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。

公开(公告)号：US3980711A

公开(公告)日：1976-09-14

申请号：US549174

申请日：1975-02-12

申请人： Bernd Lippsmeier ,  Klaus Hestermann ,  Gero Heymer

发明人： Bernd Lippsmeier ,  Klaus Hestermann ,  Gero Heymer

IPC分类号： B01J31/00 ,  C07F9/53 ,  C07F9/02

CPC分类号： C07F9/53

摘要： Methylphosphine oxides of the general formula (I) ##EQU1## are produced from hydroxymethylphosphines of the general formula (II) ##EQU2## in which formulae R and R' each stand for identical or different alkyl-, cycloalkyl-, aralkyl- or aryl groups having from 1 to 18 carbon atoms, or carrying substituents being inert under the reaction conditions.The methylphosphine oxides are more particularly produced by subjecting the hydroxymethylphosphines to a rearrangement reaction with the aid of radical-yielding compounds.

摘要翻译： 由通式（I）R HOCH2-P ANGLE（II）R'的羟甲基膦制备通式（I）的二甲基膦氧化物。其中式R和R'各自为 代表具有1至18个碳原子的相同或不同的烷基 - ，环烷基 - ，芳烷基 - 或芳基，或在反应条件下携带取代基是惰性的。

公开(公告)号：US3956462A

公开(公告)日：1976-05-11

申请号：US451911

申请日：1974-03-18

申请人： Gero Heymer ,  Wolfgang Scheibitz ,  Hasso Spott

发明人： Gero Heymer ,  Wolfgang Scheibitz ,  Hasso Spott

IPC分类号： C01B25/06 ,  C01B25/16 ,  C01B25/24 ,  C01B25/00

CPC分类号： C01B25/06 ,  C01B25/16

摘要： Waste material consisting substantially of contaminated phosphorous acid is utilized. To this end, the phosphorous acid is introduced, with agitation into a liquid phase. Liquid phase and phosphorous acid are maintained in a ratio by volume between 1:1 and 10:1. The liquid phase is placed in a reactor, maintained between 250.degree. and 400.degree.C and selected from a phosphoric acid of the general formula H.sub.n.sub.+2 P.sub.n O.sub.3n.sub.+1, in which n substantially stands for a number between 1 and 5. Resulting hydrogen phosphide is removed. In the event of continuous operation, newly formed liquid phase is removed from the reactor, at the same rate as it is being formed.

摘要翻译： 使用基本上由污染的亚磷酸组成的废料。 为此，在搅拌下将亚磷酸引入液相中。 液相和亚磷酸的体积比保持在1:1至10:1之间。 将液相置于保持在250℃至400℃的反应器中，并选自通式为Hn + 2PnO3n + 1的磷酸，其中n基本上代表1至5之间的数字。产生的磷化氢为 删除。 在连续操作的情况下，新形成的液相以与形成的相同的速率从反应器中除去。

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。

公开(公告)号：US4639331A

公开(公告)日：1987-01-27

申请号：US603120

申请日：1984-04-23

申请人： Georg Elsner ,  Horst Staendeke ,  Gero Heymer

发明人： Georg Elsner ,  Horst Staendeke ,  Gero Heymer

IPC分类号： C08L1/00 ,  A62D1/00 ,  C01B25/40 ,  C08G18/00 ,  C08K3/32 ,  C08K9/04 ,  C08K9/08 ,  C08K9/10 ,  C08L75/00 ,  C08L75/04 ,  C09K21/02 ,  C09K21/04 ,  C09K21/12 ,  D06M11/00 ,  D06M11/72 ,  D06M15/423 ,  D06M23/12 ,  D06M101/00 ,  D06M101/02 ,  D06M101/06 ,  D06M101/08 ,  D21H17/10 ,  D21H17/47 ,  D21H17/51 ,  D21H17/63 ,  D21H21/34 ,  D21H27/00 ,  C08K3/28 ,  C09K21/10

CPC分类号： C01B25/405 ,  C08K3/32 ,  C08K9/08 ,  C08K9/10 ,  C09K21/02 ,  C09K21/12 ,  D21H5/0002 ,  D21H21/34 ,  Y10S521/907

摘要： The disclosure relates to a process for making a particulate agent stable to hydrolysis based on free-flowing, pulverulent ammonium polyphosphate by treating the ammonium polyphosphate with a thermosetting, artificial resin being water-insoluble when cured. More specifically, the disclosure provides for the ammonium polyphosphate, an aliphatic alcohol as a diluent, and a melamine/formaldehyde-resin or phenol/formaldehyde-resin to be placed in an autoclave and intimately mixed at room temperature; for the mixture to be heated to a temperature of about 80.degree. to about 180.degree. C. and allowed to remain over a period of 15 to 240 minutes at that temperature and under the pressure corresponding to the vapor pressure of the diluent; for the diluent to be separated and for the product so obtained to be dried.

摘要翻译： 本公开涉及一种通过在固化时用热固性人造树脂处理水不溶性的方法，通过用聚酰亚胺铵处理聚磷酸铵来制备基于自由流动的多磷酸铵的水解稳定的颗粒剂的方法。 更具体地，本公开内容提供了多磷酸铵，脂肪醇作为稀释剂，将三聚氰胺/甲醛树脂或酚/甲醛树脂置于高压釜中并在室温下充分混合; 将混合物加热到约80℃至约180℃的温度，并在该温度和在与稀释剂的蒸汽压力相对应的压力下保持15至240分钟的时间; 用于分离稀释剂和所得产品进行干燥。

公开(公告)号：US4601887A

公开(公告)日：1986-07-22

申请号：US428947

申请日：1982-09-30

申请人： Friedrich-Wilhelm Dorn ,  Manfred Wolter ,  Gero Heymer

发明人： Friedrich-Wilhelm Dorn ,  Manfred Wolter ,  Gero Heymer

IPC分类号： C09C1/00 ,  C09C1/56 ,  F27B9/06 ,  C01B31/04 ,  C09C1/46

CPC分类号： C09C1/56 ,  C01P2006/12

摘要： The invention relates to improving the degree of graphitization of carbon black produced by subjecting hydrocarbons which are liquid or gaseous under normal conditions to a thermal conversion reaction in the presence of oxygen or an oxygen-containing gas and steam, if desired, at temperatures of 1200.degree. to 2000.degree. C. and pressures of 1 to 80 bars. To this end, the carbon black is conveyed downwardly in a quasi-fluid state, within 1 to 5 hours through a sojourn zone in upright position, the sojourn zone being maintained at a temperature of at least 1200.degree. C.The invention relates to an apparatus for carrying out this process, the apparatus comprising a graphite tube; a steel container concentrically surrounding the graphite tube; a feed pipe penetrating into the interior of the graphite tube; a water-cooled discharge means; and a nitrogen feed inlet arranged below the lower end of the graphite tube; the space left between the graphite tube and steel container being occupied by insulating material.

摘要翻译： 本发明涉及通过在氧气或含氧气体和蒸汽的存在下，在正常条件下对液态或气态烃进行热转化反应，如果需要，在1200℃的温度下，提高炭黑的石墨化程度 DEG至2000℃，压力为1至80巴。 为此，炭黑在准流体状态下通过直立位置的居住区域在1至5小时内向下输送，住宅区域保持在至少1200℃的温度。本发明涉及一种 用于执行该处理的装置，该装置包括石墨管; 围绕石墨管的钢制容器; 进料管穿入石墨管的内部; 水冷式排放装置; 以及配置在所述石墨管的下端下方的氮气进料口; 石墨管和钢容器之间留下的空间被绝缘材料占据。

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。

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。

公开(公告)号：US4457848A

公开(公告)日：1984-07-03

申请号：US412142

申请日：1982-08-27

申请人： Gunther Schimmel ,  Reinhard Gradl ,  Gero Heymer

发明人： Gunther Schimmel ,  Reinhard Gradl ,  Gero Heymer

IPC分类号： C01B25/32 ,  C01B25/234 ,  C01B25/46 ,  C01F11/46 ,  C02F1/52 ,  C02F1/66 ,  C01B25/26

CPC分类号： C02F1/66 ,  C01B25/461 ,  C02F1/5236 ,  Y10S210/906

摘要： The disclosure relates to a process for after-treating extraction residues, termed raffinates, originating from the extractive decontamination of crude phosphoric acid. To this end, the disclosure provides for the raffinates to be converted to two separate solid matter fractions of differant chemical composition by admixing the raffinates with a calcium compound so as to establish a pH-value of 1.2 up to 2.5. Next, the resulting precipitate consisting essentially of gypsum is filtered off as a first solid matter fraction, and washed with water. The resulting filtrate and the wash water are made into a mixture and predetermined proportions of calcium compound are added so as to obtain, after complete reaction, a fully reacted filter cake with a pH-value of 9 up to 12, the resulting suspension being filtered off at a pH-value of 6 to 8. The filter cake consisting essentially of calcium phosphate is separated as the second solid matter fraction, and allowed to react completely.

摘要翻译： 本公开涉及用于后处理来自粗磷酸的萃取去污的萃取残余物（称为残油）的方法。 为此，本公开内容提供了通过将残液与钙化合物混合而将残液物转化为两种不同化学成分的固体物质组分，以便建立1.2至2.5的pH值。 接下来，将所得到的基本上由石膏组成的沉淀物作为第一固体成分进行过滤，并用水洗涤。 将所得滤液和洗涤水制成混合物，并加入预定比例的钙化合物，以便在完全反应后获得pH值为9至12的完全反应的滤饼，将所得悬浮液过滤 在pH值为6至8的情况下，基本上由磷酸钙组成的滤饼作为第二固体成分分离，并使其完全反应。

公开(公告)号：US4368179A

公开(公告)日：1983-01-11

申请号：US209845

申请日：1980-11-24

申请人： Gunther Shimmel ,  Gero Heymer ,  Hasso Scott

发明人： Gunther Shimmel ,  Gero Heymer ,  Hasso Scott

IPC分类号： C01B25/30 ,  C01B25/41 ,  C01B25/42 ,  C01B15/16 ,  C01B25/26

CPC分类号： C01B25/30 ,  C01B25/41 ,  C01B25/425

摘要： The present invention relates to a process for the oxidation of alkali metal phosphites to alkali metal phosphates at temperatures of between 400.degree. and 500.degree. C. To this end, alkali metal phosphites are employed in the form of an aqueous solution or suspension and, if necessary, the alkali metal : P atomic ratio in this feed material is adjusted to a ratio which at least corresponds to the atomic ratio desired for the final product.More particularly, the solution or suspension is spray-dried in a tower, in a single operational stage, by spraying in a flame zone. Starting material free from alkali metal phosphate and with an alkali metal : P atomic ratio equal to or greater than 3.5 is used for making a trialkali metal phosphate which is obtained in admixture with an alkali metal hydroxide. Starting material which contains from 25 to 45% by weight of alkali metal phosphate, calculated as phosphorus, based on their total phosphorus content, is employed for making alkali metal polyphosphates.

摘要翻译： 本发明涉及在400〜500℃的温度下将碱金属亚磷酸盐氧化为碱金属磷酸盐的方法。为此，碱金属亚磷酸盐以水溶液或悬浮液的形式使用，如果 必要时，将该原料中的碱金属：P原子比调节至至少对应于最终产物所需的原子比的比例。 更具体地说，溶液或悬浮液在塔中在单个操作阶段通过在火焰区域中喷雾进行喷雾干燥。 使用不含碱金属磷酸盐和碱金属的原料：P原子比等于或大于3.5，用于制备与碱金属氢氧化物混合得到的三碱金属磷酸盐。 使用含有25〜45重量％碱金属磷酸盐的起始原料，以磷总计计为磷，用于制造碱金属多磷酸盐。