Distillation system for electronic grade analysis acid

Abstract

The utility model provides a distillation system for electronic grade analysis acid, and aims to solve the technical problems of poor distillation continuity and unstable purification quality in the conventional laboratory. The liquid storage tank is provided with a liquid outlet pipeline, and the liquid outlet pipeline is provided with a regulating valve and a pump. The input end of the multi-stage distillation unit is connected with the liquid outlet pipeline, and the multi-stage distillation unit comprises a plurality of distillers which are connected in series. And an acid receiving disc is arranged in each distiller and is used for accommodating condensed acid liquor of the distiller. And the filling unit comprises a turntable and subpackaging bottles. The turntable is communicated with the output end of the multi-stage distillation unit through a connecting pipe and is provided with a filling pipe group. And the split charging bottle is matched with the infusion tube group. And the condensed acid liquid in one acid receiving disc is conveyed to the next distiller for continuous distillation until the target acid liquid flowing out of the output end of the multi-stage distillation unit reaches the electronic-grade purity and flows to the rotating disc to be filled into the subpackaging bottles. And the continuity of the experiment is ensured through the distillation of the multi-stage distillation unit, so that the obtained target acid liquid can be directly filled into a subpackaging bottle.

Description

Technical Field

[0001] This application relates to the field of purification of electronic-grade analytical acids, and particularly to a distillation system for electronic-grade analytical acids. Background Art

[0002] Electronic Grade Acid refers to high-purity acids used in industries such as semiconductors, optoelectronics, and microelectronics. These acids have extremely low impurity contents and can meet the strict requirements of high-end manufacturing. It mainly includes electronic-grade hydrofluoric acid, electronic-grade nitric acid, electronic-grade hydrochloric acid, etc. Although China has gradually made progress in the production of electronic-grade acids, the overall technical level still lags behind the international advanced level. Taking the production of ultra-high-purity hydrofluoric acid as an example, it is usually prepared in the following way: First, liquid hydrogen fluoride is distilled in a distillation column, and the resulting hydrogen fluoride gas then enters a spray absorption column for reverse water absorption. After the spray absorption liquid reaches a certain concentration, it can be stored in a high-level storage tank as an intermediate product. Subsequently, the intermediate product is rectified to obtain the target ultra-high-purity hydrofluoric acid, which is then stored in a finished product tank. However, this method is mainly applied to large-scale production and has extremely high requirements for equipment. It is not suitable for laboratory preparation and purification of acids.

[0003] As is well known, using laboratory-scale trials to evaluate the feasibility of later large-scale production is an indispensable means in the process optimization. During the process of preparing acid solutions in laboratory-scale trials, technicians found that the acid distillation purifier had serious problems of running, overflowing, dripping, and leaking, posing certain safety hazards. Therefore, some artificial auxiliary treatment operations were usually required, which not only led to poor continuity of the reaction process but also increased the risk of introducing impurities into the target acid solution, being unfavorable for the purification of the target acid solution. At the same time, the quality of distilled hydrofluoric acid was completely controlled by technicians' experience. Therefore, the purity error of the target acid solution in different batches was large, and subsequent packaging processes could not be directly carried out, resulting in low efficiency. Utility Model Content

[0004] The present utility model provides a distillation system for electronic-grade analytical acids to solve the problems raised in the above background art.

[0005] A distillation system for electronic-grade analytical acids, which includes:

[0006] A liquid storage tank, provided with a liquid outlet pipe; the liquid outlet pipe is provided with a regulating valve and a pump;

[0007] A multi-stage distillation unit, whose input end is connected to the liquid outlet pipe, and includes a plurality of distillers connected in series; each distiller is provided with an acid receiving tray for accommodating the condensed acid liquid of the distiller;

[0008] The filling unit includes a turntable and dispensing bottles; the turntable is communicated with the output end of the multi-stage distillation unit through a connecting pipe, and the turntable is provided with a perfusion pipe group; the dispensing bottles are arranged to match the perfusion pipe group.

[0009] Among them, the condensed acid liquid in an acid receiving tray is sent to the next distiller for continuous distillation until the target acid liquid flowing out of the output end of the multi-stage distillation unit reaches electronic grade purity and flows to the turntable for filling the dispensing bottles.

[0010] Further, the multi-stage distillation unit includes a first distiller and a second distiller connected in series; the input end of the first distiller is connected to the liquid outlet pipe, and the distillate pipe of the acid receiving tray arranged thereon is connected to the input end of the second distiller for condensing the conveyance of acid liquid to the second distiller; the output end of the second distiller is connected to the filling unit.

[0011] Further, a heating plate is provided at the bottom end inside each distiller, and a condenser is provided at the top end inside it. The acid receiving tray is arranged between the heating plate and the condenser; a first liquid level sensor and a first controller are provided on the side wall of the first distiller, and a second liquid level sensor and a second controller are provided on the side wall of the second distiller.

[0012] Further, the output end of the first controller is connected to the regulating valve, and its input end is connected to the first liquid level sensor.

[0013] Further, the input end of the second controller provided in the second distiller is connected to the second liquid level sensor, and its output end is connected to the heating plate provided in the first distiller.

[0014] Further, a waste liquid discharge pipe is also provided on the side wall near the bottom end of each distiller; a liquid outlet valve is provided on each waste liquid discharge pipe.

[0015] Further, a control valve is provided on the distillate pipe of the second distiller.

[0016] The turntable includes a connecting pipe, a meshing disc and a power disc; one end of the connecting pipe is connected to the distillate pipe of the second distiller, and the other end is installed at the top of the meshing disc and is communicated with the meshing disc; a perfusion pipe group communicated with the meshing disc is installed at the bottom end of the meshing disc; the power disc is arranged to match and mesh with the meshing disc; the center of the power disc is externally connected to the movable end of a motor.

[0017] Further, the filling unit further includes a dispensing table; the dispensing table is arranged below the meshing disc; a plurality of mounting rack groups are uniformly spaced along the circumferential direction at the top of the dispensing table; the mounting rack groups are arranged to match the perfusion pipe group.

[0018] Further, the perfusion tube group has two perfusion tubes, and the two perfusion tubes are disposed opposite to the turntable with the center of the turntable as the center; the number of the mounting brackets is an even number.

[0019] Further, a third liquid level sensor is provided on the side wall of each dispensing bottle; a third controller is installed on the dispensing table, and the output ends of the third controller are respectively connected to the motor and the control valve, and its input end is connected to the third liquid level sensor.

[0020] Compared with the prior art, the beneficial effects of the present utility model are as follows:

[0021] (1) The crude acid in the liquid storage tank can be distilled by a two-stage distillation unit, and during the distillation, the purity of the target acid solution distilled out is adjusted by controlling the input amount of the crude acid through the liquid level feedback of the first liquid level sensor and controlling the heating power of the heating plate provided in the first distiller through the liquid level feedback of the second liquid level sensor. While ensuring the continuity of the experiment, the target acid solution can also reach the electronic grade purity.

[0022] (2) By the liquid level feedback of the third liquid level sensor, the rotation state of the motor and the opening and closing state of the control valve are respectively controlled, thereby realizing the automatic filling of the target acid solution. Description of the Drawings

[0023] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0024] Figure 1 It is a connection schematic diagram of a distillation system for electronic grade analytical acid according to an embodiment of the present application;

[0025] Figure 2 It is a schematic diagram of a distillation system for electronic grade analytical acid according to an embodiment of the present application, in which a mounting bracket group with dispensing bottles is matched with a perfusion tube group.

[0026] Reference Signs:

[0027] 1. Liquid storage tank; 11. Regulating valve; 12. Pump;

[0028] 20. First distiller; 21. Second distiller; 2200. First liquid level sensor; 2201. First controller; 2210. Second liquid level sensor; 2211. Second controller; 23. Acid receiving tray; 24. Heating plate; 25. Condenser; 26. Liquid outlet valve;

[0029] 30. Control valve; 31. Meshing disc; 32. Perfusion pipe group; 33. Sub-packaging table; 34. Sub-packaging bottle; 350. Third liquid level sensor; 351. Third controller; 36. Mounting rack; 37. Connecting pipe;

[0030] 40. Motor; 41. Power disc. Detailed implementation manners

[0031] In the following text, only some exemplary embodiments are simply described. As those skilled in the art can recognize, the described embodiments can be modified in various different ways without departing from the spirit or scope of the present invention. Therefore, the drawings and the description are considered to be exemplary in nature rather than restrictive.

[0032] In the description of the present invention, it should be understood that the orientation or positional relationships indicated by the terms "center", "upper", "lower", "top", "bottom", "inner", "outer", "circumferential", etc. are based on the orientation or positional relationships shown in the drawings, or the orientation or positional relationships in which the products of the present invention are customarily placed during use, or the orientation or positional relationships commonly understood by those skilled in the art. These are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as a limitation to the present invention.

[0033] In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include one or more of such features. In the description of the present invention, "a plurality" means two or more unless otherwise specifically defined.

[0034] In the present invention, unless otherwise clearly specified and defined, the terms "mount", "connect", "couple", etc. should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral body; it can be a mechanical connection, an electrical connection, or a communication connection; it can be directly connected, or indirectly connected through an intermediate medium, and can be the internal communication of two elements or the interaction relationship between two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0035] In the present utility model, unless otherwise clearly defined and limited, the first feature being "above" or "below" the second feature may include direct contact between the first and second features, or may include the situation where the first and second features are not in direct contact but in contact through additional features therebetween. Moreover, the first feature being "above", "over" and "on top of" the second feature includes the first feature being directly above and obliquely above the second feature, or merely indicating that the horizontal height of the first feature is higher than that of the second feature. The first feature being "below", "beneath" and "underneath" the second feature includes the first feature being directly below and obliquely below the second feature, or merely indicating that the horizontal height of the first feature is lower than that of the second feature.

[0036] The following disclosure provides many different embodiments or examples for implementing different structures of the present utility model. To simplify the disclosure of the present utility model, components and settings of specific examples are described below. Of course, they are merely examples and are not intended to limit the present utility model. In addition, the present utility model may repeat reference numerals in different examples. This repetition is for the purpose of simplification and clarity, and does not itself indicate the relationship between various embodiments discussed. In addition, the present utility model provides examples of various specific processes and materials, but those of ordinary skill in the art may be aware of the application of other processes and / or the use of other materials.

[0037] The embodiments of the present utility model will be described in detail below with reference to the accompanying drawings.

[0038] The embodiments of the present utility model provide a distillation device for electronic grade analytical acid. Please refer to Figure 1 - Figure 2 . The distillation device for electronic grade analytical acid includes a liquid storage tank 1, a multi-stage distillation unit and a filling unit.

[0039] Specifically,

[0040] The liquid storage tank 1 is used for storing crude acid. It is provided with a liquid outlet pipeline, and a regulating valve 11 and a pump 12 are sequentially arranged at the liquid outlet pipeline. Preferably, the pump 12 can adopt a peristaltic pump.

[0041] The multi-stage distillation unit, whose input end is connected to the liquid outlet pipeline, includes a plurality of distillers connected in series. The crude acid is pumped into the distillers for distillation. Through the non-contact treatment and transfer of the crude acid, the risk of introducing impurities in the reaction process is reduced. Moreover, after the crude acid is distilled through the multi-stage distillation unit, it is beneficial to obtain electronic grade acid solution.

[0042] Each distiller can be made of corrosion-resistant materials such as high-purity PTFE, FEP, and PFA. It is internally provided with an acid receiving tray 23 for accommodating the condensed acid liquid of the distiller. A distillate pipeline is provided near the bottom end of the acid receiving tray 23. A liquid level sensor and a controller are provided on the side wall of each distiller. Preferably, the liquid level sensor uses a non-contact liquid level gauge. A waste liquid discharge pipeline is provided on the side wall near the bottom end of each distiller, and a liquid discharge valve 26 is provided at the waste liquid discharge pipe to facilitate the treatment of the waste liquid that accumulates at the bottom end of the distiller. A heating plate 24 is provided at the inner bottom end of each distiller. To prevent damage to the heating plate 24, the heating plate 24 is preferably coated with corrosion-resistant materials such as high-purity PTFE, FEP, and PFA. A condenser 25 is provided at the inner top end of each distiller. The acid receiving tray 23 is arranged between the heating plate 24 and the condenser 25. Preferably, the multi-stage distillation unit adopts a two-stage distillation form, so it includes a first distiller 20 and a second distiller 21. The first distiller 20 and the second distiller 21 are connected in series. Among them,

[0043] The first distiller 20 has its input end connected to the liquid outlet pipeline. The side wall of the first distiller is provided with a first liquid level sensor 2200 and a first controller 2201. The input end of the first controller is electrically connected to the first liquid level sensor 2200, and its output end is electrically connected to the regulating valve 11. After the liquid level signal of the first liquid level sensor 2200 is transmitted to the first controller 2201, the first controller 2201 processes and controls the adjustment of the regulating valve 11, thereby improving the automatic control of the crude acid inflow from the storage tank 1 to the first distiller 20. When the crude acid in the storage tank 1 is heated by the heating plate 24 and condensed by the condenser 25 in the first distiller 20 in sequence, it falls into the acid receiving tray 23 provided in the first distiller 20.

[0044] The second distiller 21, whose input end is connected to the distillate pipeline of the first distiller 20, enables the condensed acid liquid contained in the acid receiving tray 23 provided in the first distiller 20 to flow to the second distiller 21 for further distillation. A second liquid level sensor 2210 and a second controller 2211 are provided on the side wall of the second distiller. During this period, the input end of the second controller is connected to the second liquid level sensor 2210, and its output end is connected to the heating plate 24 provided in the first distiller 20. After the liquid level signal of the second liquid level sensor 2210 is transmitted to the second controller 2211, the second controller 2211 processes and controls the heating power of the heating plate 24, thus realizing the automatic control of acid liquid distillation. In addition, a temperature probe is provided near the heating plate 24, and the temperature probe is electrically connected to the input end of the second controller 2211. Therefore, in summary, the heating power of the heating plate 24 provided in the first distiller 20 can be jointly controlled through the temperature feedback of the temperature probe and the liquid level feedback of the second liquid level sensor 2210 to avoid the danger caused by overheating of the first distiller 20. When the acid distillate in the first distiller 20 is heated by the heating plate 24 provided in the second distiller 21 and then condensed by the condenser 25, it falls into the acid receiving tray 23 provided in the second distiller 21.

[0045] The crude acid in the liquid storage tank 1 is distilled in a two-stage distillation form, ensuring the continuity of the acid distillation process. During distillation, the purity of the target acid liquid after distillation is adjusted by controlling the feed amount of the crude acid through the liquid level feedback of the first liquid level sensor 2200 and controlling the heating power of the heating plate 24 provided in the first distiller 20 through the liquid level feedback of the second liquid level sensor 2210, so that the target acid liquid can reach the electronic grade purity.

[0046] The filling unit includes a turntable, a dispensing table 33 and dispensing bottles 24. The turntable is connected and communicated with the distillate pipeline of the second distiller 21 through a connecting pipe 37, and a control valve 30 is provided at the distillate pipeline of the second distiller 21. The turntable is provided with a perfusion pipe group, so that the target acid liquid collected by the turntable can be diverted outward by the perfusion pipe group 32. The dispensing bottles 24 are installed on the dispensing table 33, and the installation positions of the dispensing bottles 24 are set to match the perfusion pipe group 32, so that each perfusion pipe can inject the target acid liquid into the dispensing bottles 24.

[0047] The turntable includes a connecting pipe 37, a meshing disc 31, and a power disc 41. One end of the connecting pipe 37 is connected to the distillate pipeline of the second distiller 21, and the other end is installed at the top of the meshing disc 31 and communicates with the meshing disc 31. At the bottom end of the meshing disc 31, a perfusion pipe group 32 communicating with the meshing disc 31 is installed. Preferably, the perfusion pipe group 32 includes two perfusion pipes, and the two perfusion pipes are symmetrically arranged at the bottom end of the meshing disc 31 with the center of the meshing disc 31 as the center, so that the target acid liquid is collected from the connecting pipe 37 to the meshing disc 31 and then diverted outward by the perfusion pipe group 32. The power disc 41 is arranged to be matched and meshed with the meshing disc 31, that is, the meshing disc 31 and the power disc 41 are at the same height. The center of the power disc 41 is externally connected to the movable end of the motor 40, so that the rotation of the power disc 41 is driven by the motor 40 to drive the rotation of the meshing disc 31.

[0048] The dispensing table 33 is arranged below the meshing disc 31. Along the circumference of the top end of the dispensing table 33, a group of mounting frames is evenly spaced. The group of mounting frames preferably has an even number of mounting frames 36. The mounting frames 36 are arranged to match the perfusion pipes, that is, each perfusion pipe is located directly above a mounting frame 36. The dispensing table 33 is equipped with a third controller 351, and the output terminals of the third controller 351 are respectively electrically connected to the motor 40 and the control valve 30.

[0049] The dispensing bottles 34 are fitted and installed on the mounting frames 36, that is, the number of dispensing bottles 34 is equal to the number of mounting frames 36. A third liquid level sensor 350 is installed on the side wall of each dispensing bottle 34, and the third liquid level sensor 350 is electrically connected to the input terminal of the third controller 351. After the signal of the full liquid level of the third liquid level sensor 350 is transmitted to the third controller 351, it is processed by the third controller 351 and then the control valve 30 is closed and the motor 40 rotates in sequence, so that the perfusion pipe can be rotated above the non-filled dispensing bottle 34. When the third liquid level sensor 350 transmits the signal of the empty liquid level to the third controller 351, it is processed by the third controller 351 and the motor 40 is controlled not to rotate, and then the control valve 30 is opened, so as to realize the injection of the perfusion pipe into the dispensing bottle 34.

[0050] When the distillate pipeline of the second distiller 21 sends the target acid liquid through the connecting pipe 37 to the meshing disc 31, the rotation state of the motor 40 and the on-off state of the control valve 30 are correspondingly controlled through the liquid level feedback of the third liquid level sensor 351, so as to realize the automatic filling of the target acid liquid.

[0051] Based on this embodiment, the working principle of the present application is as follows:

[0052] The crude acid in the liquid storage tank 1 is distilled in a two-stage distillation form. During the distillation, the purity of the target acid solution after distillation is adjusted by controlling the feed rate of the crude acid through the liquid level feedback of the first liquid level sensor 2200 and controlling the heating power of the heating plate 24 provided in the first distiller 20 through the liquid level feedback of the second liquid level sensor 2210, so that the target acid solution reaches the electronic grade purity;

[0053] The mounting rack group provided on the dispensing table 33 is provided with corresponding dispensing bottles 34. After the third liquid level sensor 350 transmits a signal indicating that the liquid level is empty to the third controller 351, the third controller 351 processes and controls the motor 40 not to rotate, and then opens the control valve 30 to make the perfusion pipe inject liquid into the dispensing bottle 34. After a group of dispensing bottles 34 are filled, the third liquid level sensor 350 transmits a signal indicating that the liquid level is full to the third controller 351. Then, the third controller 350 processes and controls the control valve 30 to close, and then rotates the motor 40 to the dispensing bottle 34 where the third controller 351 can receive a signal indicating that the liquid level is empty, waiting for the next group of filling. The above process is repeated until all the dispensing bottles 34 are filled with the target acid solution.

[0054] Based on this embodiment, the advantages of the present application are as follows:

[0055] (1) The crude acid in the liquid storage tank 1 is distilled in a two-stage distillation form. During the distillation, the purity of the target acid solution after distillation is adjusted by controlling the feed rate of the crude acid through the liquid level feedback of the first liquid level sensor 2200 and controlling the heating power of the heating plate 24 provided in the first distiller 20 through the liquid level feedback of the second liquid level sensor 2210. While ensuring the continuity of the experiment, the target acid solution can also reach the electronic grade purity;

[0056] (2) By the liquid level feedback of the third liquid level sensor 350 to respectively control the rotation state of the motor 40 and the opening and closing state of the control valve 30, the automatic filling of the target acid solution is realized.

Claims

1. A distillation system for electronic grade analytical acid, characterized in that: The distillation system of the electronic grade analytical acid comprises: The liquid storage tank is provided with a liquid outlet pipeline; the liquid outlet pipeline is provided with a regulating valve and a pump; A multi-stage distillation unit, whose input end is connected to the liquid outlet pipeline, comprises a plurality of distillers connected in series; each distiller is provided with an acid receiving tray for accommodating the condensed acid liquid of the distiller; The filling unit comprises a turntable and a sub-filling bottle; the turntable is connected to the output end of the multi-stage distillation unit through a connecting pipe; the turntable is provided with a filling pipe group; the sub-filling bottle is provided to match the filling pipe group; The condensed acid liquid in an acid receiving plate is sent to the next distiller for further distillation until the target acid liquid flowing out of the output end of the multi-stage distillation unit reaches electronic grade purity and flows to the turntable to be filled into the sub-filling bottle.

2. The distillation system for electronic grade analytical acid according to claim 1, characterized in that: The multi-stage distillation unit includes two first distiller and second distiller connected in series; the input end of the first distiller is connected to the liquid outlet pipeline, and the distillate pipeline arranged on the acid receiving plate is connected to the input end of the second distiller for conveying the condensed acid to the second distiller; the output end of the second distiller is connected to the filling unit.

3. The distillation system for electronic grade analytical acid according to claim 2, characterized in that: A heating plate is provided at the bottom of each distiller, a condenser is provided at the top thereof, and the acid receiving plate is provided between the heating plate and the condenser; a first liquid level sensor and a first controller are provided on the side wall of the first distiller, and a second liquid level sensor and a second controller are provided on the side wall of the second distiller.

4. The distillation system for electronic grade analytical acid according to claim 3, characterized in that: The output end of the first controller is connected to the regulating valve, and the input end thereof is connected to the first liquid level sensor.

5. The distillation system for electronic grade analytical acid according to any one of claims 3 or 4, characterized in that: The second controller provided in the second distiller has an input end connected to the second liquid level sensor, and an output end connected to the heating plate provided in the first distiller.

6. The electronic grade analytical acid distillation system according to claim 1, characterized in that: Each of the distiller is also provided with a waste liquid discharge pipe near the bottom side wall thereof; each of the waste liquid discharge pipe is provided with a liquid discharge valve.

7. The electronic grade analytical acid distillation system according to claim 1, characterized in that: The distillate pipeline of the second distiller is provided with a control valve; The turntable includes a connecting pipe, a meshing disc and a power disc; one end of the connecting pipe is connected to the distillate pipeline of the second distiller, and the other end is installed on the top of the meshing disc and communicated with the meshing disc; a perfusion pipe group communicated with the meshing disc is installed at the bottom of the meshing disc; the power disc is matched and meshed with the meshing disc; the center of the power disc is externally connected to the movable end of the motor.

8. The electronic grade analytical acid distillation system according to claim 7, characterized in that: The filling unit also includes a filling station; the filling station is arranged below the engagement plate; a plurality of mounting rack groups are evenly spaced and installed on the top of the filling station along its circumference; the mounting rack groups are arranged to match the perfusion pipe groups.

9. The electronic grade analytical acid distillation system according to claim 8, characterized in that: The perfusion pipe group has two perfusion pipes, and the two perfusion pipes are arranged opposite to each other on the turntable with the center of the turntable in mind; the number of the mounting frames is an even number.

10. The electronic grade analytical acid distillation system according to claim 8, characterized in that: A third liquid level sensor is provided on the side wall of each of the filling bottles; a third controller is installed on the filling station, the output end of the third controller is respectively connected to the motor and the control valve, and the input end is connected to the third liquid level sensor.

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