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    • 2. 发明公开
    • Method of producing crystalline ammonium metatungstate
    • Verfahren zur Herstellung von kristallinem Ammoniummetawolframat。
    • EP0193171A2
    • 1986-09-03
    • EP86102455.2
    • 1986-02-25
    • GTE Products Corporation
    • Boyer, Carl W.Ennis, Donald H.Kim, Tai K.McInnis, Martin B.
    • C01G41/00
    • C01G41/00
    • A method is disclosed for producing crystalline ammonium metatungstate from ammonium paratungstate. The method involves heating the ammonium paratungstate in a multiple hearth furnace at from about 200°C to about 400°C to form a relatively uniformly heated ammonium paratung-state. Then in one embodiment of the method the heated ammonium paratungstate is digested in water by adding it to the water in separate portions, the addition of each portion being followed by heating the respective resulting mixture at from about 80 to 100°C for from about 5 to about 13 hours at relatively constant volume while maintaining the pH of the respective resulting mixture at from about 3.5 to about 4.5 by the addition of ammonia as necessary. The addition of the separate portions of the heated ammonium paratungstate is carried out until the concentration of the resulting aqueous ammonium metatungstate solution reaches about 260 grams of W0 3 per liter. In an alternative embodiment a slurry of the heated ammonium paratungstate in water is then digested at from about 70°C to about 100°C for less than about 6 hours at a relatively constant volume while maintaining the pH of the slurry at from about 4.2 to about 3.0 by the addition of ammonia as necessary to form a solution of ammonium metatungstate. The resulting ammonium metatungstate solution is then evaporated to a fraction of its original volume to concentrate it, any insoluble material is separated from the solution, and the ammonium metatungstate is then crystallized from the concentrated solution.
    • 公开了从仲钨酸铵生产结晶态偏钨酸铵的方法。 该方法包括在约200℃至约400℃的多床炉中加热仲钨酸铵以形成相对均匀加热的仲钨酸铵。 然后在该方法的一个实施方案中,加热的仲钨酸铵在水中通过在分开的部分中加入到水中而消化,每个部分的加入之后,将各自所得混合物在约80至100℃加热约5 至约13小时,同时通过根据需要通过加入氨维持各自所得混合物的pH为约3.5至约4.5。 加入加热的仲钨酸铵的单独部分进行直到所得到的多余的Metetungstate溶液的浓度达到每升约260克的WO 3。 在替代实施方案中,然后将加热的仲钨酸铵在水中的浆料以相对恒定的体积在约70℃至约100℃下消化少于约6小时,同时将浆料的pH保持在约4.2至约 根据需要通过加入氨来制备约3.0,以形成偏钨酸铵的溶液。 然后将所得的偏钨酸铵溶液蒸发至其原始体积的一部分以使其浓缩,将任何不溶物质与溶液分离,然后将该偏钨酸铵从浓缩溶液中结晶。
    • 3. 发明公开
    • Method of producing crystalline ammonium metatungstate
    • 生产结晶白云母的方法
    • EP0193171A3
    • 1988-07-06
    • EP86102455
    • 1986-02-25
    • GTE Products Corporation
    • Boyer, Carl W.Ennis, Donald H.Kim, Tai K.McInnis, Martin B.
    • C01G41/00
    • C01G41/00
    • A method is disclosed for producing crystalline ammonium metatungstate from ammonium paratungstate. The method involves heating the ammonium paratungstate in a multiple hearth furnace at from about 200°C to about 400°C to form a relatively uniformly heated ammonium paratung-state. Then in one embodiment of the method the heated ammonium paratungstate is digested in water by adding it to the water in separate portions, the addition of each portion being followed by heating the respective resulting mixture at from about 80 to 100°C for from about 5 to about 13 hours at relatively constant volume while maintaining the pH of the respective resulting mixture at from about 3.5 to about 4.5 by the addition of ammonia as necessary. The addition of the separate portions of the heated ammonium paratungstate is carried out until the concentration of the resulting aqueous ammonium metatungstate solution reaches about 260 grams of W0 3 per liter. In an alternative embodiment a slurry of the heated ammonium paratungstate in water is then digested at from about 70°C to about 100°C for less than about 6 hours at a relatively constant volume while maintaining the pH of the slurry at from about 4.2 to about 3.0 by the addition of ammonia as necessary to form a solution of ammonium metatungstate. The resulting ammonium metatungstate solution is then evaporated to a fraction of its original volume to concentrate it, any insoluble material is separated from the solution, and the ammonium metatungstate is then crystallized from the concentrated solution.
    • 5. 发明公开
    • Method of producing crystalline ammonium metatungstate
    • 生产结晶偏钨酸铵的方法
    • EP0196027A1
    • 1986-10-01
    • EP86103907.1
    • 1986-03-21
    • GTE Products Corporation
    • Kim, Tai K.McClintic, Robert P.
    • C01G41/00
    • C01G41/00
    • A method is disclosed for producing crystalline ammonium metatungstate from ammonium paratungstate. The method involves heating the ammonium paratungstate at from about 130 to about 400°C for from about 1 to about 8 hours to remove some ammonia and water, and heating a slurry of the resulting heated ammonium paratungstate in water at from about 80 to about 100°C at relatively constant volume until the pH of the slurry becomes stabilized at from about 5.8 to about 6.0. The pH of the resulting pH stabilized slurry is then adjusted to from about 4.2 to about 3.0 by introducing a porous container containing a strongly acidic cation exchange resin into the slurry, the amount of resin being essentially sufficient to accomplish the pH adjustment. Thereafter the container and resin are removed from the resulting pH adjusted slurry which is then digested at from about 80 to about 100°C for from about 2 to about 6 hours at relatively constant volume to form a solution of ammonium metatungstate. The solution is then evaporated to a fraction of its original volume to concentrate it. Any insoluble material is then separated from the solution, and ammonium metatungstate is.crystallized from the solution.
    • 公开了一种由仲钨酸铵生产结晶偏钨酸铵的方法。 该方法包括将仲钨酸铵在约130至约400℃加热约1至约8小时以除去一些氨和水,并且将所得的加热的仲钨酸铵在水中的浆液加热至约80至约100 ℃,体积相对恒定,直到浆液的pH值稳定在约5.8至约6.0。 通过将含有强酸性阳离子交换树脂的多孔容器引入浆料中,将得到的pH稳定的浆料的pH调节至约4.2至约3.0,该树脂的量基本上足以实现pH调节。 此后,将容器和树脂从所得的调节过的pH值的浆液中除去,然后在约80至约100℃下以相对恒定的体积将其消化约2至约6小时以形成偏钨酸铵溶液。 然后将溶液蒸发至其原始体积的一部分以浓缩它。 然后将任何不溶物质从溶液中分离出来,偏钨酸铵从溶液中结晶出来。