公开(公告)号：US08741226B2

公开(公告)日：2014-06-03

申请号：US13321975

申请日：2010-05-27

申请人： Xiaomei Feng ,  Jin Li ,  Dong Li ,  Guangming Li ,  Zhenmin Zhang ,  Jiacai Wang ,  Jian Zou ,  Yongqiang Ma ,  Jun Hou

发明人： Xiaomei Feng ,  Jin Li ,  Dong Li ,  Guangming Li ,  Zhenmin Zhang ,  Jiacai Wang ,  Jian Zou ,  Yongqiang Ma ,  Jun Hou

IPC分类号： B01J19/00 ,  C01B25/00

CPC分类号： F27D3/16 ,  C01B25/01 ,  C01B25/02 ,  C01B25/04 ,  F27B1/10

摘要： The present invention discloses a reduction-oxidation furnace for thermally refining phosphorus. The reduction-oxidation furnace comprises a furnace body and a blow gun, wherein the furnace body has a slag outlet, a fume outlet, and a melt inlet for feeding melts formed by melting rock phosphate into the furnace body and wherein the blow gun has an end inserted into the furnace body. The content of impurities in fumes containing phosphorus pentaoxide is low, the phosphorus pentaoxide can be easily extracted with a high purity of the phosphorus pentaoxide and at low cost by means of the reduction-oxidation furnace for thermally refining phosphorus according to the present invention.

摘要翻译： 本发明公开了一种用于热精炼磷的还原氧化炉。 还原氧化炉包括炉体和吹气枪，其中炉体具有炉渣出口，烟气出口和用于将熔融磷酸盐熔融形成的熔体进料到炉体中的熔体入口，并且其中喷枪具有 端插入炉体。 含有五氧化二磷的烟气中的杂质含量低，五氧化二磷可以用五氧化二磷的高纯度容易地提取，并且通过根据本发明的用于热精炼磷的还原氧化炉以低成本提取。

公开(公告)号：US20110212405A1

公开(公告)日：2011-09-01

申请号：US13026506

申请日：2011-02-14

申请人： Yongli Mi ,  Xiaoping Wang ,  Zhen Zhang ,  Xiaojin He

发明人： Yongli Mi ,  Xiaoping Wang ,  Zhen Zhang ,  Xiaojin He

IPC分类号： F24J3/00

CPC分类号： C01B25/04 ,  Y02P20/123

摘要： In general, the present invention relates to the production of ultrapure phosphorus. In particular, the present invention relates to the method for the production of ultrapure phosphorus by zone melting in a Non-flammable environment and the equipments used in such method. The process of the present invention is clean, chemical free, fast, and energy efficient.

摘要翻译： 通常，本发明涉及超纯磷的生产。 特别地，本发明涉及在不易燃环境中通过区域熔融生产超纯磷的方法和该方法中使用的设备。 本发明的方法是清洁，无化学，快速和节能的。

公开(公告)号：US5296212A

公开(公告)日：1994-03-22

申请号：US871422

申请日：1992-04-21

申请人： Arndt Zschalich ,  Rudolf Schumann

发明人： Arndt Zschalich ,  Rudolf Schumann

IPC分类号： C01B25/04 ,  C01B25/047

CPC分类号： C01B25/04

摘要： A method for purifying white phosphorus contaminated with sulfur bound thereto involves contacting contaminated white phosphorus with water, steam, aqueous solutions, or vaporized aqueous solutions, preferably alkaline, to remove bound sulfur from the phosphorus. The purified phosphorus is characterized by a sulfur content as low as 50 ppm.

摘要翻译： 用于净化被硫结合的硫被污染的白磷的方法包括将受污染的白磷与水，蒸汽，水溶液或蒸发的水溶液（优选碱性）接触，以从磷中除去结合的硫。 纯化的磷的特征在于低至50ppm的硫含量。

公开(公告)号：US4620968A

公开(公告)日：1986-11-04

申请号：US419537

申请日：1982-09-17

申请人： Christian G. Michel ,  Rozalie Schachter ,  Mark A. Kuck ,  John A. Baumann ,  Paul M. Raccah

发明人： Christian G. Michel ,  Rozalie Schachter ,  Mark A. Kuck ,  John A. Baumann ,  Paul M. Raccah

IPC分类号： C01B25/00 ,  C01B25/02 ,  C01B25/04 ,  C01B25/08 ,  C03C17/22 ,  C09K21/04 ,  C23C14/06 ,  C23C14/54 ,  C30B23/02 ,  C30B25/02 ,  H01L29/24 ,  H01L51/05 ,  C01B25/01 ,  C04B35/00

CPC分类号： H01L29/24 ,  C01B25/003 ,  C01B25/02 ,  C01B25/04 ,  C01B25/08 ,  C01B25/081 ,  C01B25/088 ,  C03C17/22 ,  C09K21/04 ,  C23C14/06 ,  C23C14/541 ,  C30B23/02 ,  C30B25/02 ,  C30B29/10 ,  C03C2217/28 ,  C03C2217/283 ,  C03C2217/29 ,  C03C2218/15 ,  H01L51/0508 ,  H01L51/0512

摘要： Monoclinic phosphorus is produced in a single source vapor transport apparatus comprising a sealed evacuated ampoule containing a mixture or compound of phosphorus and an alkali metal with the phosphorus to alkali metal ratio being 11 or greater. The charge is heated to 550.degree.-560.degree. C. and the monoclinic phosphorus crystals are formed on the cooler surface at the top of the ampoule over the temperature range of 500.degree.-560.degree. C. The preferred heating temperature is in the neighborhood of 555.degree. C. and the preferred deposition temperature is in the neighborhood of 539.degree. C. Alkali metals that may be employed include sodium, potassium, rubidium and cesium. The monoclinic phosphorus crystals form in two habits. Those formed in the presence of sodium and cesium are in the form of flat square platelets up to 4 mm on a side and 2 mm thick. These platelets may be easily cleaved into thinner platelets, like mica. The other habit formed in the presence of potassium and rubidium is in the form of a truncated pyramid up to 4 mm.times.3 mm.times.2 mm high. This habit is hard to cleave. The crystals are semiconductors with a band gap, indicated by photoluminescence, of about 2.1 eV at room temperature. Powder X-ray diffraction, and differential thermal analysis are consistent with that reported for Hittorf's phosphorus prepared according to the prior art. The crystals are a deep red on transmission and birefringent, rotating the plane of polarization in a polarizing microscope. They contain from 50 to 2000 parts per million of alkali metal and therefore may be utilized as a form of very pure phosphorus as well as for their semiconducting and birefringent qualities and as phosphors.

摘要翻译： 在单源蒸气输送装置中制备单斜磷，其包括含有磷与碱金属的比例为11以上的磷和碱金属的混合物或化合物的密闭的真空安瓿。 将电荷加热至550〜-560℃，在500〜-560℃的温度范围内，在安瓿顶部的较冷的表面形成单斜晶磷晶体。优选的加热温度在 555℃，优选的沉积温度在539℃附近。可以使用的碱金属包括钠，钾，铷和铯。 单斜磷晶体形成两种习惯。 在钠和铯存在下形成的那些是平面方形血小板的形式，一侧高达4毫米，2mm厚。 这些血小板可以容易地切割成更薄的血小板，如云母。 在钾和铷存在下形成的另一个习惯是高达4毫米×3毫米×2毫米高的截顶棱锥的形式。 这种习惯很难解剖。 晶体是在室温下具有约2.1eV的光致发光带隙的半导体。 粉末X射线衍射和差示热分析与根据现有技术制备的Hittorf磷报道的一致。 晶体是透射和双折射的深红色，在偏光显微镜中旋转偏振平面。 它们含有50至2000ppm的碱金属，因此可以用作非常纯的磷以及它们的半导体和双折射性质以及作为荧光体的形式。

公开(公告)号：US1984674A

公开(公告)日：1934-12-18

申请号：US69957833

申请日：1933-11-24

申请人： RUMFORD CHEMICAL WORKS

发明人： FISKE AUGUSTUS H ,  BRYAN CHARLES S

IPC分类号： C01B25/04

CPC分类号： C01B25/003 ,  C01B25/01 ,  C01B25/04

公开(公告)号：US20150175423A1

公开(公告)日：2015-06-25

申请号：US14409487

申请日：2013-06-21

申请人： Outotec (Finland) Oy

发明人： Dirk Lohrberg ,  Bertold Stegemann ,  Guenter Schneider ,  Ludwig Hermann

IPC分类号： C01B25/04 ,  B01J8/18 ,  B01J8/24

CPC分类号： C01B25/04 ,  B01J8/1836 ,  B01J8/24 ,  B01J2208/00017 ,  C02F11/004 ,  C02F11/10 ,  C02F2101/20 ,  C05B7/00 ,  Y02P20/129

摘要： A process for separating heavy metals from a phosphoric starting material includes, in a step (i), heating the starting material to a temperature between 700 and 1,100° C. in a first reactor and withdrawing combustion gas. In a step (ii), the heated starting material at the temperature between 700 and 1,100° C. is transferred to a second reactor, chlorides of alkaline and earth alkaline metals are added and process gas is withdrawn.

摘要翻译： 从磷酸原料中分离重金属的方法包括在步骤（i）中，将起始原料在第一反应器中加热至700至1100℃的温度并排出燃烧气体。 在步骤（ii）中，将加热的起始材料在700和1100℃之间的温度下转移到第二反应器中，加入碱金属和碱土金属的氯化物并除去工艺气体。

公开(公告)号：US08747792B2

公开(公告)日：2014-06-10

申请号：US13179882

申请日：2011-07-11

申请人： Yutaka Kinose ,  Toru Hata ,  Mari Aikawa

发明人： Yutaka Kinose ,  Toru Hata ,  Mari Aikawa

IPC分类号： C01B25/02 ,  C01B25/04 ,  C01B25/20

CPC分类号： C01B25/02 ,  C01B25/04 ,  C01B25/20

摘要： Provided is a method for preparing high-purity elemental phosphorus capable of simultaneously reducing both arsenic and antimony from crude white phosphorus containing a great amount of arsenic and antimony as impurities. Provided is a method for preparing high-purity elemental phosphorus, the method including bringing liquid crude white phosphorus into contact with an iodic acid-containing compound selected from iodic acid and iodates in an aqueous solvent in the presence of a chelating agent, wherein the chelating agent is selected from polyvalent carboxylic acids, polyvalent carboxylates, phosphonic acid and phosphonates.

摘要翻译： 本发明提供一种能够同时从含有大量砷和锑作为杂质的粗白磷中同时还原砷和锑的高纯度元素磷的方法。 本发明提供一种制备高纯度元素磷的方法，其特征在于，在螯合剂的存在下，在含水溶剂中使液态粗白磷与选自碘酸和碘酸的碘​​酸化合物接触， 试剂选自多价羧酸，多价羧酸酯，膦酸和膦酸酯。

公开(公告)号：US5310530A

公开(公告)日：1994-05-10

申请号：US117884

申请日：1993-09-07

申请人： Arndt Zschalich ,  Rudolf Schumann

发明人： Arndt Zschalich ,  Rudolf Schumann

IPC分类号： C01B25/04

CPC分类号： C01B25/04

摘要： A method for purifying phosphorus to insure a low sulfur content involves intensively mixing phosphorus and concentrated sulfuric acid to form an emulsion, breaking the emulsion by contact with water or dilute sulfuric acid, and then immediately separating the phosphorus and diluted sulfuric acid. The separated phosphorus is then stored in water until further processing is desired and is characterized by a sulfur content as low as about 50 ppm.

摘要翻译： 用于纯化磷以确保低硫含量的方法包括浓缩磷和浓硫酸形成乳液，通过与水或稀硫酸接触来破坏乳液，然后立即分离出磷和稀硫酸。 然后将分离的磷储存在水中直至需要进一步处理，其特征在于低至约50ppm的硫含量。

公开(公告)号：US5032472A

公开(公告)日：1991-07-16

申请号：US322688

申请日：1989-03-13

申请人： Christian G. Michel ,  Rozalie Schachter ,  Mark A. Kuck ,  John A. Baumann ,  Paul M. Raccah

发明人： Christian G. Michel ,  Rozalie Schachter ,  Mark A. Kuck ,  John A. Baumann ,  Paul M. Raccah

IPC分类号： C01B25/00 ,  C01B25/02 ,  C01B25/04 ,  C01B25/08 ,  C03C17/22 ,  C09K21/04 ,  C23C14/06 ,  C23C14/24 ,  C23C14/54 ,  C30B23/02 ,  C30B25/02 ,  H01L21/28 ,  H01L21/314 ,  H01L21/3205 ,  H01L21/363 ,  H01L23/29 ,  H01L23/31 ,  H01L29/24 ,  H01L29/49 ,  H01L29/51 ,  H01L29/812 ,  H01L31/032 ,  H01L51/00 ,  H01L51/05 ,  H01L51/40

CPC分类号： H01L51/0541 ,  C01B25/003 ,  C01B25/02 ,  C01B25/04 ,  C01B25/08 ,  C01B25/081 ,  C01B25/088 ,  C03C17/22 ,  C09K21/04 ,  C23C14/06 ,  C23C14/24 ,  C23C14/541 ,  C30B23/02 ,  C30B25/02 ,  C30B29/10 ,  H01L21/02422 ,  H01L21/02521 ,  H01L21/02576 ,  H01L21/02581 ,  H01L21/02631 ,  H01L21/28167 ,  H01L21/314 ,  H01L21/32051 ,  H01L23/291 ,  H01L23/3171 ,  H01L29/24 ,  H01L29/4908 ,  H01L29/51 ,  H01L29/8126 ,  H01L31/032 ,  H01L51/0545 ,  C03C2217/28 ,  C03C2217/283 ,  C03C2217/29 ,  C03C2218/15 ,  H01L2924/0002 ,  H01L51/001 ,  H01L51/0508 ,  H01L51/0512

摘要： High phosphorus polyphosphides, namely MP.sub.x, where M is an alkali metal (Li, Na, K, Rb, and Cs) or metals mimicking the bonding behavior of an alkali metal, and x=7 to 15 or very much greater than 15 (new forms of phosphorus) are useful semiconductors in their crystalline, polycrystalline and amorphous forms (boules and films). MP.sub.15 appears to have the best properties and KP.sub.15 is the easier to synthesize. P may include other pnictides as well as other trivalent atomic species. Resistance lowering may be accomplished by doping with Ni, Fe, Cr, and other metals having occupied d or f outer electronic levels; or by incorporation of As and other pnictides. Top contacts forming junction devices doped with Ni and employing Ni as a back contact comprise Cu, Al, Mg, Ni, Au, Ag, and Ti. Photovoltaic, photoresistive, and photoluminescent devices are also disclosed. All semiconductor applications appear feasible.These semiconductors belong to the class of polymer forming, trivalent atomic species forming homatomic, covalent bonds having a coordination number slightly less than 3. The predominant local order appears to be all parallel pentagonal tubes in all forms, including amorphous, except for the monoclinic and twisted fiber allotropes of phosphorus.Large crystal monoclinic phosphorus (a birefringent material) in two habits, a twisted fiber phosphorus allotrope and a star shaped fibrous high phosphorus material are also disclosed.Single and multiple source vapor transport, condensed phase, melt quench, flash evaporation, chemical vapor deposition, and molecular flow deposition may be employed in synthesizing these materials. Vapor transport may be employed to purify phosphorus.

摘要翻译： 高磷多磷化物，即MPx，其中M是碱金属（Li，Na，K，Rb和Cs）或模拟碱金属键合行为的金属，x = 7至15或非常大于15（新 磷的形式）是其晶体，多晶和无定形形式（晶粒和膜）中的有用的半导体。 MP15似乎具有最好的性能，KP15更容易合成。 P可以包括其他三价物以及其它三价原子物种。 电阻降低可以通过掺杂Ni，Fe，Cr和其他具有d或f外电子水平的金属来实现; 或通过并入As和其他pnictides。 掺杂有Ni并且以Ni作为背接触的结合装置的顶部触点包括Cu，Al，Mg，Ni，Au，Ag和Ti。 还公开了光电，光致抗蚀剂和光致发光器件。 所有半导体应用似乎都是可行的。 这些半导体属于聚合物形成类型，三价原子物质形成具有略小于3的配位数的同原子，共价键。主要的局部顺序似乎是所有形式的所有平行五边形管，包括无定形，除了单斜晶和 扭曲的纤维同素异形体的磷。 还公开了两种习惯中的大晶体单斜晶磷（双折射材料），扭曲纤维磷同素异形体和星形纤维状高磷材料。 可以在合成这些材料时采用单源和多源蒸气输送，冷凝相，熔融淬火，闪蒸，化学气相沉积和分子流沉积。 可以使用蒸气传输来净化磷。

公开(公告)号：US4818636A

公开(公告)日：1989-04-04

申请号：US680367

申请日：1984-12-11

申请人： Christian G. Michel ,  Rozalie Schachter ,  Mark A. Kuck ,  John A. Baumann ,  Paul M. Raccah

发明人： Christian G. Michel ,  Rozalie Schachter ,  Mark A. Kuck ,  John A. Baumann ,  Paul M. Raccah

IPC分类号： C01B25/00 ,  C01B25/02 ,  C01B25/04 ,  C01B25/08 ,  C03C17/22 ,  C09K21/04 ,  C23C14/06 ,  C23C14/54 ,  C30B23/02 ,  C30B25/02 ,  H01L29/24 ,  H01L31/032 ,  H01L51/05 ,  B32B9/00 ,  B32B13/00

CPC分类号： H01L31/032 ,  C01B25/003 ,  C01B25/02 ,  C01B25/04 ,  C01B25/08 ,  C01B25/081 ,  C01B25/088 ,  C03C17/22 ,  C09K21/04 ,  C23C14/06 ,  C23C14/541 ,  C30B23/02 ,  C30B25/02 ,  C30B29/10 ,  H01L29/24 ,  C03C2217/28 ,  C03C2217/283 ,  C03C2217/29 ,  C03C2218/15 ,  H01L51/0508 ,  H01L51/0512

摘要： High phosphorus polyphosphides, namely MP.sub.x, where M is an alkali metal (Li, Na, K, Rb, and Cs) or metals mimicking the bonding behavior of an alkali metal, and x=7 to 15 or very much greater than 15 (new forms of phosphorus) are useful semiconductors in their crystalline, polycrystalline and amorphous forms (boules and films). MP.sub.15 appears to have the best properties and KP.sub.15 is the easier to synthesize. P may include other pnictides as well as other trivalent atomic species. Resistance lowering may be accomplished by doping with Ni, Fe, Cr, and other metals having occupied d or f outer electronic levels; or by incorporation of As and other pnictides. Top contacts forming junction devices doped with Ni and employing Ni as a back contact comprise Cu, Al, Mg, Ni, Au, Ag, and Ti. Photovoltaic, photoresistive, and photoluminescent devices are also disclosed. All semiconductor applications appear feasible.These semiconductors belong to the class of polymer forming, trivalent atomic species forming homatomic, covalent bonds having a coordination number slightly less than 3. The predominant local order appears to be all parallel pentagonal tubes in all forms, including amorphous, except for the monoclinic and twisted fiber allotropes of phosphorus.Large crystal monoclinic phosphorus (a birefringent material) in two habits, a twisted fiber phosphorus allotrope and a star shaped fibrous high phosphorus material are also disclosed.Single and multiple source vapor transport, condensed phase, melt quench, flash evaporation, chemical vapor deposition, and molecular flow deposition may be employed in synthesizing these materials. Vapor transport may be employed to purify phosphorus.The materials may be employed as protective coatings, optical coatings, fire retardants, fillers and reinforcing fillers for plastics and glasses, antireflection coatings for infrared optics, infrared transmitting windows, and optical rotators.