CN112047302A - Preparation device and preparation process for electronic-grade hydrofluoric acid - Google Patents

Preparation device and preparation process for electronic-grade hydrofluoric acid Download PDF

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Publication number
CN112047302A
CN112047302A CN202010861870.3A CN202010861870A CN112047302A CN 112047302 A CN112047302 A CN 112047302A CN 202010861870 A CN202010861870 A CN 202010861870A CN 112047302 A CN112047302 A CN 112047302A
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Prior art keywords
driving
feeding
feed
condenser
communicated
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CN202010861870.3A
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CN112047302B (en
Inventor
吴全贵
郑义达
吴俊贤
赖延恩
艾合买提艾尔肯
陈国民
李文斌
骆彦成
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Fujian Tianfu Electronic Materials Co ltd
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Fujian Tianfu Electronic Materials Co ltd
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Priority to CN202010861870.3A priority Critical patent/CN112047302B/en
Publication of CN112047302A publication Critical patent/CN112047302A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00Halogens; Halogen acids
    • C01B7/19Fluorine; Hydrogen fluoride
    • C01B7/191Hydrogen fluoride
    • C01B7/195Separation; Purification
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/70Pre-treatment of the materials to be mixed
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/70Pre-treatment of the materials to be mixed
    • B01F23/708Filtering materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/71Feed mechanisms
    • B01F35/712Feed mechanisms for feeding fluids

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Transmission Devices (AREA)

Abstract

A production apparatus for electronic grade hydrofluoric acid comprising: a feed tank for storing anhydrous hydrogen fluoride; a tower kettle for obtaining anhydrous hydrogen fluoride gas; a condenser for liquefying anhydrous hydrogen fluoride gas; a blending tank for blending anhydrous hydrogen fluoride liquid; and a finished product tank for storing hydrofluoric acid; the outlet of the feeding groove is communicated with the inlet of the tower kettle, the outlet of the tower kettle is communicated with the inlet of the condenser, the outlet of the condenser is communicated with the inlet of the blending groove, and the outlet of the blending groove is communicated with the inlet of the finished product groove. The structure is simple, the simplification of the complex process is realized, the simplification of the production flow is facilitated, the production cost is reduced, and the positive significance on improving the production efficiency is achieved. The preparation process is realized based on the preparation device, the operation is simple, the implementation is easy, the whole production process is simplified, and the production efficiency is improved.

Description

Preparation device and preparation process for electronic-grade hydrofluoric acid
Technical Field
The invention relates to the field of hydrofluoric acid preparation, in particular to a preparation device and a preparation process for electronic-grade hydrofluoric acid.
Background
At present, the existing equipment for preparing electronic-grade hydrofluoric acid is complex in structure, complex in whole manufacturing process, high in difficulty of matching control among all parts, relatively complex in use and low in production efficiency.
In view of this, the present application is specifically made.
Disclosure of Invention
The first purpose of the invention is to provide a preparation device for electronic grade hydrofluoric acid, which has a simple structure, realizes simplification of the complex process, is beneficial to simplifying the production flow, reduces the production cost and has positive significance for improving the production efficiency.
The second purpose of the invention is to provide a preparation process for electronic-grade hydrofluoric acid, which is simple to operate and easy to implement, so that the whole production process is simplified, and the production efficiency is improved.
The embodiment of the invention is realized by the following steps:
a production apparatus for electronic grade hydrofluoric acid comprising: a feed tank for storing anhydrous hydrogen fluoride; a tower kettle for obtaining anhydrous hydrogen fluoride gas; a condenser for liquefying anhydrous hydrogen fluoride gas; a blending tank for blending anhydrous hydrogen fluoride liquid; and a finished product tank for storing hydrofluoric acid; the outlet of the feeding groove is communicated with the inlet of the tower kettle, the outlet of the tower kettle is communicated with the inlet of the condenser, the outlet of the condenser is communicated with the inlet of the blending groove, and the outlet of the blending groove is communicated with the inlet of the finished product groove.
Further, the manufacturing apparatus includes: a one-way feeding mechanism; the one-way feeding mechanism comprises a driving assembly, a feeding channel and a feeding piston, the feeding piston is arranged at the feeding channel, the driving assembly is arranged at one end of the feeding channel and used for driving the feeding piston to reciprocate, a discharging port is formed in one end, away from the driving assembly, of the feeding channel, the discharging port is communicated with an inlet of the condenser, and a feeding port communicated with an outlet of the tower kettle is formed in the side wall of the feeding channel;
the feeding hole and the discharging hole are intermittently communicated through the reciprocating motion of the feeding piston, so that the material in the feeding channel quickly enters the condenser.
Further, the drive assembly includes: the device comprises a device box, a driving rod, a driving arm and a first arc-shaped tooth block, wherein the device box is arranged at one end of the feeding channel, which is far away from the condenser, and the driving rod can movably penetrate through the side wall of the device box and then is connected with a feeding piston; the driving rod is movably connected with the equipment box along the axial direction of the driving rod, the driving rod is provided with a first tooth part along the axial direction of the driving rod, the driving arm can be rotatably arranged on the equipment box, the first arc-shaped tooth block is arranged at one end, close to the driving rod, of the driving arm, and the first arc-shaped tooth block and the first tooth part are meshed with each other;
can rotate the axis through the actuating arm together and rotate as the axle, drive first arc tooth piece and rotate for first arc tooth piece meshes with first tooth portion, so that actuating lever along its axial reciprocating motion.
Further, the driving arm is connected with a rotating assembly for driving the driving arm to rotate, and the rotating assembly comprises: the rotating shaft can movably penetrate through the equipment box; the rotating shaft is movably connected with the equipment box along the circumferential direction of the rotating shaft; one end of the rotating shaft is connected with an output shaft of the rotating motor, the other end of the rotating shaft is positioned in the equipment box, a driving block is arranged at the end part of the rotating shaft, one end of the transmission arm is eccentrically and rotatably connected with the driving block, and the other end of the transmission arm is rotatably connected with the driving arm.
Furthermore, a second tooth part is arranged on one side, away from the first tooth part, of the driving rod, and the second tooth part is arranged along the axial direction of the driving rod; the inner wall of the equipment box is provided with a supporting arm, and a limit gear meshed with the second tooth part is rotatably arranged between the two supporting arms.
Furthermore, one end of the driving arm, which is far away from the first arc-shaped tooth block, is connected with a second arc-shaped tooth block, a movable rack which is meshed with the second arc-shaped tooth block is movably arranged on the inner wall of the equipment box, the movable rack is arranged in parallel with the driving rod, and the movable rack is movably connected with the inner wall of the equipment box along the axial direction of the movable rack; the movable rack is connected with a driving component for driving the movable rack to move;
can change its position with second arc tooth piece meshing department through the motion of activity rack to when making the actuating arm use second arc tooth piece meshing department as the axle rotation, the rotation range of actuating arm is different, so that the home range of messenger's actuating lever changes.
Further, the feeding channel comprises a feeding section, a closed section, a negative pressure section and a compression section which are sequentially communicated;
when the feeding piston moves to the feeding section, the feeding hole is communicated with the inlet of the condenser so as to enable the material to enter the feeding channel;
when the feeding piston moves to the closing section, feeding seals the feeding hole;
when the feeding piston moves to the negative pressure section, the feeding hole is sealed, and meanwhile, the material in the feeding piston is pushed to move towards one side of the discharging hole;
when the feeding piston moves to the compression section, the material is discharged through the discharge port.
Furthermore, a discharge port of the feeding channel is connected with a pressure valve, an inlet of the pressure valve is communicated with the discharge port, and an outlet of the pressure valve is communicated with an inlet of the condenser; the anhydrous hydrogen fluoride gas in the feed channel can be compressed by the movement of the feed piston to open the pressure valve.
The preparation process for preparing the electronic-grade hydrofluoric acid by using the preparation device comprises the steps of putting anhydrous hydrogen fluoride into a feeding groove according to a preset proportion, heating the feeding groove by using a tower kettle to generate anhydrous hydrogen fluoride gas, enabling the anhydrous hydrogen fluoride gas to quickly enter a condenser by using a one-way feeding mechanism, liquefying the anhydrous hydrogen fluoride gas by using the condenser, then diluting the anhydrous hydrogen fluoride gas in a blending groove, then entering a finished product groove, and subpackaging and warehousing.
The embodiment of the invention has the beneficial effects that:
according to the preparation device for the electronic grade hydrofluoric acid, provided by the embodiment of the invention, during production, the anhydrous hydrogen fluoride in the feeding groove can enter the tower kettle, hot water is introduced into the tower kettle, a low-temperature evaporation mode is adopted, anions and cations are removed by utilizing different boiling points to obtain high-purity anhydrous hydrogen fluoride gas, then the anhydrous hydrogen fluoride gas is introduced into the condenser to liquefy the anhydrous hydrogen fluoride gas, then the anhydrous hydrogen fluoride gas enters the blending groove, a certain amount of ultrapure water is introduced into the blending groove, and the blended anhydrous hydrogen fluoride gas is conveyed to the finished product groove to be subpackaged and warehoused.
In general, the preparation device for electronic grade hydrofluoric acid provided by the embodiment of the invention has a simple structure, realizes simplification of the complex process, is beneficial to simplifying the production flow, reduces the production cost, and has positive significance for improving the production efficiency. The preparation process for the electronic grade hydrofluoric acid provided by the embodiment of the invention is simple to operate and easy to implement, so that the whole production process is simplified, and the production efficiency is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic structural diagram of a manufacturing apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a condenser according to an embodiment of the present invention;
FIG. 3 is a schematic mechanical diagram of a unidirectional feeding mechanism provided in an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a driving mechanism according to an embodiment of the present invention;
FIG. 5 is a schematic structural diagram of a feed channel provided in an embodiment of the present invention;
fig. 6 is a schematic flow chart of a manufacturing process according to an embodiment of the present invention.
Icon: 1-feeding groove, 2-tower kettle, 3-condenser, 4-blending groove, 5-finished product groove, 6-unidirectional feeding mechanism, 61-driving component, 611-equipment box, 612-driving rod, 613-driving arm, 614-first arc-shaped tooth block, 615-first tooth part, 62-feeding channel, 621-feeding section, 622-closing section, 623-negative pressure section, 624-compression section, 63-feeding piston, 64-feeding hole, 65-discharging hole, 7-rotating motor, 8-rotating shaft, 9-driving arm, 10-driving block, 11-second tooth part, 12-supporting arm, 13-limiting gear, 14-second arc-shaped tooth block, 15-movable rack, 16-driving component, 17-pressure valve, 18-buffer tank, 19-buffer tower, 20-metering tank, 21-primary filter and 22-purification tower.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "parallel," "perpendicular," and the like do not require that the components be absolutely parallel or perpendicular, but may be slightly inclined. For example, "parallel" merely means that the directions are more parallel relative to "perpendicular," and does not mean that the structures are necessarily perfectly parallel, but may be slightly tilted.
Furthermore, the terms "horizontal", "vertical", "overhang" and the like do not imply that the components are required to be absolutely horizontal or overhang, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Examples
Referring to fig. 1-6, the present embodiment provides an apparatus for preparing electronic grade hydrofluoric acid, comprising: a feed tank 1 for storing anhydrous hydrogen fluoride; a tower kettle 2 for obtaining anhydrous hydrogen fluoride gas; a condenser 2 for liquefying anhydrous hydrogen fluoride gas; a blending tank 4 for blending anhydrous hydrogen fluoride liquid; and a finished product tank 5 for storing hydrofluoric acid.
Wherein, the outlet of the feeding groove 1 is communicated with the inlet of the tower kettle 2, the outlet of the tower kettle 2 is communicated with the inlet of the condenser 2, the outlet of the condenser 2 is communicated with the inlet of the blending groove 4, and the outlet of the blending groove 4 is communicated with the inlet of the finished product groove 5.
During production, the anhydrous hydrogen fluoride in the feeding groove 1 can enter the tower kettle 2, hot water (50-60 ℃) is introduced into the tower kettle 2, a low-temperature evaporation mode is adopted, anions and cations are removed by utilizing different boiling points, high-purity anhydrous hydrogen fluoride gas is obtained, then the anhydrous hydrogen fluoride gas is introduced into the condenser 2, the anhydrous hydrogen fluoride gas is liquefied, then the anhydrous hydrogen fluoride gas enters the blending groove 4, a certain amount of ultrapure water is introduced into the blending groove 4, and the blended anhydrous hydrogen fluoride gas is conveyed into the finished product groove 5 and can be subpackaged and stored.
In general, the preparation device for electronic grade hydrofluoric acid provided by the embodiment of the invention has a simple structure, realizes simplification of the complex process, is beneficial to simplifying the production flow, reduces the production cost, and has positive significance for improving the production efficiency.
Further, referring to fig. 2 and fig. 3, in the present embodiment, in order to avoid the backflow of the anhydrous hydrogen fluoride gas entering the condenser 2 from the condenser 2, and to improve the efficiency of the anhydrous hydrogen fluoride gas entering the condenser 2, the preparation apparatus is particularly matched with the one-way feeding mechanism 6. Wherein the one-way feeding mechanism 6 comprises a driving assembly 61, a feeding channel 62 and a feeding piston 63.
The feeding piston 63 is arranged on the feeding channel 62, the driving assembly 61 is arranged at one end of the feeding channel and used for driving the feeding piston 63 to reciprocate, a discharging hole 65 is formed in one end, away from the driving assembly 61, of the feeding channel, the discharging hole 65 is communicated with an inlet of the condenser 2, and a feeding hole 64 communicated with an outlet of the tower kettle 2 is formed in the side wall of the feeding channel.
Can be through feed piston 63 reciprocating motion in feedstock channel 62 for anhydrous hydrogen fluoride gas passes through feed inlet 64 earlier and gets into feedstock channel 62 in, then moves through feed piston 63, makes anhydrous hydrogen fluoride gas get into condenser 2 fast under the state of compression, and anhydrous hydrogen fluoride gas is in by the compression state, after getting into condenser 2, liquefaction that can be quick improves liquefaction efficiency.
Through above-mentioned global design back, before anhydrous hydrogen fluoride gas gets into condenser 2, can get into feed channel 62 earlier, then utilize feed piston 63 motion, compress anhydrous hydrogen fluoride gas, can enough make anhydrous hydrogen fluoride gas get into condenser 2 fast, prevent the backward flow, can compress anhydrous hydrogen fluoride gas again, make it get into condenser 2 back fast liquefaction.
Further, the driving assembly 61 includes: the device comprises an equipment box 611, a driving rod 612, a driving arm 613 and a first arc-shaped tooth block 614, wherein the equipment box 611 is arranged at one end of the feeding channel 62 far away from the condenser 2, and the driving rod 612 can movably penetrate through the side wall of the equipment box 611 and then is connected with a feeding piston 63; the driving rod 612 is movably connected with the equipment box 611 along the axial direction of the driving rod 612, the driving rod 612 is provided with a first tooth portion 615 along the axial direction, the driving arm 613 is rotatably arranged on the equipment box 611, a first arc-shaped tooth block 614 is arranged at one end of the driving arm 613 close to the driving rod 612, and the first arc-shaped tooth block 614 is meshed with the first tooth portion 615;
the driving arm 613 can rotate together with the shaft 8 to rotate, and the first arc-shaped tooth block 614 is rotated, so that the first arc-shaped tooth block 614 engages with the first tooth portion 615 to reciprocate the driving rod 612 in the axial direction thereof.
The driving arm 613 is connected to a rotating assembly for driving the driving arm to rotate, and the rotating assembly includes: the rotating motor 7, the rotating shaft 8 and the transmission arm 9 are rotated, and the rotating shaft 8 can movably penetrate through the equipment box 611; the rotating shaft 8 is movably connected with the equipment box 611 along the circumferential direction of the rotating shaft 8; one end of the rotating shaft 8 is connected to an output shaft of the rotating motor 7, the other end is located in the equipment box 611, and an end portion thereof is provided with a driving block 10, one end of the transmission arm 9 is eccentric and rotatably connected to the driving block 10, and the other end is rotatably connected to the driving arm 613.
In this embodiment, the axis of the drive rod 612 coincides with the axis of the feed channel 62. And the outer wall of the feeding piston 63 is provided with a sealing rubber layer, so that the feeding piston 63 can normally move in the feeding channel 62 without gas leakage. In order to avoid the feed piston 63 from being damaged by friction, the inner wall of the feed passage 62 is smooth by surface treatment in the present embodiment.
In this embodiment, the arc corresponding to the first arc-shaped tooth block 614 is tangent to the axis of the first tooth portion 615, so as to ensure that when the driving arm 613 drives the first arc-shaped tooth block 614 to rotate, the driving arm 612 is driven to reciprocate in the axial direction by the engagement of the first arc-shaped tooth block 614 and the first tooth portion 615.
In this embodiment, driving motor is connected with the stopper, guarantees to drive tonna and after the outage, and its rotor is locked, can not take place to rotate.
In this embodiment, the driving arm 9 may be connected to the driving block 10 and the driving arm 613 in a rotatable manner by a shaft hinge.
In this embodiment, the driving arm 9 is eccentrically connected to the driving block 10, which means that the connection point of the driving arm 9 and the driving block 10 is far away from the center of the rotation shaft 8 of the driving block 10.
Can rotate through driving motor, drive axis of rotation 8 and rotate, thereby make drive block 10 synchronous rotation, because transmission arm 9 is connected with drive block 10 off-centre, thereby when making transmission arm 9 rotate along with drive block 10, can produce the displacement of vertical direction, through the displacement of the vertical direction of transmission arm 9, can drive actuating arm 613 and use its department of rotation as the reciprocal swing of axle, thereby be equivalent to reciprocating rotation with regard to first arc tooth piece 614, and then make actuating lever 612 at vertical direction reciprocating motion, thereby drive feed piston 63 reciprocating motion in feedstock channel 62.
Through the design, the driving rod 612 can be driven to reciprocate in the vertical direction more stably through the driving mechanism, and the driving motor always keeps continuous rotation in a single direction in the process, so that the stability of the driving motor is ensured, and the control difficulty of the driving motor is reduced.
Further, in order to ensure the stability of the driving rod 612 during the reciprocating motion in the vertical direction, in the present embodiment, a second tooth portion 11 is disposed on a side of the driving rod 612 away from the first tooth portion 615, and the second tooth portion 11 is disposed along the axial direction of the driving rod 612; the inner wall of the equipment box 611 is provided with a supporting arm 12, and a limit gear 13 engaged with the second tooth part 11 is rotatably arranged between the two supporting arms 12.
Furthermore, one end of the driving arm 613, which is far away from the first arc-shaped tooth block 614, is connected with a second arc-shaped tooth block 14, a movable rack 15 which is meshed with the second arc-shaped tooth block 14 is movably arranged on the inner wall of the equipment box 611, the movable rack 15 is arranged in parallel with the driving rod 612, and the movable rack 15 is movably connected with the inner wall of the equipment box 611 along the axial direction of the movable rack 15; the movable rack 15 is connected with a driving member 16 for driving the movable rack to move;
in this embodiment, the circle corresponding to the second arc-shaped tooth block 14 and the circle corresponding to the first arc-shaped tooth block 614 are located at the same center, and the radii of the corresponding circles are the same.
In this embodiment, the connection between the driving arm 9 and the driving arm 613 is located between the first arc-shaped tooth block 614 and the second arc-shaped tooth block 14.
The second arc-shaped tooth block 14 can rotate by a certain angle through the movement of the movable rack 15, so that the driving arm 613 rotates by a certain angle, thereby changing the position of the engagement between the movable rack 15 and the second arc-shaped tooth block 14, and when the driving arm 613 rotates by taking the engagement between the second arc-shaped tooth block 14 as an axis, the rotating range of the driving arm 613 is different, so that the moving range of the driving rod 612 is changed.
Through the above design, the position of the center of the rotating shaft 8 when the driving arm 613 rotates can be changed, so that the reciprocating swing range of the first arc-shaped tooth block 614 is changed, the moving range of the driving rod 612 in the vertical direction is changed, and the material amount in the feeding channel 62 can be changed through the mode, so that the conveying efficiency is changed.
In this embodiment, the inner wall of the equipment box 611 is provided with a chute (not shown) for moving the movable rack 15; the concrete chute can adopt a 'T' -shaped chute, and both sides of the movable rack 15 are provided with extending parts (not shown) matched with the chute, so as to ensure that the movable rack 15 can stably move.
In this embodiment, the driving member 16 for driving the movable rack 15 to move may adopt an air cylinder, an oil cylinder or other conventional technologies, in this embodiment, an air cylinder is adopted, a fixed end of the air cylinder is disposed on an outer wall of the equipment box 611, and an output end of the air cylinder movably penetrates through a side wall of the equipment box 611 and then is connected with the movable rack 15; the cylinder is movably connected with the side wall of the equipment box 611 along the axial direction of the cylinder; and the central axis of the cylinder coincides with the central axis of the movable rack 15.
Further, the feeding channel 62 comprises a feeding section 621, a closed section 622, a negative pressure section 623 and a compression section 624 which are communicated in sequence;
the discharge hole 65 of the feeding channel 62 is connected with a pressure valve 17, the inlet of the pressure valve 17 is communicated with the discharge hole 65, and the outlet of the pressure valve 17 is communicated with the inlet of the condenser 2; the anhydrous hydrogen fluoride gas in the feed passage 62 can be compressed by the movement of the feed piston 63 to open the pressure valve 17.
When the feed piston 63 moves to the feed section 621, the feed port 64 communicates with the inlet of the condenser 2 to allow the material to enter the feed passage 62;
when the feed piston 63 moves to the closing section 622, the feed seals the feed opening 64;
when the feeding piston 63 moves to the negative pressure section 623, the feeding hole 64 is closed, and meanwhile, the material in the feeding hole is pushed to move towards the side where the discharging hole 65 is located;
when the feed piston 63 moves to the compression section 624, the material is discharged through the discharge port 65.
When the feed piston 63 moves upward, the compression section 624 moves to the negative pressure section 623, and a negative pressure is generated in the feed passage 62, which is the same as the force when the pressure valve 17 is closed, so that the pressure valve 17 can be closed more tightly, thereby preventing the gas in the condenser 2 from flowing back.
In this embodiment, the feeding chute 1 is connected with a buffer chute 18, and an inlet of the feeding chute 1 is communicated with an outlet of the buffer chute 18.
In this embodiment, a buffer tower 19, a metering tank 20 and a primary filter 21 are further disposed between the feeding tank 1 and the tower kettle 2, an outlet of the feeding tank 1 is communicated with an inlet of the buffer tower 19, an outlet of the buffer tower 19 is communicated with an inlet of the metering tank 20, an outlet of the metering tank 20 is communicated with an inlet of the primary filter 21, and an outlet of the primary filter 21 is communicated with an inlet of the tower kettle 2.
In this embodiment, the purification tower 22 is disposed between the tower bottom 2 and the condenser 2, an inlet of the purification tower 22 is communicated with an outlet of the tower bottom 2, and an outlet of the purification tower 22 is communicated with the feed port 64 of the unidirectional feed mechanism 6.
The high-purity anhydrous hydrogen fluoride gas is obtained by introducing an oxidizing agent (a mixed gas of nitrogen and fluorine) into the purification column 22.
Please refer to fig. 6, this embodiment further provides a process for preparing electronic-grade hydrofluoric acid by using the above preparation apparatus, where anhydrous hydrogen fluoride is put into the feeding tank 1 according to a predetermined ratio, and heated by the tower kettle 2 to generate anhydrous hydrogen fluoride gas, and the anhydrous hydrogen fluoride gas rapidly enters the condenser 2 through the one-way feeding mechanism 6, and then is liquefied by the condenser 2, enters the blending tank 4, diluted and enters the finished product tank 5, and then is packaged and stored.
The whole preparation process is simple to operate and easy to implement, so that the whole production process is simplified, and the production efficiency is improved. By means of the special design of the preparation device, the quality of the hydrofluoric acid can be improved, and the preparation efficiency of the electronic-grade hydrofluoric acid can be improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A production apparatus for electronic grade hydrofluoric acid, comprising:
a feed tank for storing anhydrous hydrogen fluoride;
a tower kettle for obtaining anhydrous hydrogen fluoride gas;
a condenser for liquefying anhydrous hydrogen fluoride gas;
a blending tank for blending anhydrous hydrogen fluoride liquid; and
a finished product tank for storing hydrofluoric acid;
the outlet of the feeding groove is communicated with the inlet of the tower kettle, the outlet of the tower kettle is communicated with the inlet of the condenser, the outlet of the condenser is communicated with the inlet of the blending groove, and the outlet of the blending groove is communicated with the inlet of the finished product groove.
2. The manufacturing apparatus according to claim 1, characterized in that it comprises: a one-way feeding mechanism; the unidirectional feeding mechanism comprises a driving assembly, a feeding channel and a feeding piston, the feeding piston is arranged in the feeding channel, the driving assembly is arranged at one end of the feeding channel and used for driving the feeding piston to reciprocate, a discharging port is formed in one end, far away from the driving assembly, of the feeding channel and communicated with an inlet of the condenser, and a feeding port communicated with an outlet of the tower kettle is formed in the side wall of the feeding channel;
the feed inlet and the discharge outlet are intermittently communicated through the reciprocating motion of the feed piston, so that the material in the feed channel quickly enters the condenser.
3. The manufacturing apparatus of claim 2, wherein the drive assembly comprises: the device box is arranged at one end of the feeding channel, which is far away from the condenser, and the driving rod can movably penetrate through the side wall of the device box and then is connected with the feeding piston; the driving rod is movably connected with the equipment box along the axial direction of the driving rod, a first tooth part is arranged on the driving rod along the axial direction of the driving rod, the driving arm can be rotatably arranged on the equipment box, the first arc-shaped tooth block is arranged at one end, close to the driving rod, of the driving arm, and the first arc-shaped tooth block and the first tooth part are meshed with each other;
the driving arm can rotate by taking the rotating axis as a shaft to drive the first arc-shaped tooth block to rotate, so that the first arc-shaped tooth block is meshed with the first tooth part, and the driving rod can reciprocate along the axial direction of the driving rod.
4. The manufacturing apparatus of claim 3, wherein the drive arm is coupled to a rotation assembly for driving rotation thereof, the rotation assembly comprising: the rotating shaft can movably penetrate through the equipment box; the rotating shaft is movably connected with the equipment box along the circumferential direction of the rotating shaft; one end of the rotating shaft is connected with an output shaft of the rotating motor, the other end of the rotating shaft is located in the equipment box, a driving block is arranged at the end of the rotating shaft, one end of the transmission arm is eccentrically and rotatably connected with the driving block, and the other end of the transmission arm is rotatably connected with the driving arm.
5. The manufacturing device according to claim 3, wherein a side of the driving rod away from the first tooth portion is provided with a second tooth portion, and the second tooth portion is arranged along an axial direction of the driving rod; the inner wall of the equipment box is provided with two supporting arms, and a limit gear meshed with the second tooth part is rotatably arranged between the two supporting arms.
6. The manufacturing device according to claim 3, wherein a second arc-shaped tooth block is connected to one end of the driving arm away from the first arc-shaped tooth block, a movable rack engaged with the second arc-shaped tooth block is movably arranged on the inner wall of the equipment box, the movable rack is arranged in parallel with the driving rod, and the movable rack is movably connected with the inner wall of the equipment box along the axial direction of the movable rack; the movable rack is connected with a driving component for driving the movable rack to move;
the position of the meshing part of the movable rack and the second arc-shaped tooth block can be changed through the movement of the movable rack, so that when the driving arm rotates by taking the meshing part of the second arc-shaped tooth block as a shaft, the rotating range of the driving arm is different, and the moving range of the driving rod is changed.
7. The manufacturing apparatus of claim 1, wherein the feed channel comprises a feed section, a closed section, a negative pressure section, and a compression section in sequential communication;
when the feed piston moves to the feed section, the feed port is communicated with the inlet of the condenser so that the material enters the feed channel;
when the feeding piston moves to the closing section, the feeding piston seals the feeding hole;
when the feeding piston moves to the negative pressure section, the feeding hole is closed, and meanwhile, the material in the feeding hole is pushed to move towards one side of the discharging hole;
when the feed piston moves to the compression section, material is discharged through the discharge port.
8. The preparation device of claim 7, wherein a pressure valve is connected to the discharge port of the feed channel, an inlet of the pressure valve is communicated with the discharge port, and an outlet of the pressure valve is communicated with an inlet of the condenser;
the anhydrous hydrogen fluoride gas in the feed passage can be compressed by movement of the feed piston to open the pressure valve.
9. The process according to any one of claims 1 to 8, wherein anhydrous hydrogen fluoride is fed into the feed tank according to a predetermined ratio, the anhydrous hydrogen fluoride is heated in the column reactor to generate anhydrous hydrogen fluoride gas, the anhydrous hydrogen fluoride gas is rapidly fed into the condenser through the one-way feed mechanism, liquefied by the condenser, fed into the blending tank to be diluted, fed into a finished product tank, and then split-charged and stored.
CN202010861870.3A 2020-08-25 2020-08-25 Preparation device and preparation process for electronic-grade hydrofluoric acid Active CN112047302B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1990009957A1 (en) * 1989-02-27 1990-09-07 Mallinckrodt, Inc. Process for the continuous recovery of hydrogen fluoride gas
CN103991847A (en) * 2013-02-18 2014-08-20 福建省邵武市永晶化工有限公司 Preparation method for electron-grade hydrofluoric acid
CN106215447A (en) * 2016-08-29 2016-12-14 成都灵感元素科技有限公司 A kind of electronic-stage hydrofluoric acid production rectifying column
CN206276053U (en) * 2016-08-29 2017-06-27 王潇 A kind of electronic-stage hydrofluoric acid production rectifying column
CN109279577A (en) * 2018-10-17 2019-01-29 杨松 A kind of application method preparing electron level hydrogen fluoride oxidation reaction apparatus
CN210163122U (en) * 2019-07-03 2020-03-20 无锡东风新能源科技有限公司 Electronic-grade hydrofluoric acid production system

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1990009957A1 (en) * 1989-02-27 1990-09-07 Mallinckrodt, Inc. Process for the continuous recovery of hydrogen fluoride gas
CN103991847A (en) * 2013-02-18 2014-08-20 福建省邵武市永晶化工有限公司 Preparation method for electron-grade hydrofluoric acid
CN106215447A (en) * 2016-08-29 2016-12-14 成都灵感元素科技有限公司 A kind of electronic-stage hydrofluoric acid production rectifying column
CN206276053U (en) * 2016-08-29 2017-06-27 王潇 A kind of electronic-stage hydrofluoric acid production rectifying column
CN109279577A (en) * 2018-10-17 2019-01-29 杨松 A kind of application method preparing electron level hydrogen fluoride oxidation reaction apparatus
CN210163122U (en) * 2019-07-03 2020-03-20 无锡东风新能源科技有限公司 Electronic-grade hydrofluoric acid production system

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