester chloride is separated from the reaction mixture by subjecting this latter to distillation under vacuum.
摘要翻译：本公开涉及制备通式（I）RP（O）ClOR'（I）的膦酸酯氯化物的方法，其中R表示具有1至6个碳原子的烷基或芳基，R'表示对于具有1至20个碳原子的烷基或芳基。更具体地，将通式（II）的化合物R-PCl 2（II）与通式（III）的硫酸单酯与式（II）中的R'-O-SO 3 H（III）R和R'与（ III）具有上述含义; 反应物以约等摩尔比例使用，反应在-20℃至50℃的温度下进行。反应终止后，将膦酸酯氯化物从反应混合物中分离，真空蒸馏。

9. 发明授权

US4242511A Production of amine salts of acid O,S-dialkylthiophosphoric acid 失效
标题翻译：生产酸O，S-二烷基硫代磷酸的胺盐
公开(公告)号：US4242511A
公开(公告)日：1980-12-30
申请号：US72084
申请日：1979-09-04
申请人： Jurgen Grosse
发明人： Jurgen Grosse
IPC分类号： C07F9/17 , C07F9/165 , C07D295/00 , C07F9/65
CPC分类号： C07F9/165
摘要： The invention relates to an improved process for making amine salts of acid O,S-dialkylthiophosphoric acid esters of the general formula (I) ##STR1## in which R.sub.1 stands for the ammonium ion of primary or secondary aliphatic, cycloaliphatic or aromatic amines or of a heterocyclic nitrogen base and R.sub.2 and R.sub.3 each stand for an alkyl group by subjecting an O,O,S-trialkyl-thiophosphate to partial dealkylation and forming the salt of the dealkylated product by treatment with an amine corresponding to the ammonium ion R.sub.1. In the improved process an O,O,S-trialkylthiophosphate of the general formula (II) ##STR2## in which R.sub.2 and R.sub.3 have the meanings given above, is mixed with at least stoechiometric proportions of water and an amine corresponding to the ammonium ion R.sub.1, the resulting mixture is reacted, with agitation, over a period of about 3 to 8 hours at a temperature within the range 0.degree. to 120.degree. C., and the amine salt of the general formula (I) is separated from the reaction mixture.
摘要翻译：本发明涉及一种制备通式（I）的酸式O，S-二烷基硫代磷酸酯的胺盐的改进方法，其中R1代表伯或仲脂族，脂环族或芳族的铵离子胺或杂环氮基，R 2和R 3各自代表烷基，通过使O，O，S-三烷基 - 硫代磷酸酯进行部分脱烷基化并通过用对应于铵离子的胺处理形成脱烷基化产物的盐 R1。在改进的方法中，其中R2和R3具有上述含义的通式（II）的二O，O，S-三烷基硫代磷酸酯与至少组分比例的水和相应于铵离子R1，所得混合物在搅拌下在0〜120℃的温度下反应约3〜8小时，通式（I）的胺盐分离从反应混合物中。

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