CN107441750B - Sub-boiling distillation device and application thereof - Google Patents
Sub-boiling distillation device and application thereof Download PDFInfo
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- CN107441750B CN107441750B CN201710886240.XA CN201710886240A CN107441750B CN 107441750 B CN107441750 B CN 107441750B CN 201710886240 A CN201710886240 A CN 201710886240A CN 107441750 B CN107441750 B CN 107441750B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/008—Liquid distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4205—Reflux ratio control splitter
Abstract
The invention belongs to the technical field of preparation of electronic-grade reagents, and relates to a sub-boiling distillation device and application thereof. The invention provides a sub-boiling distillation device, which comprises a tank body, a preheating device and a condensing device, wherein a falling film heat exchanger and a gas purging device are arranged in the tank body, and the gas purging device is arranged at one side of the falling film heat exchanger and is used for purging a gas-phase product generated in the falling film heat exchanger; the top of the tank body is provided with a raw material inlet, the bottom of the tank body is provided with a residual liquid outlet, and the side of the tank body is provided with a gas phase outlet; the preheating device is connected with the raw material inlet, the gas phase outlet is connected with the condensing device, and the residual liquid outlet is connected with the preheating device. The sub-boiling distillation device can greatly improve the evaporation efficiency, has high yield, saves time and has low energy consumption; reasonable structure, low cost, convenient operation, good economic benefit and easy popularization and application.
Description
Technical Field
The invention belongs to the technical field of preparation of electronic-grade reagents, and relates to a sub-boiling distillation device for preparing an electronic-grade reagent or an ultra-clean high-purity reagent, in particular to the sub-boiling distillation device and application thereof.
Background
The high-purity electronic grade chemicals refer to ultra-clean high-purity reagents and solvents for the electronic industry, are mainly used for cleaning and corroding chips and cleaning the surfaces of silicon wafers, and comprise photoresist diluents, photosensitizers, photoacid generators, etchants, photoresist stripping agents, cleaning agents, chemical mechanical polishing abrasive matching agents of the chips, electroplating solutions and the like for chip processing. Electronic grade chemicals are key basic chemical materials in the manufacturing process of large-scale and ultra-large-scale Integrated Circuits (ICs), are used in many processes such as cleaning, photoetching, etching, photoresist removal and the like, and the purity and cleanliness of the electronic grade chemicals have very important influence on the yield, the electrical property and the reliability of the ICs. With the rapid development of the semiconductor industry and the continuous improvement of the semiconductor device technology, the quality requirement of electronic grade chemicals is higher and higher.
The basic requirement for electronic grade reagents is ultra-clean and high-purity, and the requirement for the content of metal ions in the reagents is more and more strict, and is already from 10-9(C9) Towards 10-12(C12) And (5) level development. In current practice, the methods for wet chemical purification are mainly ion exchange, molecular sieve separation, gas absorption, ultra-clean filtration and rectification. The general wet chemical production usually adopts a rectification method, and can be industrially carried out by using an azeotropic distillation method and a reduced pressure continuous distillation methodChemical preparation of C7、C8A grade of reagent. However, for wet chemicals with higher requirements, the metal ion content in the reagent is difficult to further reduce by using a distillation separation method alone, and in actual production, electronic-grade reagents are mostly prepared by using rectification for primary purification and matching with methods such as ion exchange and the like.
The sub-boiling distillation is a process of heating the solution to a temperature close to the boiling point and performing distillation separation while avoiding boiling of the solution. The principle of a general sub-boiling distiller is that the surface of a solution is heated by a heat radiation method, so that the surface temperature of the solution is slightly higher than the internal temperature of the solution, and static evaporation in a stable state is realized; thereby preparing the ultra-clean high-purity reagent. By the aid of the sub-boiling distillation method, the solution can escape from a gas-liquid interface in a molecular state in a sub-boiling process, and small droplets generated by boiling and impurities such as metal ions carried by aerosol are prevented from being mixed into a gas-phase product, so that purity of a distillation product can be greatly improved, and especially, removal of the metal ions is obviously improved.
Although C can now be prepared directly in the laboratory by a sub-boiling distillation process12The electronic grade reagent has the defects of very low evaporation efficiency, slow preparation speed, very small yield, high time and material consumption and the like. And the prior sub-boiling distillation device still has the problems of repeated evaporation and condensation of the solution, difficult control of the temperature of the evaporation surface and the like, is not beneficial to industrial large-scale production and can not be applied to industrial production.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The first purpose of the present invention is to provide a sub-boiling distillation apparatus which has high evaporation efficiency, is easy to control, can greatly improve the yield, and is advantageous for industrial mass production.
The second purpose of the invention is to provide the application of the sub-boiling distillation device in preparing electronic-grade reagents, and the reagents prepared by the device have high purity and high yield, and the quality can meet the requirements of ultra-clean high-purity reagents in the semiconductor industry.
In order to achieve the purpose, the invention adopts the technical scheme that:
according to one aspect of the invention, the invention provides a sub-boiling distillation device, which comprises a tank body, a preheating device and a condensing device, wherein a falling film heat exchanger and a gas purging device are arranged in the tank body, and the gas purging device is arranged at one side of the falling film heat exchanger and is used for purging a gas-phase product generated in the falling film heat exchanger;
the top of the tank body is provided with a raw material inlet, the bottom of the tank body is provided with a residual liquid outlet, and the side of the tank body is provided with a gas phase outlet;
the preheating device is connected with the raw material inlet, the gas phase outlet is connected with the condensing device, and the residual liquid outlet is connected with the preheating device.
According to the invention, through the arrangement of the pre-heating device, the falling film heat exchanger, the gas purging device, the condensing device and the like, the problems of low evaporation efficiency, small yield, large material and time consumption and the like of the sub-boiling distillation device in the prior art are solved, the evaporation efficiency is greatly improved while the product quality is ensured, the production efficiency is greatly improved, the operation is convenient, the control is easy, the cost is low, and a solid foundation is laid for industrial mass production and rapid realization of industrialization. The preheating device is convenient to control the temperature of the raw materials; the arrangement of the falling film heat exchanger improves the heat exchange efficiency in the sub-boiling distillation process; the arrangement of the gas purging device is beneficial to quickly discharging evaporated gas-phase products, and under the condition of not changing the evaporation temperature and the saturated vapor pressure, the evaporation efficiency is improved by a method of reducing the molecular content of the isolate in the environment, so that the yield is greatly improved, and the efficient production of the electronic-grade reagent is realized.
As a further preferred technical scheme, the falling film heat exchanger is a plate-type falling film heat exchanger, a liquid distributor is arranged at the upper end of the plate-type falling film heat exchanger, and the liquid distributor is communicated with the raw material inlet.
The plate-type falling film heat exchanger has the advantages of low manufacturing cost, small occupied area, high heat transfer coefficient, easy cleaning and convenient maintenance. In the falling film evaporation heat transfer, the flowing state of the liquid film is one of more important parameters, and the arrangement of the liquid distributor is favorable for improving the distribution uniformity of the liquid film and improving the heat exchange efficiency of the heat exchanger.
As a further preferred technical scheme, the liquid distributor is a double-layer liquid distribution plate type falling film liquid distributor, the liquid distributor comprises an upper liquid distribution plate and a lower liquid distribution plate, a plurality of through holes are formed in the upper liquid distribution plate and the lower liquid distribution plate, a flow guide channel communicated with the lower portion is formed in the liquid distributor, a liquid distribution plate is arranged below the lower liquid distribution plate, and a plurality of small holes are formed in the bottom of the liquid distribution plate uniformly.
Furthermore, the liquid distributor comprises an upper liquid distribution plate and a lower liquid distribution plate, a plurality of through holes are formed in the upper liquid distribution plate and the lower liquid distribution plate, the upper end face of the upper liquid distribution plate is connected with a cylindrical overflow plate, a plurality of liquid distribution holes used for spraying the solution entering the overflow plate to the lower liquid distribution plate are uniformly formed in the part, located inside the overflow plate, of the upper liquid distribution plate, and a film distribution gap is formed between the lower liquid distribution plate and the heat exchange plate.
Adopt two-layer cloth liquid plate formula falling film spreader, and go up and all open the through-hole on cloth liquid plate and the cloth liquid plate down, but also be provided with the water conservancy diversion passageway, can guarantee the even inflow cloth liquid dish of material in, and then make on the even runner heat transfer board of material for cloth membrane is effectual, and heat transfer performance is high.
Optionally, in the liquid distributor of the present invention, a cylindrical overflow plate may be further disposed on the upper liquid distribution plate, so that the material can be kept at a certain liquid level inside the cylindrical overflow plate, thereby preventing occurrence of a dry wall phenomenon during a film distribution process, and the liquid distributor has advantages of uniform liquid film distribution and stable film formation.
The through holes are uniformly arranged.
As a further preferred technical scheme, the plate-type falling film heat exchanger comprises a heat exchange plate group, wherein the heat exchange plate group is provided with a medium inlet and a medium outlet, the heat exchange plate group is arranged between a fixed plate and a movable plate, and the fixed plate and the movable plate are fixed through pull rods arranged on two sides of the heat exchange plate group.
Furthermore, the heat exchange plate group comprises a plurality of heat exchange plates, and a sealing rubber gasket is arranged between every two adjacent heat exchange plates.
Furthermore, an angle steel or channel steel or a baffle plate is arranged between two adjacent heat exchange plates.
Further, different heat exchange media can be selected according to actual needs for the plate-type falling film heat exchanger.
The detachable plate type falling film heat exchanger is adopted, and the heat exchange plates are easily increased or reduced through the arrangement of the fixed plate, the movable plate and the pull rod, so that the effect of increasing or reducing the heat exchange area can be achieved, the heat exchange area can be conveniently adjusted according to the process requirement, and the effective utilization rate of the heat exchange plates is high; but also is convenient for the replacement of the heat exchange medium. Meanwhile, the device is convenient to clean and maintain, convenient to install and disassemble, and has the advantages of small occupied area, large treatment capacity and high evaporation efficiency.
As a further preferable technical scheme, the condensation device also comprises a reflux controller, wherein the reflux controller is connected with the condensation device;
the reflux controller is provided with a liquid phase reflux outlet and a liquid phase finished product outlet, the condensing device is provided with a gas phase product outlet, the liquid phase reflux outlet is connected with the preheating device, the gas phase product outlet is connected with the gas blowing device through an inert gas circulating device, and the liquid phase finished product outlet is connected with the finished product storage tank.
As a further preferable technical scheme, the reflux controller is a reflux controller with an adjustable reflux ratio, comprises a reflux ratio controller and an electromagnetic coil, and sets reflux time and extraction time through the reflux ratio controller.
The reflux controller with adjustable reflux ratio is adopted, so that the proportion of reflux quantity to produced quantity is more conveniently adjusted, and the reflux controller is visual, easy to control and operate, can reduce labor intensity and is convenient to repeat.
As a further preferred technical scheme, the condensing device is a vertical condenser with a pressure reduction nozzle.
Further, the pressure reduction nozzle is a detachable nozzle, the detachable nozzle is installed inside the vertical condenser, and the detachable nozzle is connected with a short port arranged outside the condenser.
Further, the detachable nozzle is connected with the short port through a nozzle connecting pipe, and the nozzle connecting pipe is a movable pipe.
The vertical condenser with the pressure reduction nozzle can reduce the occupied area and save energy. In addition, the detachable nozzle is adopted, so that the cleaning and the replacement are convenient, the maintenance is convenient, the maintenance cost is reduced, and the working efficiency is improved.
As a further preferable technical scheme, the preheating device is a microwave preheating device adopting digital control.
Further, the microwave preheating device comprises a microwave generator, a temperature sensor and a digital controller, wherein the microwave generator and the temperature sensor are connected with the digital controller.
Furthermore, the control system of the microwave preheating device is a control system based on PLC control so as to realize the collection and control of the temperature in the heating device. The temperature sensor is arranged in a microwave field, converts a temperature signal into an electric signal and then sends the electric signal to the PLC for data processing, and an output control signal is calculated through a fuzzy control algorithm to adjust the power supply of the microwave generator, so that the constant temperature control in the microwave preheating device is realized.
The invention adopts the microwave preheating device with digital control, is convenient for temperature control, solves the problem that the evaporation surface temperature is difficult to control in the prior art, improves the control capability of the device on the raw material temperature in the sub-boiling distillation process, and further improves the heat exchange efficiency. Meanwhile, the device realizes high precision and digitization of temperature measurement, and has the advantages of uniform heating, good temperature controllability, reliable operation, simple equipment, convenient operation, easy maintenance, small occupied area and low operation cost.
As a further preferable technical solution, the gas purging device is an inert gas purging device with an electric heating device.
Further, the gas purging device is a gas curtain type high-speed inert gas purging device with an electric heating device.
Further, preheating inert gas to a set evaporation temperature, wherein the purging direction is along the horizontal direction of the heat exchange plate group, and the distance between the gas curtain and the liquid level of the falling film is 1-3 mm; preferably, the gas curtain is 2mm from the falling film liquid level.
Further, the inert gas is one or more of nitrogen, helium and argon.
The gas curtain type high-speed inert gas purging device is adopted to inject inert gas into the falling film heat exchanger, so that gas phase generated in the heat exchanger is transferred, the evaporation efficiency is further improved, and the yield is further improved.
As a further preferable mode, a sight glass for observing a liquid film inside the falling film heat exchanger is provided on the tank.
According to another aspect of the invention, there is provided the use of a sub-boiling distillation apparatus as hereinbefore described in the preparation of an electronic grade reagent.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the sub-boiling distillation device provided by the invention, the combined arrangement of the pre-heating device, the falling film heat exchanger, the gas purging device and the condensing device effectively improves the temperature control capability of the device in the sub-boiling distillation process, greatly improves the evaporation efficiency, has high yield, saves time and has low energy consumption; further effectively solves the problem that the sub-boiling distillation device in the prior art is not beneficial to industrialized scale production, and lays a solid foundation for the rapid realization of industrialization of the sub-boiling distillation technology. Meanwhile, the device has the advantages of reasonable structure, low cost, safety, reliability, easy realization, convenient operation, good economic benefit and easy popularization and application.
2. The electronic-grade reagent prepared by the sub-boiling distillation device provided by the invention can effectively remove solid impurities, metal impurities and the like in raw materials, has high purity, high yield and good benefit, the product purity (calculated by the metal impurities) is not lower than 99.99999% (w/w), and is beneficial to industrial large-scale production, the product quality can meet the requirement of ultra-clean high-purity reagents in the semiconductor industry, and the continuous and stable development of the semiconductor industry is promoted.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic view of a sub-boiling distillation apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a liquid distributor according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a heat exchange plate set according to an embodiment of the present invention;
fig. 4 is a schematic structural diagram of a condensing device according to an embodiment of the present invention.
Icon: 100-tank body; 101-raw material inlet; 102-a gas phase outlet; 103-raffinate outlet; 200-preheating device; 300-a condensing unit; 301-gas phase product outlet; 302-a depressurization nozzle; 303-short interface; 304-nozzle connection tube; 400-a falling film heat exchanger; 401-heat exchange plate groups; 402-a fixed plate; 403-a movable plate; 404-a pull rod; 500-a gas purge; 600-liquid distributor; 601-arranging a liquid distribution plate; 602-lower liquid distribution plate; 603-liquid distribution disc; 604-small holes; 700-reflux controller; 701-liquid phase reflux outlet; 702-liquid phase product outlet.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present 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.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top", "bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically 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.
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
Examples
Fig. 1 is a schematic view of a sub-boiling distillation apparatus according to an embodiment of the present invention, and as shown in fig. 1, the embodiment provides a sub-boiling distillation apparatus including a tank 100, a preheating device 200, and a condensing device 300, wherein a falling film heat exchanger 400 and a gas purging device 500 are disposed in the tank 100, and the gas purging device 500 is disposed at one side of the falling film heat exchanger 400 for purging a gas-phase product generated in the falling film heat exchanger 400; the top of the tank body 100 is provided with a raw material inlet 101, the bottom is provided with a residual liquid outlet 103, and the side is provided with a gas phase outlet 102; the preheating device 200 is connected with the raw material inlet 101, the gas phase outlet 102 is connected with the condensing device 300, and the residual liquid outlet 103 is connected with the preheating device 200.
Wherein, falling film heat exchanger 400 is plate-type falling film heat exchanger, and plate-type falling film heat exchanger's upper end is provided with liquid distributor 600, and liquid distributor 600 is linked together with raw materials import 101.
The sub-boiling distillation device also comprises a reflux controller 700, wherein the reflux controller 700 is connected with the condensing device 300; the reflux controller 700 is provided with a liquid phase reflux outlet 701 and a liquid phase finished product outlet 702, the condensing device 300 is provided with a gas phase product outlet 301, the liquid phase reflux outlet 701 is connected with the preheating device 200, the gas phase product outlet 301 is connected with the gas purging device 500 through an inert gas circulating device, and the liquid phase finished product outlet 702 is connected with a finished product storage tank.
Fig. 2 is a schematic structural view of a liquid distributor according to an embodiment of the present invention, as shown in fig. 2, the liquid distributor 600 is a double-layer liquid distribution plate type falling film liquid distributor, the liquid distributor 600 includes an upper liquid distribution plate 601 and a lower liquid distribution plate 602, a plurality of through holes are respectively formed on the upper liquid distribution plate 601 and the lower liquid distribution plate 602, a flow guide channel communicated with the lower portion is formed on the liquid distributor 600, a liquid distribution plate 603 is arranged below the lower liquid distribution plate 602, and a plurality of small holes 604 are uniformly formed in the bottom of the liquid distribution plate 603.
As an optional technical scheme, the liquid distributor 600 comprises an upper liquid distribution plate 601 and a lower liquid distribution plate 602, a plurality of through holes are formed in the upper liquid distribution plate 601 and the lower liquid distribution plate 602, a cylindrical overflow plate is connected to the upper end face of the upper liquid distribution plate 601, a plurality of liquid distribution holes for spraying the solution entering the overflow to the lower liquid distribution plate 602 are uniformly formed in the part, located inside the overflow plate, of the upper liquid distribution plate 601, and a film distribution gap is formed between the lower liquid distribution plate 602 and the heat exchange plate. The through holes are uniformly arranged.
Fig. 3 is a schematic structural view of a heat exchange plate group according to an embodiment of the present invention, and as shown in fig. 3, a plate-type falling film heat exchanger includes a heat exchange plate group 401, a medium inlet and a medium outlet are disposed on the heat exchange plate group 401, the heat exchange plate group 401 is disposed between a fixed plate 402 and a movable plate 403, and the fixed plate 402 and the movable plate 403 are fixed by tie rods 404 disposed on two sides of the heat exchange plate group 401.
Further, the heat exchange plate set 401 includes a plurality of heat exchange plates, and a sealing rubber gasket is disposed between two adjacent heat exchange plates. Angle steel or channel steel or a baffle is arranged between two adjacent heat exchange plates.
Further, different heat exchange media can be selected according to actual needs for the plate-type falling film heat exchanger.
In this embodiment, the reflux controller 700 is a reflux controller with adjustable reflux ratio, and includes a reflux ratio controller and an electromagnetic coil, and sets reflux time and extraction time by the reflux ratio controller.
Fig. 4 is a schematic structural diagram of a condensing device according to an embodiment of the present invention, and as shown in fig. 4, the condensing device 300 is a vertical condenser with a pressure-reducing nozzle 302.
Further, pressure reduction nozzle 302 is detachable nozzle, and detachable nozzle installs in the inside of vertical condenser, and detachable nozzle is connected with the short circuit mouth 303 that sets up at the condenser outside. The detachable nozzle is connected to the short connector 303 through a nozzle connection pipe 304, and the nozzle connection pipe 304 is a movable pipe.
In this embodiment, the preheating device 200 is a microwave preheating device using digital control.
Further, the microwave preheating device comprises a microwave generator, a temperature sensor and a digital controller, wherein the microwave generator and the temperature sensor are connected with the digital controller. The control system of the microwave preheating device is a control system based on PLC control so as to realize the collection and control of the temperature in the heating device. The temperature sensor is arranged in a microwave field, converts a temperature signal into an electric signal and then sends the electric signal to the PLC for data processing, and an output control signal is calculated through a fuzzy control algorithm to adjust the power supply of the microwave generator, so that the constant temperature control in the microwave preheating device is realized.
In this embodiment, the gas purging device 500 is an inert gas purging device with an electric heating device.
Further, the gas purging device 500 is a gas curtain type high-speed inert gas purging device with an electric heating device. Preheating inert gas to a set evaporation temperature, wherein the purging direction is along the horizontal direction of the heat exchange plate group 401, and the distance between the gas curtain and the liquid level of the falling film is 1-3 mm; preferably, the gas curtain is 2mm from the falling film liquid level. The inert gas is one or more of nitrogen, helium and argon.
The inert gas in this example is helium.
As an alternative solution, a sight glass for observing the liquid film inside the falling film heat exchanger 400 is provided on the tank 100.
The embodiment also provides the application of the sub-boiling distillation device in preparing electronic-grade reagents. For example, the reagents for preparing ultra-clean high-purity hydrochloric acid, nitric acid, acetic acid, ethylene carbonate, dimethyl carbonate, tetraethyl orthosilicate and the like.
The working principle of the sub-boiling distillation device provided by the invention is as follows:
preheating the raw material by adopting a digitally controlled microwave preheating device 200 to ensure that the feeding temperature is raised to be equal to or slightly lower than the set evaporation temperature; then, the preheated material enters the falling film heat exchanger 400 from the raw material inlet 101 of the tank 100, forms falling film flow through the liquid distributor 600 to ensure the uniformity of liquid film distribution, and then enters the falling film heat exchanger 400; the falling film flows through the plate-type falling film heat exchanger 400 heated to the set evaporation temperature to form falling film sub-boiling evaporation, and the residual liquid flows back to the preheating device 200 from the residual liquid outlet 103.
The gas phase product separated by the sub-boiling distillation is purged out of the falling film heat exchanger 400 using an inert gas purging device 500 preheated to a set evaporation temperature; the gas purging device 500 is a gas curtain type high-speed inert gas purging device with an electric heating device, the inert gas is helium, the helium is purged horizontally along the direction of the heat exchange plate group 401, and the distance between a gas curtain and the liquid level of the falling film is 2 mm.
Helium blown at a high speed carries an evaporated gas-phase product to enter a vertical condenser through a depressurization nozzle 302, the condensed liquid-phase product and the condensed gas-phase product are respectively discharged from the condenser, the gas-phase product flows back to the gas blowing device 500 from a gas-phase product outlet 301 through an inert gas circulation device, a part of the liquid-phase product adopts a finished product through a liquid-phase finished product outlet 702 of the backflow controller 700, and a part of the liquid-phase product flows back to the preheating device 200 through a liquid-phase backflow outlet 701, so that high-efficiency production of the electronic-grade high-purity reagent is realized.
According to the invention, through the arrangement of the preheating device 200, the falling film heat exchanger 400, the gas purging device 500, the condensing device 300 and the like, the evaporation efficiency is greatly improved, the production efficiency is greatly improved, the operation is convenient, the control is easy, the cost is low, and a solid foundation is laid for industrial mass production and rapid realization of industrialization. The arrangement of the microwave preheating device 200 improves the control capability of the distillation device on the temperature of the raw materials; the arrangement of the plate-type falling film heat exchanger 400 improves the heat exchange efficiency in the sub-boiling distillation process; the arrangement of the high-speed inert gas purging device 500 is helpful for quickly discharging evaporated gas-phase products, and under the condition of not changing the evaporation temperature and the saturated vapor pressure, the evaporation efficiency is improved by a method of reducing the molecular content of the separator in the environment, so that the yield is greatly improved, and the high-efficiency production of the electronic-grade reagent is realized.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. The sub-boiling distillation device is characterized by comprising a tank body, a preheating device and a condensing device, wherein a falling film heat exchanger and a gas purging device are arranged in the tank body, and the gas purging device is arranged on one side of the falling film heat exchanger and used for purging a gas-phase product generated in the falling film heat exchanger;
the top of the tank body is provided with a raw material inlet, the bottom of the tank body is provided with a residual liquid outlet, and the side of the tank body is provided with a gas phase outlet;
the falling film heat exchanger is a plate type falling film heat exchanger, a liquid distributor is arranged at the upper end of the plate type falling film heat exchanger, and the liquid distributor is communicated with the raw material inlet;
the sub-boiling distillation device also comprises a reflux controller, and the reflux controller is connected with the condensing device; the reflux controller is provided with a liquid phase reflux outlet and a liquid phase finished product outlet, the condensing device is provided with a gas phase product outlet, the liquid phase reflux outlet is connected with the preheating device, the gas phase product outlet is connected with the gas purging device through an inert gas circulating device, and the liquid phase finished product outlet is connected with the finished product storage tank;
the preheating device is connected with the raw material inlet, the gas phase outlet is connected with the condensing device, and the residual liquid outlet is connected with the preheating device.
2. The sub-boiling distillation apparatus according to claim 1, wherein the liquid distributor is a double-layer liquid distribution plate type falling film liquid distributor, the liquid distributor comprises an upper liquid distribution plate and a lower liquid distribution plate, a plurality of through holes are formed in the upper liquid distribution plate and the lower liquid distribution plate, a flow guide channel communicated with the lower part is arranged on the liquid distributor, a liquid distribution disc is arranged below the lower liquid distribution plate, and a plurality of small holes are uniformly formed in the bottom of the liquid distribution disc.
3. A sub-boiling distillation apparatus according to claim 1, wherein the plate-type falling-film heat exchanger comprises a heat exchange plate group, the heat exchange plate group is provided with a medium inlet and a medium outlet, and the heat exchange plate group is arranged between a fixed plate and a movable plate, and the fixed plate and the movable plate are fixed by a pull rod arranged on both sides of the heat exchange plate group.
4. The sub-boiling distillation apparatus according to claim 1, wherein the reflux controller is an adjustable reflux ratio reflux controller comprising a reflux ratio controller and a solenoid, and the reflux time and the withdrawal time are set by the reflux ratio controller.
5. A sub-boiling distillation apparatus according to any one of claims 1 to 4, wherein the condensing means is a vertical condenser with a pressure reduction nozzle.
6. A sub-boiling distillation apparatus according to any one of claims 1 to 4, wherein the preheating means is digitally controlled microwave preheating means.
7. A sub-boiling distillation apparatus according to any one of claims 1 to 4, wherein the gas purging means is an inert gas purging means with electrical heating means.
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| RU223285U1 (en) * | 2023-12-22 | 2024-02-12 | Общество с ограниченной ответственностью "Торговый Дом "ХИММЕД" | DEVICE FOR PRODUCING HIGH-PURITY SULFURIC ACID BY SURFACE EVAPORATION METHOD |
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| CN101570318A (en) * | 2008-04-28 | 2009-11-04 | 多氟多化工股份有限公司 | Method for producing electronic-stage hydrofluoric acid |
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| CN203123596U (en) * | 2012-12-27 | 2013-08-14 | 华东理工大学 | Vertical falling-film evaporator |
| CN104192803A (en) * | 2014-09-10 | 2014-12-10 | 太仓中化环保化工有限公司 | Sub-boiling distillation method for high-purity hydrochloric acid |
| CN104826351A (en) * | 2015-05-11 | 2015-08-12 | 珠海格力电器股份有限公司 | Falling-film evaporator, liquid distributor and liquid equalizing plate |
| CN206444214U (en) * | 2017-01-25 | 2017-08-29 | 东莞瑞德环保科技有限公司 | A kind of combined type sub-boiling distillation system |
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| RU223285U1 (en) * | 2023-12-22 | 2024-02-12 | Общество с ограниченной ответственностью "Торговый Дом "ХИММЕД" | DEVICE FOR PRODUCING HIGH-PURITY SULFURIC ACID BY SURFACE EVAPORATION METHOD |
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| CN107441750A (en) | 2017-12-08 |
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