Ultrasonic microwave hydrothermal synergistic strengthening method and equipment for preparing high-purity ammonium paratungstate

Abstract

Ultrasonic microwave hydrothermal synergistic strengthening method and equipment for preparing high-purity ammonium paratungstate. The equipment includes a magnetic stirrer, a microwave generator, an ultrasonic generator, a three-necked flask, a temperature sensor, and the like. The specific steps of the method are: put the ammonium tungstate solution with a WO3 concentration of not less than 220g / l in a three-necked flask, turn on the magnetic stirrer, and stir at a stirring speed of 70-300rpm; turn on the microwave generator and ultrasonic The generator heats the ammonium tungstate solution with ultrasonic and microwave hydrothermal methods with a power of 1-3KW, a microwave frequency of 0.5-1.5Hz, and an ultrasonic frequency of 100-200KHz; at the same time, the camera and temperature sensor are turned on; when the heating temperature reaches At 80°C, start hydrothermal evaporation and crystallization, and control the temperature above 80°C; control the crystallization rate within 65%, that is, to produce high-purity ammonium paratungstate products. The ammonium paratungstate prepared by the invention has high 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] ①The 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] ②When 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 and increase the difficulty of operation

[0011] ③ It is difficult to separate the crystallized sodium tungstate crystals from the alkali, which requires higher equipment requirements, and at the same time increases more equipment investment, equipment maintenance and operating costs

[0012] ④The processing procedure is increased, and the labor intensity of workers increases

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

[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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