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1. 发明授权

US4410466A Process for extractively separating a mixture containing phosphoric acid monoalkylesters into its components 失效
标题翻译：将含有磷酸单烷基酯的混合物萃取分离成其组分的方法
公开(公告)号：US4410466A
公开(公告)日：1983-10-18
申请号：US327429
申请日：1981-12-04
申请人： Gunther R. Schimmel , Werner Klose
发明人： Gunther R. Schimmel , Werner Klose
IPC分类号： C07F9/02 , C07F9/11 , C07F9/09
CPC分类号： C07F9/025 , C07F9/11
摘要： The invention relates to a process for separating a mixture containing phosphoric acid monoalkylesters, phosphoric acid dialkylesters and minor proportions of diphosphoric acid dialkylesters, each with 6 to 12 carbon atoms in the alkyl radical, by extractively distributing them between an aliphatic or aromatic hydrocarbon as an unpolar solvent and a polar solvent. To this end, the invention provides: for the ester mixture to be admixed with the quantity of water stoichiometrically necessary for hydrolyzing the P-O-P-bond of the diphosphoric acid dialkylester with the resultant formation of the phosphoric acid monoalkylester; for the whole to be maintained for at least 1 hour at temperatures higher than 60.degree. C.; for the partially hydrolyzed ester mixture to be treated in a countercurrent apparatus comprising n-stages with the solvents immiscible or partially miscible with one another so as to ensure introduction of pure solvent into stage 1 and stage n, respectively, and the introduction of partially hydrolyzed mixture into one of the stages 2 to (n-1), n standing for a whole number of at least 3.
摘要翻译：本发明涉及一种在烷基中分离含有磷酸单烷基酯，磷酸二烷基酯和较少比例的二磷酸二烷基酯的混合物的方法，它们各自具有6至12个碳原子，通过将其分散在脂族或芳族烃之间，作为非极性溶剂和极性溶剂。为此，本发明提供：将酯混合物与水解磷酸二烷基酯的P-O-P键的化学计量所需的水量混合，从而形成磷酸单烷基酯; 整体在高于60℃的温度下保持至少1小时。对于部分水解的酯混合物在包含n阶段的逆流装置中进行处理，其中溶剂与溶剂彼此不混溶或部分混溶，以确保将纯溶剂分别引入阶段1和阶段n，并引入部分水解的混合物进入阶段2至（n-1）之一，n代表至少3的整数。

2. 发明授权

US4960928A 1-Hydroxy-omega-(alkyl- or arylphosphinico)alkane-1,1-diphosphonic acids, salts thereof, and processes for the preparation of these compounds 失效
标题翻译： 1-羟基-ω-（烷基 - 或芳基膦基）烷烃-1,1-二膦酸，其盐，以及这些化合物的制备方法
公开(公告)号：US4960928A
公开(公告)日：1990-10-02
申请号：US308840
申请日：1989-02-09
申请人： Werner Klose , Helmut Klemp
发明人： Werner Klose , Helmut Klemp
IPC分类号： A61K8/00 , A61Q11/00 , C07F9/32 , C07F9/38 , C09K3/00
CPC分类号： C07F9/386
摘要： The present invention relates to 1-hydroxy-.omega.-(alkyl- or arylphosphinico)alkane-1,1-diphosphonic acids of the general formula I ##STR1## and to the salts of these acids of the general formula II ##STR2## where, in these formulae, R.sup.1 denotes an alkyl radical having 1 to 6 carbon atoms, a cycloalkyl radical having 5 to 7 carbon atoms or an aryl radical having 6 to 10 carbon atoms, R.sup.2 denotes a straight-chain or branched alkylene radical having 1 to 6 carbon atoms and A denotes a monovalent equivalent of a cation of an inorganic or organic base. In addition, processes are described for the preparation of these novel compounds.
摘要翻译：本发明涉及通式I的1-羟基-ω-（烷基 - 或芳基膦基）烷烃-1,1-二膦酸和通式II的这些酸的盐，其中在这些式中，R 1表示碳原子数1〜6的烷基，碳原子数5〜7的环烷基或碳原子数6〜10的芳基，R2表示直链或支链的亚烷基， 6个碳原子，A表示无机或有机碱的阳离子的一价等价物。另外还描述了制备这些新化合物的方法。

3. 发明授权

US4418019A Process for the manufacture of 1-aminoalkane-1,1-diphosphonic acids 失效
标题翻译：制备1-氨基链烷-1,1-二膦酸的方法
公开(公告)号：US4418019A
公开(公告)日：1983-11-29
申请号：US327888
申请日：1981-12-07
申请人： Werner Klose , Theodor Auel
发明人： Werner Klose , Theodor Auel
IPC分类号： C07F9/38 , C07F9/40
CPC分类号： C07F9/3873
摘要： The invention relates to a process for making 1-aminoalkane-1,1-diphosphonic acids of the general formula (I): ##STR1## in which R stands for an aliphatic hydrocarbon radical having from 1 to 12 carbon atoms.To this end, the invention provides:(a) for tetraphosphorus hexoxide to be reacted with at least one compound of the general formula (II) ##STR2## in which R has the meaning given above and X stands for an --ONH.sub.4 or NH.sub.2 -radical, in inert gas atmosphere at elevated temperature, the molar ratio of tetraphosphorus hexoxide to the compound of general formula (II) being about 1 to 2-6; and(b) for 1-aminoalkane-1,1-diphosphonic acid to be crystallized from the reaction mixture.
摘要翻译：本发明涉及制备通式（I）的1-氨基烷烃-1,1-二膦酸的方法：其中R代表具有1至12个碳原子的脂族烃基。为此，本发明提供：（a）与至少一种通式（II）的化合物（II）反应的四氧化二鏻，其中R具有上述含义，X代表-ONH 4 或NH 2 - 自由基，在高温下在惰性气体气氛中，六
氧化四磷与通式（II）化合物的摩尔比为约1〜2-6; 和（b）从反应混合物中结晶的1-氨基烷烃-1,1-二膦酸。

4. 发明授权

US4915865A Dimensionally stable alkaline cleansing agents of low density, and a process for their preparation 失效
标题翻译：尺寸稳定的低密度碱性清洁剂及其制备方法
公开(公告)号：US4915865A
公开(公告)日：1990-04-10
申请号：US207454
申请日：1988-06-16
申请人： Lothar Westermann , Hannsjorg Ulrich , Werner Klose
发明人： Lothar Westermann , Hannsjorg Ulrich , Werner Klose
IPC分类号： C11D7/36 , C11D1/78 , C11D3/06 , C11D3/10 , C11D3/36 , C11D17/00
CPC分类号： C11D17/0052 , C11D1/78 , C11D17/0073 , C11D3/06 , C11D3/10 , C11D3/362
摘要： Dimensionally stable alkaline cleansing agents of low density consist at least of 2 to 50% by weight of alkali metal phosphates, 2 to 50% by weight of silicates and 1 to 60% by weight of alkali metal hydroxides and/or alkali metal carbonates or bicarbonates and additionally contain 0.25 to 10% by weight of phosphoric acid partial esters.These cleansing agents are prepared by first foaming phosphoric acid partial esters with water in a weight ratio of (1:2) to (1:80), using intensive stirring. When the remaining components have been incorporated into the foam, using stirring or kneading, the resulting mixture is converted to moldings. The moldings are allowed to set for 0.5 to 15 hours.
摘要翻译：尺寸稳定的低密度碱性清洁剂至少含有2至50重量％的碱金属磷酸盐，2至50重量％的硅酸盐和1至60重量％的碱金属氢氧化物和/或碱金属碳酸盐或碳酸氢盐另外含有0.25〜10重量％的磷酸偏酯。这些清洁剂的制备方法是，通过在强烈搅拌下，以重量比为（1:2）至（1:80）的水，首先使磷酸偏酯进行发泡。当其余组分已经被引入到泡沫中时，使用搅拌或捏合，将所得混合物转化成模制品。允许模制品设定0.5至15小时。

5. 发明授权

US4118443A Production of acid phosphoric acid ester salts 失效
标题翻译：生产酸式磷酸酯盐
公开(公告)号：US4118443A
公开(公告)日：1978-10-03
申请号：US761054
申请日：1977-01-21
申请人： Werner Klose
发明人： Werner Klose
IPC分类号： C07F9/09
CPC分类号： C07F9/09
摘要： A product consisting essentially of an acid orthophosphoric acid ester salt and containing at most about 1 weight % of water is made. The ester group R contains 1 to 50 carbon atoms, and the salt-forming cation M is a mono- or bivalent metal ion or an ammonium ion. To make the product, molar proportions of P.sub.2 O.sub.5 and of a compound of the general formulae M.sub.2 O, M.sub.2 CO.sub.3, MO or MCO.sub.3 are reacted at about 0.degree. to 150.degree. C, with thorough agitation, with 2/m mol of an at least partially liquid or molten organic hydroxyl compound of the general formula R(OH).sub.m, in which formulae the substituents M and R have the meanings given above and m is a number of 1 to 4. The reaction is terminated and the reaction product is cooled.
摘要翻译：制备基本上由酸性正磷酸酯盐组成并且含有至多约1重量％水的产物。酯基R含有1至50个碳原子，并且成盐阳离子M是一价或二价金属离子或铵离子。为了制备该产物，P2O5和通式M 2 O，M 2 CO 3，MO或MCO 3的化合物的摩尔比例在约0℃至150℃下反应，充分搅拌，以2摩尔的至少部分液体或通式R（OH）m的熔融有机羟基化合物，其中取代基M和R具有上述含义，m为1至4的数。反应终止，反应产物冷却。

6. 发明授权

US4752648A Process for making chlorophosphines and thiophosphinic acid chlorides, and 9-chloro-9-thioxo-9-phosphabicyclononanes 失效
标题翻译：制备氯膦和硫代次膦酸氯化物的方法和9-氯-9-硫代-9-磷杂双环壬烷
公开(公告)号：US4752648A
公开(公告)日：1988-06-21
申请号：US908999
申请日：1986-09-18
申请人： Norbert Weferling , Werner Klose
发明人： Norbert Weferling , Werner Klose
IPC分类号： C07F9/34 , C07F9/52 , C07F9/6568 , C07C161/02 , C07F9/53
CPC分类号： C07F9/65681 , C07F9/34 , C07F9/52
摘要： Chlorophosphines or thiophosphinic acid chlorides of the general formulae RPCl.sub.2, R.sub.2 PCl or R.sub.2 P(.dbd.S)Cl are made from feed materials selected from hydrogen-functional primary or secondary phosphines or secondary phosphine sulfides, where R stands for identical or different, linear or branched, substituted or unsubstituted alkyl radicals having from 1-16 carbon atoms, aryl radicals, aralkyl radicals or alkylaryl radicals having from 6-9 carbon atoms or cycloalkyl radicals having from 5-10 carbon atoms. To this end, the feed materials are reacted with phosphorus pentachloride, or with chlorine gas in the presence of phosphorus trichloride at temperatures within the range -78.degree. to +145.degree. C. It is possible for two radicals R to be linked together by one or two substituted or unsubstituted hydrocarbon chains having from 1-4 carbon atoms.
摘要翻译：通式为RPCl2，R2PCl或R2P（= S）Cl的氯膦或硫代次膦酸氯化物由选自氢功能的伯或次膦或次膦硫化物的原料制成，其中R代表相同或不同的直链或支链，具有1-16个碳原子的取代或未取代的烷基，具有6-9个碳原子的芳基，芳烷基或烷基芳基或具有5-10个碳原子的环烷基。为此，在三氯化磷存在下，在-78℃至+ 145℃的温度范围内，使进料与五氯化磷或氯气反应。两个基团R可能连接在一起或两个具有1-4个碳原子的取代或未取代的烃链。

7. 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。

8. 发明授权

US4258022A Continuous production of phosphine 失效
标题翻译：连续生产磷化氢
公开(公告)号：US4258022A
公开(公告)日：1981-03-24
申请号：US75001
申请日：1979-09-12
申请人： Georg Elsner , Werner Klose , Christian May , Gero Heymer
发明人： Georg Elsner , Werner Klose , Christian May , Gero Heymer
IPC分类号： C01B25/06 , C01B25/00
CPC分类号： C01B25/06
摘要： The invention relates to the continuous production of phosphine. To this end, elemental phosphorus is reacted with an aqueous alkali metal hydroxide solution and at least one alcohol, the reactants being used in admixture with 0.01 to 2 weight % of a surfactant, the percentage being based on the alcohol.
摘要翻译：本发明涉及磷化氢的连续生产。为此，元素磷与碱金属氢氧化物水溶液和至少一种醇反应，反应物与0.01至2重量％的表面活性剂混合使用，其百分比基于醇。

9. 发明授权

US4141938A Production of acid orthophosphoric acid ester mixtures 失效
标题翻译：生产酸性正磷酸酯混合物
公开(公告)号：US4141938A
公开(公告)日：1979-02-27
申请号：US851944
申请日：1977-11-16
申请人： Werner Klose
发明人： Werner Klose
IPC分类号： C07F9/09 , C11D3/36
CPC分类号： C07F9/09 , C11D3/362
摘要： Orthophosphoric acid esters are made by reacting phosphorus(V)-oxide with an alcoholic component. More specifically, phosphorus(V)-oxide is reacted by mixing or kneading it with a blend consisting of a monohydric alcohol and an alkane polyol containing 2 to 12 carbon atoms and 2 to 6 hydroxyl groups, at approximately 0 to 120.degree. C. with the exclusion of moisture, in the presence of an inert gas, and over a period of approximately 1 to 6 hours. The resulting reaction product is cooled.
摘要翻译：正磷酸酯通过使磷（V） - 氧化物与醇组分反应制备。更具体地，通过在约0至120℃下将含有2至12个碳原子和2至6个羟基的一元醇和一种含有多元醇的烷烃多元醇混合或混合，在惰性气体的存在下排除水分，并且在约1至6小时的时间内排除水分。将所得反应产物冷却。

10. 发明授权

US4136154A Stabilized red phosphorus and process for making it 失效
公开(公告)号：US4136154A
公开(公告)日：1979-01-23
申请号：US841833
申请日：1977-10-13
申请人： Horst Staendeke , Franz-Josef Dany , Joachim Kandler , Werner Klose
发明人： Horst Staendeke , Franz-Josef Dany , Joachim Kandler , Werner Klose
IPC分类号： C09K15/32 , C01B25/00
CPC分类号： C01B25/006
摘要： Production of stabilized pulverulent red phosphorus. The phosphorus so stabilized comprises a homogeneous blend of red phosphorus particles with a size of at most about 2 mm and a metal compound of the second or third group of the Periodic System as an oxidation stabilizer, wherein the metal compound is the aluminum, calcium or zinc salt of a phosphinic acid of the general formula ##STR1## in which R.sub.1 and R.sub.2 each stand for an alkyl, cycloalkyl, aryl or aralkyl group having 1 to 20 carbon atoms, the metal compound being present in the homogeneous blend in a proportion of about 0.5 to 5 weight %.

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