A clean process for preparing tungsten disulfide in a closed loop

Abstract

The invention discloses a cleaning process for preparing tungsten disulfide in a closed-circuit cycle. The molar ratio of tungsten, sulfur and tungsten disulfide is 1000: (2000-6000): (1-50); It is sent into a segmented box-type reaction tube under an inert atmosphere, and is kept at 230-850 °C for 1-24 hours in the high-temperature zone of the reaction tube. A sulfur recovery device is added in the air-cooled low-temperature zone of the reaction tube to realize sulfur recovery and reuse, and the water cooling effect in the cooling zone is reduced to Tungsten disulfide was obtained at room temperature. A tungsten disulfide vacuum device is connected to the side wall of the low temperature zone of the reaction tube, and tungsten disulfide is added to make the sulfur solution contain 0.05% to 10% of tungsten disulfide. The process of the invention is closed-circuit circulation and the sulfur is completely used, which solves the problem that SO is common in the traditional tungsten disulfide production process. X , H 2 S, NH 3 It has the advantages of simple process, low cost, cleanliness and environmental protection due to the problems of toxic gas emissions polluting the environment, low sulfur utilization rate, and high external energy.

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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