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1. 发明授权

US4163760A Continuous production of organic phosphines 失效
标题翻译：连续生产有机膦
公开(公告)号：US4163760A
公开(公告)日：1979-08-07
申请号：US872250
申请日：1978-01-25
申请人： Georg Elsner , Gero Heymer , Hans-Werner Stephan
发明人： Georg Elsner , Gero Heymer , Hans-Werner Stephan
IPC分类号： C07F9/50 , C07F9/6568 , C07F9/54
CPC分类号： C07F9/5059 , C07F9/65683
摘要： Organic phosphines are produced by reacting an alkylene, cycloalkylene or aralkylene in the presence of a free radical-yielding catalyst. More specifically, a pressure reactor, which is provided in its interior with mixing elements, kept free from oxygen, and subdivided so as to comprise an upper cooling zone and a lower reaction zone, is continuously supplied from above with (a) a solution of the alkylene, cycloalkylene or aralkylene and the catalyst in an inert solvent, and (b) a stoichiometric excess of hydrogen phosphide, the said (a) and (b) reactants being supplied jointly with but separately from one another; the (a) and (b) reactants are mixed in the upper cooling zone of the reactor at about 0.degree. to 35.degree. C. and under a PH.sub.3 -pressure of about 80 to 300 bars; the resulting mixture, which travels downwardly in the reactor, is reacted in the lower reaction zone at about 90.degree. to 190.degree. C., the reactants being allowed to remain in the reactor for a period of time about 13 to 15 times longer than the half life period of the catalyst; the reaction mixture is removed through the bottom portion of the reactor and subjected to distillation so as to separate the organic phosphines.
摘要翻译：有机膦通过在产生自由基的催化剂存在下使亚烷基，亚环烷基或亚芳烷基反应来制备。更具体地，在其内部设置有保持无氧的并且被分为包括上部冷却区和下部反应区的混合元件的压力反应器从上方连续地供给（a）所述（a）和（b）反应物是由彼此共同供应的;（b）化学计量过量的磷酸氢盐，所述（a）和（b）（a）和（b）反应物在反应器的上部冷却区中在约0℃至35℃下混合，并在约80至300巴的PH3压力下混合; 在反应器中向下移动的所得混合物在下部反应区中在约90℃至190℃下反应，使反应物在反应器中保留约13至15倍的时间催化剂的半衰期; 将反应混合物通过反应器的底部除去并进行蒸馏以分离有机膦。

2. 发明授权

US4273752A Process for making red phosphorus 失效
标题翻译：制造红磷的工艺
公开(公告)号：US4273752A
公开(公告)日：1981-06-16
申请号：US123106
申请日：1980-02-20
申请人： Klaus Lehr , Gero Heymer , Hans-Werner Stephan , Ursus Thummler
发明人： Klaus Lehr , Gero Heymer , Hans-Werner Stephan , Ursus Thummler
IPC分类号： B01J8/10 , B01J19/28 , B02C17/00 , C01B25/02 , C01B25/023 , C01B25/01 , C01B25/04
CPC分类号： C01B25/023
摘要： The invention relates to a process for making red phosphorus by subjecting molten yellow phosphorus to a thermal conversion reaction in a closed reaction zone. To this end, a hollow shaft-provided and closed ball mill is preheated to a reaction temperature within the range 280.degree. to 590.degree. C. Yellow phosphorus is continuously introduced into the ball mill through the hollow shaft in quantities per unit time which permit the reaction temperature prevailing inside the ball mill to be maintained without supply of heat from the outside. More particularly, decreasing quantities of yellow phosphorus are introduced per unit time at increasing temperature and increasing quantities of yellow phosphorus are introduced per unit time at decreasing temperature within the limits specified. Red phosphorus is allowed to cool inside the ball mill, water is poured over it and the whole is subjected to wet-grinding. An aqueous suspension of red phosphorus is finally removed from the ball mill.
摘要翻译：本发明涉及通过使熔融黄磷在封闭反应区中进行热转化反应来制备红磷的方法。为此，空心轴提供和封闭的球磨机被预热到280℃至590℃的反应温度。黄磷通过空心轴以每单位时间的量连续地引入球磨机，这允许球磨机内部的反应温度保持不受外界的热量的限制。更特别地，在增加的温度下每单位时间引入黄磷的减少量，并且在规定的限度内在降低的温度下每单位时间引入增加量的黄磷。使红磷在球磨机内冷却，将水倒在其上，整体进行湿磨。最终从球磨机中除去红磷水悬浮液。

3. 发明授权

US4355010A Process for removing phosphorus in vapor form and phosphanes from gas mixtures 失效
标题翻译：从气体混合物中除去蒸汽形式的磷和磷烷的方法
公开(公告)号：US4355010A
公开(公告)日：1982-10-19
申请号：US201761
申请日：1980-10-29
申请人： Klaus Jodden , Friedrich-Wilhelm Dorn , Gero Heymer , Hans-Werner Stephan
发明人： Klaus Jodden , Friedrich-Wilhelm Dorn , Gero Heymer , Hans-Werner Stephan
IPC分类号： B01D53/46 , C01B25/027 , B01D53/34 , C01B25/12
CPC分类号： B01D53/46 , C01B25/027
摘要： Phosphorus in vapor form and phosphanes are separated from gas mixtures which consist of carbon monoxide, with or without hydrogen, nitrogen and steam. Concerned are more particularly the off-gases of phosphorus-producing furnaces. To this end, the gas mixture is admixed with at least the stoichiometric amount of oxygen and/or of oxygen-containing gases necessary to achieve conversion of the total phosphorus contained in the gas mixture to oxidation level V. The resulting mixture is introduced into a reaction zone maintained at a temperature within the range 200.degree. to 700.degree. C. and allowed to remain therein over a period of 0.5 to 20 seconds. Resulting phosphorus-V compounds are finally separated from the gas mixture.
摘要翻译：蒸气形式的磷和磷烷与由一氧化碳，有或没有氢气，氮气和蒸汽组成的气体混合物分离。更关心的是生产磷的炉的废气。为此，将气体混合物与至少化学计量的氧和/或含氧气体混合，以使气体混合物中所含的总磷转化为氧化水平V.将所得混合物引入到反应区保持在200℃至700℃的温度范围内，并允许其在0.5至20秒的时间内保留。最终从气体混合物中分离所得的磷-V化合物。

4. 发明授权

US4530769A Process for separating carbon black from an aqueous suspension 失效
标题翻译：从水性悬浮液中分离炭黑的方法
公开(公告)号：US4530769A
公开(公告)日：1985-07-23
申请号：US479965
申请日：1983-03-29
申请人： Manfred Wolter , Friedrich-Wilhelm Dorn , Gero Heymer , Hans-Werner Stephan
发明人： Manfred Wolter , Friedrich-Wilhelm Dorn , Gero Heymer , Hans-Werner Stephan
IPC分类号： B01D25/12 , C09C1/48 , C10G31/09 , B01D29/10
CPC分类号： C09C1/487 , C01P2006/12
摘要： The disclosure relates to a process for the discontinuous separation of a solid consisting predominantly of carbon black from its aqueous suspension by filtration. To this end, the disclosure provides for use to be made of a tube pressure filter which is operated under a final pressure of 30 to 100 bars.
摘要翻译：本公开涉及通过过滤从其水悬浮液中主要由炭黑组成的固体的不连续分离的方法。为此，本公开提供了用于在30至100巴的最终压力下操作的管式压力过滤器的使用。

5. 发明授权

US3931294A Production of 2-phenyl-ethylene phosphonic acid 失效
标题翻译： 2-苯基 - 乙烯膦酸的制备
公开(公告)号：US3931294A
公开(公告)日：1976-01-06
申请号：US481813
申请日：1974-06-21
申请人： Theodor Auel , Gero Heymer , Hans-Werner Stephan
发明人： Theodor Auel , Gero Heymer , Hans-Werner Stephan
IPC分类号： C07F9/38 , C07F9/40 , C07F9/42
CPC分类号： C07F9/3826 , C07F9/42
摘要： Production of 2-phenyl-ethylene phosphonic acid by reacting styrene with phosphorus pentachloride in a molar ratio of about 1 : 2 in liquid phase and hydrolyzing the resulting complex 2-phenyl-ethylene phosphonic acid tetrachloride with water. The reaction is more particularly started with the use as the liquid phase of the equimolar mixture of 2-phenyl-ethylene phosphonic acid dichloride and phosphorus oxychloride obtained as an intermediary product; styrene and phosphorus pentachloride are introduced thereinto with continuous agitation; resulting complex 2-phenyl-ethylene phosphonic acid tetrachloride is partially hydrolyzed by adding a predetermined quantity of water to an equimolar mixture of 2-phenyl-ethylene phosphonic acid dichloride and phosphorus oxychloride; a portion of the resulting clear solution is continuously used as the liquid phase and phosphorus oxychloride is continuously distilled off under reduced pressure from the balance portion of the solution; remaining 2-phenyl-ethylene phosphonic acid dichloride is hydrolyzed by continuous addition of overstoichiometric proportions of water to an aqueous solution of 2-phenyl-ethylene phosphonic acid; the aqueous solution is cooled and crystalline phosphonic acid is precipitated therefrom.
摘要翻译：通过苯乙烯与五氯化磷在液相中以约1:2的摩尔比反应制备2-苯基 - 乙烯膦酸，并用水将所得的络合物2-苯基 - 乙烯膦酸四氯化物水解。反应更特别地以作为中间产物获得的2-苯基 - 乙烯膦酸二氯化物和磷酰氯的等摩尔混合物的液相的用途开始; 连续搅拌引入苯乙烯和五氯化磷; 通过向2-苯基 - 乙烯膦酰氯和磷酰氯的等摩尔混合物中加入预定量的水，使得2-苯基 - 乙烯膦酸四氯化物的复合物部分水解; 所得澄清溶液的一部分连续地用作液相，并且在减压下从溶液的平衡部分连续蒸馏除去三氯氧磷; 剩余的2-苯基 - 乙烯膦酸二氯化物通过将过度化学计量比例的水连续加入到2-苯基 - 乙烯膦酸的水溶液中来水解; 将水溶液冷却并从其中沉淀出结晶的膦酸。

6. 发明授权

US4540558A Process for removing organic contaminants from wet-processed phosphoric acid 失效
标题翻译：从湿法处理的磷酸中除去有机污染物的方法
公开(公告)号：US4540558A
公开(公告)日：1985-09-10
申请号：US627456
申请日：1984-07-03
申请人： Reinhard Gradl , Hans-Werner Stephan , Gero Heymer , Gunther Schimmel
发明人： Reinhard Gradl , Hans-Werner Stephan , Gero Heymer , Gunther Schimmel
IPC分类号： C01B25/235 , C01B25/237
CPC分类号： C01B25/235
摘要： The disclosure relates to a process for removing organic compounds from wet-processed phosphoric acid with the aid of an adsorbant. To this end the disclosure provides for the acid to be heated to at least 250.degree. C. prior to treating it with the adsorbant. The disclosure also relates to an apparatus for carrying out the process.
摘要翻译：本公开涉及借助吸附剂从湿法处理的磷酸中除去有机化合物的方法。为此，本公开提供了在用吸附剂处理之前将其加热至至少250℃的酸。本公开还涉及一种用于执行该过程的装置。

7. 发明授权

US4517163A Process for making titanium dioxide concentrates 失效
标题翻译：制备二氧化钛浓缩物的方法
公开(公告)号：US4517163A
公开(公告)日：1985-05-14
申请号：US469220
申请日：1983-02-24
申请人： Klaus Jodden , Gero Heymer , Hans-Werner Stephan
发明人： Klaus Jodden , Gero Heymer , Hans-Werner Stephan
IPC分类号： C22B34/12 , C01G23/07 , C01G23/08
CPC分类号： C22B34/1209
摘要： The disclosure relates to a process for making titanium dioxide concentrates from material containing titanium oxide and iron oxides. More particularly, the titanium oxide-containing material is calcined at temperatures of 870.degree. to 1300.degree. C., and then treated with a chlorine-containing gas at temperatures of 800.degree. to 1300.degree. C., if desired with addition of carbon.
摘要翻译：本公开涉及由含有氧化钛和氧化铁的材料制备二氧化钛浓缩物的方法。更具体地说，含氧化钛的材料在870℃至1300℃的温度下煅烧，然后如果需要，加入碳，然后在含有800℃至1300℃的温度下用含氯气体处理。

8. 发明授权

US4330504A Apparatus for making red phosphorus 失效
标题翻译：制备红磷的装置
公开(公告)号：US4330504A
公开(公告)日：1982-05-18
申请号：US226468
申请日：1981-01-19
申请人： Klaus Lehr , Gero Heymer , Hans-Werner Stephan , Ursus Thummler
发明人： Klaus Lehr , Gero Heymer , Hans-Werner Stephan , Ursus Thummler
IPC分类号： B01J8/10 , B01J19/28 , B02C17/00 , C01B25/02 , C01B25/023
CPC分类号： C01B25/023
摘要： The invention relates to an apparatus for making red phosphorus by subjecting molten yellow phosphorus to a thermal conversion reaction in a closed reaction zone. To this end, a hollow shaft-provided and closed ball mill is preheated to a reaction temperature within the range 280.degree. to 590.degree. C. Yellow phosphorus is continuously introduced into the ball mill through the hollow shaft in quantities per unit time which permit the reaction temperature prevailing inside the ball mill to be maintained without supply of heat from the outside. More particularly, decreasing quantities of yellow phosphorous are introduced per unit time at increasing temperature and increasing quantities of yellow phosphorus are introduced per unit time at decreasing temperature within the limits specified. Red phosphorus is allowed to cool inside the ball mill, water is poured over it and the whole is subjected to wet-grinding. An aqueous suspension of red phosphorus is finally removed from the ball mill.
摘要翻译：本发明涉及一种通过使熔融黄磷在封闭反应区中进行热转化反应来制备红磷的装置。为此，空心轴提供和封闭的球磨机被预热到280℃至590℃的反应温度。黄磷通过空心轴以每单位时间的量连续地引入球磨机，这允许球磨机内部的反应温度保持不受外界的热量的限制。更特别地，在增加的温度下每单位时间引入黄磷的量减少，并且在规定的限度内在逐渐降低的温度下每单位时间引入增加量的黄磷。使红磷在球磨机内冷却，将水倒在其上，整体进行湿磨。最终从球磨机中除去红磷水悬浮液。

9. 发明授权

US4278647A Production of phosphorous acid 失效
标题翻译：生产亚磷酸
公开(公告)号：US4278647A
公开(公告)日：1981-07-14
申请号：US60659
申请日：1979-07-25
申请人： Klaus Jodden , Hans-Werner Stephan , Gero Heymer
发明人： Klaus Jodden , Hans-Werner Stephan , Gero Heymer
IPC分类号： C01B25/163 , C01B25/16 , C01B25/26
CPC分类号： C01B25/163
摘要： The invention relates to a process for making aqueous phosphorous acid solutions by admixing an aqueous sodium phosphite solution with hydrochloric acid. More specifically, phosphorous acid solutions substantially free from sodium in hydrochloric acid are produced by introducing hydrogen chloride, into the sodium phosphite solution until the latter is saturated therewith and separating precipitating sodium chloride from the resulting phosphorous acid solution in hydrochloric acid.
摘要翻译：本发明涉及通过将亚磷酸钠水溶液与盐酸混合来制备亚磷酸水溶液的方法。更具体地说，在盐酸中基本上不含钠的亚磷酸溶液通过将氯化氢引入到亚磷酸钠溶液中而产生，直至后者被饱和，并从所得的亚磷酸溶液中在盐酸中分离沉淀的氯化钠。

10. 发明授权

US3978195A Process for the production of substantially water-insoluble linear ammonium polyphosphates 失效
标题翻译：用于生产大量不溶于水的无定形直链氨基磷酸酯的方法
公开(公告)号：US3978195A
公开(公告)日：1976-08-31
申请号：US475820
申请日：1974-06-03
申请人： Hermann Schrodter , Hans-Werner Stephan , Gero Heymer
发明人： Hermann Schrodter , Hans-Werner Stephan , Gero Heymer
IPC分类号： C01B25/40 , C05B13/06 , C01B15/16 , C01B25/26
CPC分类号： C05B13/06
摘要： Production of substantially water-insoluble linear ammonium polyphosphates of the general formula (NH.sub.4 PO.sub.3).sub.n, in which n is a number between 10 and 1000. To this end, substantially equimolecular proportions of ammonium orthophosphate and phosphorus pentoxide are reacted by heating them to temperatures within the range 170.degree. and 350.degree.C in the presence of gaseous ammonia. The reaction is effected while continuously and simultaneously mixing, kneading and comminuting the reaction material in a reactor. The reactor is closed, provided with means for the supply of solid feed material, a gas inlet and a gas outlet, a discharge opening for the removal of final product, and with mixing, kneading and comminuting implements which are rotatably secured to the inside of the reactor.

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