Cleaning process for preparing tungsten disulfide by closed-loop circulation

Abstract

The invention discloses a cleaning process for preparing tungsten disulfide by closed-loop circulation. The cleaning process comprises the following steps of: taking tungsten, sulfur and the tungsten disulfide according to the molar ratio of 1000:(2000-6000):(1:50), firstly mixing uniformly and activating by a ball mill, then feeding the mixture into a sectional box-type reaction tube under the inert atmosphere, insulating for 1-24 hours at the temperature of 230-850 DEG C of a high-temperature area of the reaction tube, adding a sulfur-recovering device at an air-cooling low-temperature area of the reaction tube to realize sulfur recovery and reuse, and reducing the temperature to room temperature under the water-cooling action of a cooling area to obtain the tungsten disulfide. A tungsten-disulfide vacuum device is arranged to be connected with the side wall of the low-temperature area of the reaction tube, and the tungsten disulfide is added to lead sulfur solution to contain 0.05%-10% of tungsten disulfide. The cleaning process disclosed by the invention has the beneficial effects that the closed-loop circulation is adopted, and sulfur is completely used, so that the problems that the environment is polluted due to discharging of toxic gases such as SOX, H2S and NH3, the sulfur utilization rate is low and the external energy is high in the traditional tungsten-disulfide production process are solved. The cleaning process disclosed by the invention has the advantages of simple process, low cost and clean and environmental-friendly effects.

Description

technical field [0001] The invention relates to a clean production process of tungsten compounds, in particular to a clean process for preparing tungsten disulfide in a closed loop. Background technique [0002] The increasing shortage of traditional energy and the deteriorating environment have greatly promoted the development of new energy and energy conservation and emission reduction. The development of new energy and energy conservation are like two sides of a coin, one is indispensable, and the two aspects have the same important status. About 1 / 3 to 1 / 2 of the energy used in the world is consumed by friction. If you can try your best to reduce useless friction consumption, you can save a lot of energy. In addition, most of the vulnerable parts of mechanical products are scrapped and replaced due to wear exceeding the limit. If the friction loss can be controlled and reduced, it will not only reduce the number and cost of equipment maintenance, but also save the cost ...

AI Technical Summary

Problems solved by technology

At present, the preparation methods of tungsten disulfide mainly include traditional high-temperature solid-phase synthesis method, chemical vapor deposition method, high-temperature thermal decomposition method, and hydrothermal method. The output of tungsten disulfide prepared above is very small, and the sulfur deposition reactor cannot production, SO X 、H 2 S, NH 3 Gas emissions pollute the environment, H 2 Easy to explode, low conversion rate, low purity of tungsten disulfide, etc.

[0005] The method of preparing tungsten disulfide through the reaction of tungsten powder and sulfur powder has long existed, but in the production process, the grinding time of tungsten powder and sulfur powder was not enough, the mixed powder could not be fully dispersed and activated, and the reaction efficiency and the purity of the reaction product decreased.

At the same time, in the liquefaction and recovery stage of excess sulfur, if no suitable lubricating material is added, part of the sulfur will adhere to the bottom of the reactor wall. Prolonged production will cause sulfur to block the reactor, and the furnace must be cleaned frequently, seriously affecting production efficiency and equipment. utilization rate

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