CN113856233A

CN113856233A - Efficient chlorine trifluoride rectifier unit

Info

Publication number: CN113856233A
Application number: CN202111230845.6A
Authority: CN
Inventors: 林坤; 马朝选; 徐海云; 张乾程
Original assignee: Peric Special Gases Co Ltd
Current assignee: Peric Special Gases Co Ltd
Priority date: 2021-10-22
Filing date: 2021-10-22
Publication date: 2021-12-31
Anticipated expiration: 2041-10-22
Also published as: CN113856233B

Abstract

The invention provides a high-efficiency chlorine trifluoride rectifying device which comprises a rectifying tower, and a fluorine gas conveying pipe, a chlorine gas conveying pipe, a diluent gas conveying pipe and a catalyst conveying pipe which are connected with the rectifying tower, wherein the chlorine gas conveying pipe, the fluorine gas conveying pipe and the diluent gas conveying pipe are respectively connected with chlorine gas, fluorine gas and diluent gas sources, the catalyst conveying pipe is connected with a medicine storage box, a conveying mechanism is arranged on the catalyst conveying pipe, and an annular spraying pipe communicated with the conveying mechanism is arranged at the top of the rectifying tower. The invention not only can realize the full mixing of chlorine trifluoride gas raw material during rectification, but also can ensure the mixing and fusing effect and quality, greatly shorten the fusing time, improve the quality of chlorine trifluoride, simultaneously improve the production efficiency of chlorine trifluoride, and has strong practicability, good use effect and obvious production and economic benefits.

Description

Efficient chlorine trifluoride rectifier unit

Technical Field

The invention belongs to the technical field of chemical industry, and particularly relates to a high-efficiency chlorine trifluoride rectifying device.

Background

Chlorine trifluoride is the most active halogen fluoride known in chemistry, and is a very powerful fluorinating agent. Chlorine trifluoride has a boiling point of 11.5 ℃ and is a gas which is easily condensed in a normal case, and the reaction can be carried out in any state of gas or liquid as required, which is not reached by a common fluorinating agent. Many metal oxides and chlorides react with chlorine trifluoride to form corresponding chlorides when heated, and by utilizing the characteristic of chlorine trifluoride, many important metal fluorides can be prepared, especially for separating and purifying rare elements. With the rapid development of semiconductor, liquid crystal, solar and LED industries, chlorine trifluoride is widely applied in the cleaning process of the CVD chamber, and the demand is increasing continuously, and chlorine trifluoride becomes one of the key special gases in the IC industry.

At present, chlorine trifluoride is rectified firstly in the preparation process of chlorine trifluoride, wherein chlorine, fluorine, diluent gas and a catalyst are usually mixed in a rectifying tower for rectifying catalysis in a first stage, but at present, the gases and the catalyst are usually required to be slowly fused, the time consumption is long, the efficiency is low, and the efficiency of chlorine trifluoride production is reduced when being mixed, therefore, a specific and remarkable chlorine trifluoride rectifying device needs to be designed to solve the problems.

Disclosure of Invention

The invention aims to solve the technical problem of providing an efficient chlorine trifluoride rectification device aiming at the defects of the prior art, the device can realize the full mixing of chlorine trifluoride gas raw materials during rectification, can ensure the mixing and fusing effects and quality, can greatly shorten the fusing time, improves the quality of chlorine trifluoride, simultaneously improves the production efficiency of chlorine trifluoride, and has strong practicability, good use effect and obvious production and economic benefits.

In order to solve the technical problems, the invention adopts the technical scheme that: the utility model provides an efficient chlorine trifluoride rectifier unit, its characterized in that includes the rectifying column and connects fluorine conveyer pipe, chlorine conveyer pipe, dilution gas conveyer pipe and the catalyst conveyer pipe on the rectifying column, fluorine conveyer pipe totally two and symmetrical connection are in the upper and lower both sides position of rectifying column lateral wall, fluorine conveyer pipe connection has the gas storage pipe, and the gas storage pipe passes through delivery line and connects the fluorine gas source, chlorine conveyer pipe totally two and symmetrical connection are in the upper and lower both sides of rectifying column lateral wall, chlorine conveyer pipe and fluorine conveyer pipe symmetry set up, chlorine conveyer pipe connection chlorine gas source, dilution gas conveyer pipe connection is in the intermediate position of rectifying column lateral wall, dilution gas conveyer pipe connection dilution gas source, the top of rectifying column is provided with heating device, the catalyst conveyer pipe passes through the delivery pump and connects the medicine storage box, and the catalyst conveying pipe is provided with a conveying mechanism, the top and the middle of the inner wall of the rectifying tower are respectively provided with two annular spraying pipes, and the two annular spraying pipes are connected with the conveying mechanism.

Preferably, the conveying mechanism comprises a conveying cylinder and a power box, the bottom of the conveying cylinder is fixedly connected with the power box, the conveying cylinder is communicated with the power box through an opening, a piston block is arranged in the conveying cylinder, a moving block is fixedly connected to the piston block through a pull rod, a power assembly is arranged in the power box, the power assembly is connected with the moving block, the piston block is pulled by the moving block to do linear reciprocating motion, the top of the conveying cylinder is communicated with the catalyst conveying pipe, the top of the conveying cylinder is connected with an installation pipe, the installation pipe is simultaneously connected with the annular spraying pipe through a connector, and the catalyst conveyed by the catalyst conveying pipe is sucked into the conveying cylinder and sprayed out of the annular spraying pipe through the reciprocating motion of the piston block.

Preferably, the power assembly comprises a driving motor, a gear and a connecting rod, the driving motor is fixedly installed on a power box, two rotating shafts are installed in the power box in a rotating mode, the gear is fixedly installed on each of the two rotating shafts and is in meshed transmission connection with the gear, an output shaft of the driving motor penetrates through the side wall of the power box and is fixedly connected with one of the rotating shafts, the gear wheel disc of the gear is eccentrically connected with one end of the connecting rod, the bottom end of the connecting rod is installed on one side of the gear wheel disc of the gear through a pin shaft, the top end of the connecting rod penetrates through an opening and is connected onto the bottom surface of the moving block through the pin shaft, connecting seats for installing the pin shaft are arranged on the bottom surface of the moving block and the gear wheel disc of the gear, when the driving motor runs, the two gears rotate oppositely, the connecting rod is pulled to do reciprocating motion of the cam connecting rod, and finally the moving block is pulled to do linear reciprocating motion along the axial direction of the conveying cylinder through pulling the piston block, when the piston block moves downwards, the catalyst in the catalyst conveying pipe is sucked into the conveying cylinder, and when the piston block moves upwards, the catalyst in the conveying cylinder is extruded to the annular spraying pipe and is sprayed into the rectifying tower, so that the catalyst is fully contacted with each gas, and the rectifying reaction efficiency is greatly improved.

Preferably, evenly be provided with a plurality of atomizer on the annular spraying pipe, the inboard equidistance of annular spraying pipe is connected with four connecting pipes, be connected with two fixed pipes simultaneously on the connecting head, four the connecting pipe passes through five-way joint connection fixed pipe.

Preferably, install the second check valve on the catalyst conveyer pipe, install first check valve on the installation pipe, the lower extreme of rectifying column is fixed with the base, the lower extreme of base is fixed with the bottom plate, equidistant flowmeter, thermometer, valve and pressure gauge of installing on the chlorine conveyer pipe, be connected with the diffusion pipe on the chlorine conveyer pipe.

Preferably, the peripheral side of the moving block is provided with a sealing disc adapted to the conveying cylinder.

Preferably, the two chlorine conveying pipes are fixedly installed through a fixing frame, the medicine storage box and the conveying barrel are both fixed on the fixing frame, and a sealing cover is arranged on the medicine storage box.

Preferably, fluorine conveyer pipe and chlorine conveyer pipe all connect on the rectifying column through the connecting cover, and the same level bilateral symmetry of rectifying column sets up two connecting covers and is used for connecting chlorine conveyer pipe and fluorine conveyer pipe of same height, and the connecting cover is hopper-shaped and sets up the diffusion velocity that can effectively accelerate input gas and increase the volume of diffusing inside the rectifying column, fluorine conveyer pipe the lower extreme of gas storage pipe is provided with the mounting bracket.

Preferably, the bottom of the rectifying tower is connected with two discharging pipes, and the two discharging pipes are connected with an output pipe together.

Compared with the prior art, the invention has the following advantages:

1. the invention has scientific and reasonable structural design, safety, reliability and simple operation, can realize the full mixing of raw material gases during rectification, ensures the effect and quality of mixing and fusion, greatly shortens the fusion time, improves the quality of chlorine trifluoride, and simultaneously improves the production efficiency of chlorine trifluoride.

2. According to the invention, chlorine and fluorine gas are conveyed through the two pipelines with different heights, the inlet of the diluent gas is arranged in the middle of the rectifying tower, the inlets of the fluorine gas and the chlorine gas are arranged at the upper side and the lower side of the inlet of the diluent gas, the gas diffusion speed is high, the mixing effect is good, the fusion time is greatly shortened, the catalyst is conveyed into the rectifying tower through the piston blocks in the conveying device and is sprayed out in a mist shape from the top and the middle of the rectifying tower, the contact area between the catalyst and the raw material gas is ensured, the fusion quality and speed are remarkably improved, and the aim of improving the production efficiency of chlorine trifluoride is finally achieved.

The present invention will be described in further detail with reference to the accompanying drawings and examples.

Drawings

Fig. 1 is a schematic structural view of the present invention.

FIG. 2 is a schematic view of the rectifying column of the present invention.

Fig. 3 is a schematic structural view of the conveying mechanism of the present invention.

FIG. 4 is a schematic diagram of the layout structure of the connecting cover in the rectifying tower of the present invention.

FIG. 5 is a schematic view of the construction of the annular shower of the present invention.

Description of reference numerals:

1-a flow meter; 2-a thermometer; 3-chlorine conveying pipe;

4, a diffusing pipe; 5, fixing a frame; 6, a valve;

7-a pressure gauge; 8-a heating device; 9-a rectifying tower;

10-fixing the tube; 11-a connector; 12-fluorine gas delivery pipe;

13-dilution gas delivery pipe; 14-a mounting frame; 15-transfer line;

16-a gas storage pipe; 17-sealing the cover; 18-a catalyst transfer pipe;

19-a discharge pipe; 20-a base; 21, an output pipe;

22-a transfer pump; 23-a medicine storage box; 24-annular shower pipe;

25-connecting cover; 26-an atomizing spray head; 27-a base plate;

28-connecting pipe; 29-installing a pipe; 30-a first one-way valve;

31-a piston block; 32-a second one-way valve; 33-opening;

34-a gear; 35-a power box; 36-a pull rod;

37-a moving block; 38-sealing disc; 39-connecting rod;

and 40, conveying the cylinder.

Detailed Description

As shown in fig. 1 to 5, the present invention includes a rectifying tower 9, fluorine conveying pipes 12, chlorine conveying pipes 3, a diluent gas conveying pipe 13 and a catalyst conveying pipe 18 connected to the rectifying tower 9, wherein two fluorine conveying pipes 12 are symmetrically connected to the upper and lower sides of the outer side wall of the rectifying tower 9, the fluorine conveying pipes 12 are connected to a gas storage pipe 16, the gas storage pipe 16 is connected to a fluorine gas source through a conveying pipeline 15, two chlorine conveying pipes 3 are symmetrically connected to the upper and lower sides of the outer side wall of the rectifying tower 9, the chlorine conveying pipes 3 and the fluorine conveying pipes 12 are symmetrically arranged, the chlorine conveying pipes 3 are connected to a chlorine gas source, the diluent gas conveying pipe 13 is connected to the middle position of the outer side wall of the rectifying tower 9, the diluent gas conveying pipe 13 is connected to a diluent gas source, a heating device 8 is arranged at the top of the rectifying tower 9, the heating device 8 heats the interior of the rectifying tower 9 to 400-, the catalyst conveying pipe 18 is connected with a medicine storage box 23 through a conveying pump 22, a conveying mechanism is arranged on the catalyst conveying pipe 18, two annular spraying pipes 24 are respectively arranged at the top and the middle of the inner wall of the rectifying tower 9, and the two annular spraying pipes 24 are connected with the conveying mechanism.

In this embodiment, the conveying mechanism includes a conveying cylinder 40 and a power box 35, the bottom of the conveying cylinder 40 is fixedly connected to the power box 35, the conveying cylinder 40 is communicated with the power box 35 through an opening 33, a piston block 31 is arranged in the conveying cylinder 40, a moving block 37 is fixedly connected to the piston block 31 through a pull rod 36, a power assembly is arranged in the power box 35, the power assembly is connected to the moving block 37, the piston block 31 is pulled by the moving block 37 to perform linear reciprocating motion, the top of the conveying cylinder 40 is communicated with the catalyst conveying pipe 18, the top of the conveying cylinder 40 is connected with an installation pipe 29, the installation pipe 29 is simultaneously connected with the annular shower pipe 24 through a connecting head 11, and the catalyst conveyed by the catalyst conveying pipe 18 is sucked into the conveying cylinder 40 through the reciprocating motion of the piston block 31 and is sprayed out of the annular shower pipe 24.

In this embodiment, the power assembly includes a driving motor, a gear 34 and a connecting rod 39, the driving motor is fixedly installed on a power box 35, two rotating shafts are rotatably installed in the power box 35, the gear 34 is fixedly installed on both the two rotating shafts, the two gears 34 are in meshing transmission connection, an output shaft of the driving motor passes through the side wall of the power box 35 and is fixedly connected with one of the rotating shafts, a gear plate of the gear 34 is eccentrically connected with one end of the connecting rod 39, the bottom end of the connecting rod 39 is installed on one side of the gear plate of the gear 34 through a pin shaft, the top end of the connecting rod 39 passes through an opening 33 and is connected on the bottom surface of a moving block 37 through a pin shaft, connecting seats for installing pin shafts are arranged on the bottom surface of the moving block 37 and the gear plate of the gear 34, when the driving motor operates, the two gears 34 rotate in opposite directions, and simultaneously the connecting rod 39 is pulled to perform reciprocating motion of a cam connecting rod, finally, the piston block 31 is pulled by the moving block 37 to do linear reciprocating motion along the axial direction of the conveying cylinder 40, when the piston block 31 moves downwards, the catalyst in the catalyst conveying pipe 18 is sucked into the conveying cylinder 40, when the piston block 31 moves upwards, the catalyst in the conveying cylinder 40 is extruded to the annular spray pipe 24 and is sprayed into the rectifying tower 9, so that the catalyst is fully contacted with each gas, and the rectifying reaction efficiency is greatly improved.

In this embodiment, evenly be provided with a plurality of atomizer 26 on annular spraying pipe 24, annular spraying pipe 24's inboard equidistance is connected with four connecting pipes 28, be connected with two fixed pipes 10 on the connector 11 simultaneously, four connecting pipe 28 passes through five-way joint connection fixed pipe 10.

In this embodiment, install second check valve 32 on the catalyst conveyer pipe 18, install first check valve 30 on the installation pipe 29, the lower extreme of rectifying column 9 is fixed with base 20, the lower extreme of base 20 is fixed with bottom plate 27, equidistant flowmeter 1, thermometer 2, valve 6 and pressure gauge 7 of installing on the chlorine conveyer pipe 3, be connected with on the chlorine conveyer pipe 3 and diffuse pipe 4.

In this embodiment, a seal disk 38 adapted to the transfer cylinder 40 is provided on the peripheral side of the moving block 37.

In this embodiment, the two chlorine gas delivery pipes 3 are fixedly mounted by a fixing frame 5, the medicine box 23 and the delivery tube 40 are both fixed to the fixing frame 5, and the medicine box 23 is provided with a seal cover 17.

In this embodiment, the fluorine gas delivery pipe 12 and the chlorine gas delivery pipe 3 are both connected to the rectifying tower 9 through the connecting covers 25, two connecting covers 25 are symmetrically arranged on both sides of the rectifying tower 9 at the same horizontal height for connecting the chlorine gas delivery pipe 3 and the fluorine gas delivery pipe 12 at the same height, the connecting covers 25 are arranged in a funnel shape in the rectifying tower 9, so that the diffusion speed of the input gas can be effectively increased, the diffusion volume can be increased, sufficient mixing of the opposite gases during ejection can be ensured, the ejection time of the fluorine gas, the chlorine gas and the diluent gas is determined by the amount of the reactant, and the reactant is matched with the catalyst in proportion to perform the rectifying reaction. The fluorine gas delivery pipe 12 is provided with a mounting frame 14 at the lower end of the gas storage pipe 16.

In this embodiment, the bottom of the rectifying tower 9 is connected with two discharging pipes 19, and the two discharging pipes 19 are connected with an output pipe 21 together, so as to discharge the rectified material into the corresponding pipeline.

When the catalyst delivery device is used, chlorine and fluorine gas are respectively delivered into a rectifying tower 9 through a chlorine delivery pipe 3 and a fluorine delivery pipe 12 and are oppositely sprayed out through a connecting cover 25, so that rapid fusion is realized, meanwhile, diluent gas is delivered into the middle position in the rectifying tower 9 through a diluent gas delivery pipe 13, a delivery pump 22 and a driving motor are simultaneously started, the catalyst in a storage box 23 is delivered into a catalyst delivery pipe 18 by the delivery pump 22, a second one-way valve 32 is opened when the catalyst is delivered, the driving motor drives two gears 34 to rotate, then two connecting rods 39 are driven to move on one side of the gears 34, the connecting rods 39 drive a moving block 37 to move up and down along with the rotation of the gears 34, so as to drive a piston block 31 to move downwards, the catalyst delivery pipe 18 delivers the catalyst into a delivery cylinder 40, and when the gears 34 rotate for one circle, the piston block 31 extrudes the catalyst in the delivery box 40 into a mounting pipe 29, meanwhile, the first check valve 30 is opened, the second check valve 32 is closed, the catalyst is sent into the annular spraying pipe 24 through the fixing pipe 10 and then sprayed out through the spraying nozzle 26, indirect spraying of the catalyst is realized due to the up-and-down movement of the piston block 31, the atomized fusion effect of the catalyst is fully improved, the reactant is obtained after full rectification reaction, and then the reactant is discharged to be cooled, liquefied, discharged and gasified to obtain chlorine trifluoride.

The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims

1. The utility model provides an efficient chlorine trifluoride rectification device, its characterized in that, including rectifying column (9) and fluorine conveyer pipe (12), chlorine conveyer pipe (3), diluent gas conveyer pipe (13) and catalyst conveyer pipe (18) of connecting on rectifying column (9), fluorine conveyer pipe (12) totally two and the upper and lower both sides of symmetric connection at rectifying column (9) lateral wall, fluorine conveyer pipe (12) are connected with gas storage tube (16), and gas storage tube (16) connect the fluorine gas source through pipeline (15), chlorine conveyer pipe (3) totally two and the upper and lower both sides of symmetric connection at rectifying column (9) lateral wall, chlorine conveyer pipe (3) and fluorine conveyer pipe (12) symmetry set up, chlorine conveyer pipe (3) connect the gas source, the intermediate position at rectifying column (9) lateral wall is connected in diluent gas conveyer pipe (13), the utility model discloses a rectification tower, including dilution gas conveyer pipe (13), rectifying column (9), catalyst conveyer pipe (18), delivery pump (22), delivery box (23), two annular shower (24) are set up respectively at the inner wall top and the middle part of rectifying column (9), two annular shower (24) all with conveying mechanism connects.

2. A highly efficient rectification apparatus of chlorine trifluoride according to claim 1, the conveying mechanism comprises a conveying cylinder (40) and a power box (35), the bottom of the conveying cylinder (40) is fixedly connected with the power box (35), the conveying cylinder (40) is communicated with the power box (35) through an opening (33), a piston block (31) is arranged in the conveying cylinder (40), the piston block (31) is fixedly connected with a moving block (37) through a pull rod (36), a power assembly is arranged in the power box (35), the power assembly is connected with a moving block (37) and pulls the piston block (31) to do linear reciprocating motion through the moving block (37), the top of the conveying cylinder (40) is communicated with the catalyst conveying pipe (18), the top of the conveying cylinder (40) is connected with a mounting pipe (29), the mounting pipe (29) is connected with the annular spraying pipe (24) through the connecting head (11) at the same time.

3. A high efficiency rectification apparatus of chlorine trifluoride as claimed in claim 2, wherein said power assembly comprises a driving motor, a gear (34) and a connecting rod (39), said driving motor is fixedly mounted on a power box (35), two gears (34) engaged with each other are rotatably mounted in said power box (35), an output shaft of said driving motor is fixedly connected with one of said gears (34), a gear plate of said gear (34) is eccentrically connected with one end of said connecting rod (39), and the other end of said connecting rod (39) passes through said opening (33) and is connected with a moving block (37).

4. The high-efficiency chlorine trifluoride rectification device according to claim 2, wherein a plurality of atomizing nozzles (26) are uniformly arranged on the annular spraying pipe (24), four connecting pipes (28) are equidistantly connected to the inner side of the annular spraying pipe (24), two fixed pipes (10) are simultaneously connected to the connecting head (11), and the four connecting pipes (28) are connected to the fixed pipes (10) through a five-way joint.

5. The high-efficiency chlorine trifluoride rectification device according to claim 2, wherein a second check valve (32) is installed on the catalyst conveying pipe (18), a first check valve (30) is installed on the installation pipe (29), a base (20) is fixed at the lower end of the rectification tower (9), a bottom plate (27) is fixed at the lower end of the base (20), a flowmeter (1), a thermometer (2), a valve (6) and a pressure gauge (7) are installed on the chlorine conveying pipe (3) at equal intervals, and a diffusion pipe (4) is connected to the chlorine conveying pipe (3).

6. A highly efficient rectification apparatus for chlorine trifluoride according to claim 2 wherein said moving block (37) is provided with a sealing plate (38) fitted to said transfer cylinder (40) on the periphery thereof.

7. The high-efficiency chlorine trifluoride rectification device according to claim 2, wherein the two chlorine conveying pipes (3) are fixedly mounted by a fixing frame (5), the medicine storage box (23) and the conveying cylinder (40) are fixed on the fixing frame (5), and the medicine storage box (23) is provided with a sealing cover (17).

8. A highly efficient rectification apparatus for chlorine trifluoride as claimed in claim 1, wherein said fluorine gas supply tube (12) and said chlorine gas supply tube (3) are connected to the rectification column (9) by means of a connecting cover (25), and said gas receiver tube (16) is provided at its lower end with a mounting frame (14).

9. A highly efficient rectification apparatus for chlorine trifluoride according to claim 1, characterized in that two discharge pipes (19) are connected to the bottom of the rectification column (9), and the two discharge pipes (19) are connected together with an output pipe (21).