Method and device for preparing high-purity ammonium paratungstate by ultrasonic and microwave hydrothermal collaborative strengthening

Abstract

Disclosed are a method and a device for preparing high-purity ammonium paratungstate by ultrasonic and microwave hydrothermal collaborative strengthening. The device comprises a magnetic stirrer, a microwave generator, an ultrasonic generator, a three-neck flask, a temperature sensor and the like. The method includes the steps that an ammonium tungstate solution with tungsten trioxide which has a concentration of no less than 220g / l is placed in the three-neck flask, the magnetic stirrer is opened, stirring is performed at a stirring speed of 70-300rpm, the microwave generator and the ultrasonic generator are opened, the powers of both the microwave generator and the ultrasonic generator are set to 1-3KW, the microwave frequency is 0.5-1.5Hz, the ultrasonic frequency is 100-200KHz, the ammonium tungstate solution is heated in an ultrasonic and microwave hydrothermal mode, a camera and the temperature sensor are simultaneously opened, when the heating temperature reaches to 80 DEG C, hydrothermal evaporation and crystallization are performed, the temperature is controlled above 80 DEG C, and the crystallization rate is controlled within 65% to obtain a high-purity ammonium paratungstate product. The prepared ammonium paratungstate by the method is high in purity.

Description

technical field [0001] The invention relates to the field of preparing ammonium paratungstate, in particular to a method and equipment for preparing high-purity ammonium paratungstate by means of ultrasonic microwave hydrothermal synergistic strengthening. Background technique [0002] Ammonium paratungstate (APT) is an important intermediate compound for the production of tungsten powder, tungsten wire, tungsten-based alloy and all tungsten materials, and it is also a bulk export commodity in my country. Due to the genetic relationship, the crystal characteristics of APT, such as crystal morphology, lattice parameters, average particle size and particle size distribution, bulk specific gravity and fluidity, have a great influence on the material properties of subsequent powder metallurgy products tungsten powder, tungsten wire and tungsten alloy, so The development of high-performance tungsten materials has put forward higher and higher requirements on the characteristics o...

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Problems solved by technology

[0009]① The cost of recovering alkali is high

Generally, the direct energy cost of recovering 1t of alkali is 1-1.5 times of the value of the alkali itself, and the production cost per unit of product will increase exponentially when dealing with low-grade ore, which is difficult for most manufacturers to accept

[0010]② When dealing with low-grade ore or complex ore, the beneficiation agent brought in the raw material will cause foaming during evaporation and concentration, which will lead to production failure in severe cases. Increased the difficulty of operation

[0011]③ It is difficult to separate the crystallized sodium tungstate crystals from the alkali, which requires high equipment requirements and increases equipment investment, maintenance and operation costs

[0012]④ Increased processing procedures and increased labor intensity of workers

[0013](2) The precipitation aluminum removal process uses more expensive copper-containing reagents, and when dealing with high-alumina ore, the production cost is high

[0014] In summary, the currently commonly used tungsten smelting process has the disadvantages that it is difficult to recover residual alkali and the cost of phase removal is high when processing high-alumina ore, which needs to be improved

[0015] In addition, the existing methods and equipment for preparing high-purity ammonium paratungstate produce high-purity ammonium paratungstate with high impurity content, and the production cannot meet the requirements of high-purity ammonium paratungstate. Therefore need to provide a kind of better preparation method and equipment

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