CN-116514066-B - Hydrofluoric acid preparation facilities

CN116514066BCN 116514066 BCN116514066 BCN 116514066BCN-116514066-B

Abstract

The invention relates to a hydrofluoric acid preparation device which comprises an oil bath heating device, a reaction tank, a fixing frame, a reverse suction prevention tank and an absorption tank, wherein the reaction tank, the reverse suction prevention tank and the absorption tank are fixed on the fixing frame, the reaction tank is partially immersed in the oil bath heating device, a first connecting pipe is arranged between an air outlet pipe of the reaction tank and an air inlet end of the reverse suction prevention tank, one end of the first connecting pipe extending into the reverse suction prevention tank is positioned at the upper part of the reverse suction prevention tank, a second connecting pipe is arranged between the absorption tank and the reverse suction prevention tank, one end of the second connecting pipe extends into the lower part of the reverse suction prevention tank, and the other end of the second connecting pipe is positioned below the liquid level of the absorption tank. The reaction tank, the anti-suck-back tank and the absorption tank are connected together, and the connecting device and the tank body are made of polytetrafluoroethylene, so that the anti-suck-back tank is corrosion-resistant and good in sealing performance, and can be used as a small-sized production device for carrying out related theoretical research on the production of hydrofluoric acid by a fluorite method.

Inventors

LI YUBIAO
ZHANG YUAN
YANG XU
SONG SHAOXIAN

Assignees

武汉理工大学

Dates

Publication Date: 20260505
Application Date: 20230413

Claims (8)

1. A hydrofluoric acid production apparatus, comprising: the anti-backflow absorbing device comprises an oil bath heating device, a reaction tank, a fixing frame, an anti-backflow absorbing tank and an absorbing tank, wherein the reaction tank, the anti-backflow absorbing tank and the absorbing tank are fixed on the fixing frame, the reaction tank is partially immersed in the oil bath heating device, a first connecting pipe is arranged between an air outlet pipe of the reaction tank and an air inlet end of the anti-backflow absorbing tank, one end of the first connecting pipe, which stretches into the anti-backflow absorbing tank, is positioned at the upper part of the anti-backflow absorbing tank, a second connecting pipe is arranged between the absorbing tank and the anti-backflow absorbing tank, one end of the second connecting pipe stretches into the lower part of the anti-backflow absorbing tank, the other end of the second connecting pipe is positioned below the liquid level of the absorbing tank, a second sealing plug is arranged at the top of the anti-backflow absorbing tank, an air inlet and an air outlet are formed in the second sealing plug, and the first connecting pipe stretches into the anti-backflow absorbing tank through the air inlet and is positioned at the upper part of the anti-backflow absorbing tank; And a magnetic stirrer is arranged in the reaction tank.
2. The hydrofluoric acid producing apparatus of claim 1, wherein: The oil bath heating device comprises an oil bath pot and a heating furnace, wherein the oil bath pot is placed on the heating furnace, silicone oil is filled in the oil bath pot, and the reaction pot is partially immersed in the silicone oil.
3. The hydrofluoric acid producing apparatus of claim 1, wherein: The top of the reaction tank is provided with a first sealing plug, an air outlet pipe of the reaction tank is arranged on the first sealing plug, and the air outlet pipe is connected with one end of the first connecting pipe through a hexagonal threaded pipe.
4. The hydrofluoric acid producing apparatus of claim 1, wherein: The secondary absorption tank is fixed on the fixing frame, a third connecting pipe is arranged between the secondary absorption tank and the absorption tank, one end of the third connecting pipe is located above the liquid level of the absorption tank, the other end of the third connecting pipe is located below the liquid level of the secondary absorption tank, and an exhaust pipe is arranged on the secondary absorption tank.
5. The hydrofluoric acid producing apparatus of claim 4, wherein: The fixing frame comprises a frame body and a plurality of clamping jaws, wherein the clamping jaws are fixed on the frame body and used for fixing the reaction tank, the anti-suck-back tank, the absorption tank and the secondary absorption tank, and the clamping jaws are used for fixing the reaction tank, the anti-suck-back tank, the absorption tank and the secondary absorption tank on the same horizontal line.
6. The hydrofluoric acid producing apparatus of claim 4, wherein: The absorption tank is characterized in that a third sealing plug is arranged at the top of the absorption tank, an air inlet and an air outlet are formed in the third sealing plug, the second connecting pipe extends into the absorption tank through the air inlet and is located below the liquid level of the absorption tank, the third connecting pipe extends into the absorption tank through the air outlet and is located above the liquid level of the absorption tank, and NaOH absorption liquid is filled in the absorption tank.
7. The hydrofluoric acid producing apparatus of claim 4, wherein: the top of the secondary absorption tank is provided with a fourth sealing plug, an air inlet and an air outlet are formed in the fourth sealing plug, the third connecting pipe extends into the secondary absorption tank through the air inlet and is positioned below the liquid level of the secondary absorption tank, the exhaust pipe extends into the secondary absorption tank through the air outlet and is positioned above the liquid level of the secondary absorption tank, and NaOH absorption liquid is filled in the secondary absorption tank.
8. The hydrofluoric acid producing apparatus of claim 4, wherein: The reaction tank, the fixing frame, the anti-suck-back tank, the absorption tank and the secondary absorption tank are made of polytetrafluoroethylene materials.

Description

Hydrofluoric acid preparation facilities Technical Field The invention relates to the technical field of hydrofluoric acid preparation, in particular to a hydrofluoric acid preparation device. Background Hydrofluoric acid is a basic raw material in the fluoride industry, is widely used for preparing products such as fluorine-containing resin, refrigerant, cryolite, aluminum fluoride, potassium fluoride and the like, and is widely applied to the fields of glass etching, petroleum industry catalysts, semiconductor, chip manufacturing and the like. The main preparation method of the hydrofluoric acid in the industry at present is a fluorite-sulfuric acid method, namely fluorite is used as a raw material to react with concentrated sulfuric acid to generate the hydrofluoric acid. The main technological process of fluorite sulfuric acid process includes adding sulfuric acid and fluorite powder in certain proportion into a rotary reaction furnace, heating the furnace wall, and making the hydrogen fluoride gas produced through the reaction pass through a coarse distillation tower, a degasser and a rectifying tower successively to obtain high purity anhydrous hydrogen fluoride. At present, a great deal of research is carried out on the aspects of preparing hydrofluoric acid by a fluorite sulfuric acid method by a plurality of domestic scholars. CN 112062091A discloses an anhydrous hydrogen fluoride production equipment and a production process thereof, wherein the production equipment comprises a crusher, a closed conveyor, a preheater, a rotary reaction furnace, a washing tower, a condensing tower, a rectifying tower and a degassing tower. CN 112142009A discloses a method for producing anhydrous hydrogen fluoride and its equipment, the equipment mainly includes fluidized bed reactor, cyclone separator, spiral reactor, spray tower, separating tank and condenser, the process uses superfine fluorite particles as raw material, mixes water vapor, sulfur trioxide vapor, sulfuric acid vapor and hydrogen fluoride gas and makes fluidized solid particles produce reaction, and the fluidized layers of all stages are in countercurrent contact, so that the mass transfer and heat transfer efficiency can be greatly raised, and the process is applicable to treating low-grade fluorite powder. The existing method for producing hydrogen fluoride by the rotary kiln only adopts fluorite powder with the calcium fluoride content of 97% and the granularity of about 100 meshes, and other processes and equipment are also suitable for industrial production, so that theoretical research cannot be carried out as small equipment, and related research on preparing hydrofluoric acid by using fluorite is greatly hindered. Therefore, developing a small fluorite device with good sealing performance and capable of simulating the internal environment of a rotary kiln is an urgent problem to be solved by those skilled in the art. Disclosure of Invention In view of the above, the present invention provides a hydrofluoric acid preparation device, which can simulate the internal environment of a rotary kiln to prepare hydrofluoric acid from small fluorite for experimental study. In order to achieve the aim, the technical scheme of the invention provides a hydrofluoric acid preparation device which comprises an oil bath heating device, a reaction tank, a fixing frame, a reverse suction prevention tank and an absorption tank, wherein the reaction tank, the reverse suction prevention tank and the absorption tank are fixed on the fixing frame, the reaction tank is partially immersed in the oil bath heating device, a first connecting pipe is arranged between an air outlet pipe of the reaction tank and an air inlet end of the reverse suction prevention tank, one end of the first connecting pipe extending into the reverse suction prevention tank is positioned at the upper part of the reverse suction prevention tank, a second connecting pipe is arranged between the absorption tank and the reverse suction prevention tank, one end of the second connecting pipe extends into the lower part of the reverse suction prevention tank, and the other end of the second connecting pipe is positioned below the liquid level of the absorption tank. Further, the oil bath heating device comprises an oil bath pot and a heating furnace, wherein the oil bath pot is placed on the heating furnace, silicone oil is filled in the oil bath pot, and the reaction tank is partially immersed in the silicone oil. Further, a first sealing plug is arranged at the top of the reaction tank, an air outlet pipe of the reaction tank is arranged on the first sealing plug, and the air outlet end is connected with one end of the first connecting pipe through a hexagonal threaded pipe. Further, a magnetic stirrer is arranged in the reaction tank. Further, the fixing frame comprises a frame body and a plurality of clamping jaws, wherein the clamping jaws are fixed on the frame body and used for fixing the re