A high efficiency purification device for ammonium bifluoride and ammonium fluoride

Abstract

The application discloses a kind of high-efficiency purification device for ammonium bifluoride and ammonium fluoride, including base and cover;The top heating hole is opened in the top surface of base;The side heating hole is also opened in the inner side wall of base, and the side heating hole is arranged obliquely;A PFA tank is inserted in each top heating hole and side heating hole;The cover is covered on the top surface of base, and the top heating hole is completely covered;A plurality of heating rods are inserted in the base;The heating rod is electrically connected with the controller;The PFA tank includes PFA reagent bottle and PFA tee bend.The purification device in the application has high purification efficiency, small floor area and no harsh requirements for working environment.The heating is uniform and stable, safe, efficient, intelligent, convenient to operate, long in service life, low in maintenance cost in later period, and can meet the use requirements of pure ammonium bifluoride and ammonium fluoride in scientific research and teaching.

Description

Technical Field

[0001] This invention relates to the field of geological sample pretreatment technology, and in particular to a highly efficient purification device for ammonium bifluoride and ammonium fluoride. Background Technology

[0002] Geological sample pretreatment technology is the cornerstone for obtaining high-precision geochemical data (elemental content, isotope ratios, and geochronological information). The classic strong acid-base digestion method has been used for nearly a century, but with significant advancements in detection techniques and the rapid development of analytical instruments, current traditional geological sample pretreatment methods lag far behind the rapid advancements in modern analytical detection technologies. They have consistently failed to escape the traditional model of low efficiency, heavy pollution, high risk, large land area requirements, significant waste, and difficult processing, seriously contradicting the modern concept of green development.

[0003] In recent years, the development of ammonium bifluoride and ammonium fluoride digestion technologies has eliminated the constraints of geological sample pretreatment. This technology creates a green, efficient, and safe geological sample digestion process that does not rely on highly toxic reagents such as hydrofluoric acid. It reduces the use of chemical reagents such as acids and alkalis by more than 80%, effectively solving the problems of high pollution associated with traditional geological sample pretreatment techniques. It also avoids safety risks during experimental operations and aligns with modern green development concepts. However, the purity of commercially available ammonium bifluoride and ammonium fluoride reagents currently falls far short of the requirements for geological sample analysis and testing, necessitating the purification of these commercially available chemical reagents.

[0004] Many acid purification devices have been developed both domestically and internationally to address traditional acid digestion methods, such as the Savvillex DST-4000 acid purifier from the United States and the Binhai Zhenghong CH-500ml acid distillation apparatus from China. These purification devices are very expensive, have high maintenance costs, and limited functionality, only suitable for purifying liquid acids, with cumbersome post-treatment cleaning processes. Furthermore, the large-scale distillation and transfer of acid during operation poses certain safety risks.

[0005] In view of this, based on existing research on commonly used inorganic reagent purification technologies and equipment in laboratories, a highly efficient purification device was developed that can not only purify ammonium bifluoride and ammonium fluoride, but also simultaneously purify commonly used laboratory nitric acid, hydrochloric acid, and hydrofluoric acid. This aims to fill the current market gap in the lack of ultrapure ammonium bifluoride and ammonium fluoride purification equipment suitable for scientific research and laboratory use, and to promote the practical application of this novel "green geological sample digestion reagent" in geological experimental testing. Currently, no dedicated equipment for the purification of ammonium bifluoride and ammonium fluoride has been found domestically or internationally. Summary of the Invention

[0006] The purpose of this invention is to provide a highly efficient purification device for ammonium bifluoride and ammonium fluoride, so as to solve the problems existing in the prior art. The device has a small footprint and no harsh requirements on the working environment. It features uniform and stable heating, good safety performance, high efficiency and intelligence, convenient operation, long service life, and low maintenance cost. It can meet the needs of scientific research, teaching and mass production of pure ammonium bifluoride and ammonium fluoride.

[0007] To achieve the above objectives, the present invention provides the following solution: The present invention provides a highly efficient purification device for ammonium bifluoride and ammonium fluoride, comprising a base and a cover; a top heating hole is provided on the top surface of the base; and a side heating hole is also provided on one side wall of the base with an inwardly inclined arrangement.

[0008] Each of the top heating holes and side heating holes is fitted with a PFA reagent bottle; the cap is placed on the top surface of the base and completely covers the top heating hole; several heating rods are also inserted through the base; the heating rods are electrically connected to the controller.

[0009] Furthermore, to better address the issue of easy condensation and crystallization clogging the channel at the bend, the device of this invention employs a graded three-channel system and a heating method with the bend wrapped around it. A corrosion-resistant Teflon coating is sprayed onto the surface of the graphite heating element. When ammonium bifluoride or ammonium fluoride reagent to be purified is placed in the middle reagent bottle and heated through the top heating hole, the vapor of the reagent rises and flows through the wrapped and heated PFA tee bend to the PFA reagent bottles on both sides. It condenses and crystallizes at the lower temperature at the mouth of the PFA reagent bottle and is collected at the bottom, improving purification efficiency. When the reagent to be purified is placed in the outer reagent bottle and heated through the side heating hole, the vapor of the reagent rises and flows through the wrapped and heated PFA tee bend. Most of it first condenses and crystallizes in the middle PFA reagent bottle and is collected at the bottom.

[0010] Because the middle PFA reagent bottle is located next to the graphite heating element, it is heated simultaneously with the bent tube, creating secondary heating. The vapor rises again and flows back to the bent tube, passing through the cooler outer PFA reagent bottle. After condensation and crystallization at the bottle mouth, it is collected at the bottom. After purification and cooling, the middle PFA collection bottle yields the first-stage high-purity ammonium bifluoride and ammonium fluoride reagents in powder form; the outer PFA collection bottle yields the second-stage ultrapure reagent after secondary purification, in slender needle-like form, which can be used for digesting special samples with low content and high blank requirements.

[0011] The PFA reagent bottle and the PFA tee elbow; each of the PFA tee elbows is equipped with three of the PFA reagent bottles, and one of the PFA reagent bottles contains ammonium bifluoride reagent or ammonium fluoride reagent.

[0012] Furthermore, high-purity ammonium bifluoride and ammonium fluoride, due to their superior digestion capabilities, extremely short digestion time, extremely low background, non-precipitation of fluoride compounds, and superior operational safety compared to hydrofluoric acid, have become a novel "green geological sample digestion reagent." This technology significantly improves the efficiency and data quality of geological sample analysis, representing a significant innovation in the field of green geological experimental testing technology. However, ultrapure ammonium bifluoride and ammonium fluoride, the main digestion reagents in this technology, are currently difficult to obtain commercially. Currently, the purity of domestically produced industrial-grade ammonium bifluoride is 98%, and the purity of analytical-grade ammonium bifluoride is 99.8%. This purity is too low to meet the requirements for trace element analysis. The highest purity domestic brand available on the market is Aladdin, whose ammonium bifluoride purity is 99.9975%. While the background values ​​for some elements meet the needs of trace element analysis, the content of impurities such as metal ions Li, Be, Cr, Co, Ni, Cu, Zn, Rb, Zr, Nb, Ba, As, and Pb is still relatively high compared to trace sample analysis. The Cr background value reaches 23 ng g⁻¹, 100 times higher than the background value of the conventional HF+HNO₃ method, and the Ni background value reaches 7.8 ng g⁻¹, 1977 times higher, far exceeding the conventional dissolution method. This cannot meet the requirements for high-precision trace element and isotope analysis of geological samples, necessitating the purification of both ammonium bifluoride and ammonium fluoride. Taking the purification of ammonium bifluoride as an example, let's first understand the physicochemical properties of ammonium bifluoride. Ammonium fluoride, also known as acidic ammonium fluoride, diammonium fluoride, or ammonium fluoride, has the molecular formula NH4HF2. It is a white or colorless transparent orthorhombic crystal, occurring in flaky form, with a slightly acidic odor. Its relative density is 1.52, melting point is 125.6℃, and boiling point is 240℃. It is hygroscopic in air, slightly soluble in alcohol, and readily soluble in cold water. It can be used as a sample digestion reagent and as a surface treatment agent, etching agent, disinfectant, and preservative in the high-precision electronics and pharmaceutical industries.

[0013] The cumbersome pretreatment process has long been a bottleneck to the rapid development of geological sample analysis. Digestion methods (open-system acid digestion, closed-system high-pressure digestion, alkali fusion) and the selection of digestion reagents (HF+HNO3, HF+HNO3+HCl, HF+HNO3+HClO4, HF+aqua regia+HClO4, and HF+HClO4) have remained largely unchanged for nearly 20 years. For samples rich in sparingly soluble accessory minerals (zircon), complete digestion requires more than 24 hours of closed digestion time.

[0014] In the field of Earth science research, with the specialization, deepening, and refinement of scientific questions, the detection limits for trace and ultra-trace element determination in geological samples have reached the ppt level, with linear dynamic ranges accurate to 10¹². However, it is worth noting that the laboratory environment and reagent selection have a significant impact on the final test results. In inorganic analysis, water and reagent purification preparation is crucial. The lower the content of the analyte, the higher the method sensitivity, and the higher the purity requirement for the reagents; the higher the accuracy requirement for the determination results, the higher the purity requirement for the reagents. In the blank values ​​of commercially available unpurified ammonium bifluoride, some elements show high background values ​​(Table 1), especially Cr and Ni, with Cr background values ​​reaching 23.23 ngg⁻¹ and Ni background values ​​reaching 7.8 ngg⁻¹, which cannot meet the requirements for trace element analysis of rock samples. Due to the physicochemical properties of ammonium bifluoride and ammonium fluoride, conventional laboratory quartz subboiling distillers and Savvillex DTS self-condensing purifiers cannot purify them.

[0015] In existing technology, the Savvillex flask subboiling distillation apparatus consists of two PFA flasks connected by a right-angle bend in the PFA tube. The ammonium bifluoride and ammonium fluoride reagents to be purified are poured into one of the PFA flasks. By adjusting the distance and angle of the infrared lamp, the temperature of the PFA flask containing the ammonium bifluoride and ammonium fluoride is maintained at 170°C. At this temperature, the ammonium bifluoride and ammonium fluoride melt into liquids (ammonium bifluoride melting point 125.6°C), slowly evaporate, and then condense and crystallize in the other PFA flask.

[0016] Because infrared lamp heating requires adjusting the distance and angle between the infrared lamp and the paired bottles and the bend, and the uncontrollable surrounding environment and human operation can affect the final purification effect, the process is challenging. During heating, due to the diameter, material, and thickness of the bend, there will be temperature loss in the internal channels. The temperature at the bend must be sufficiently high and uniform (170℃-200℃). Otherwise, if the temperature is too low, the condensed ammonium bifluoride and ammonium fluoride will easily crystallize and solidify at the bend, clogging the channels and eventually accumulating at the bend opening, making purification impossible. It is necessary to repeatedly turn off the infrared lamp, wait for the PFA bottle to cool, unscrew the bend, collect the condensed crystals, and gently tap and vibrate the bend to loosen and clean it before further purification can proceed. Using this paired-bottle sub-boiling distillation apparatus, the purification efficiency of ammonium bifluoride and ammonium fluoride is very low, and the operation is complex and subject to chance. Purifying approximately 50 grams of ammonium bifluoride and ammonium fluoride to meet sample pretreatment requirements takes about 2-3 days, and the low yield is insufficient to support large-scale sample analysis reagent consumption. In addition, ammonium bifluoride and ammonium fluoride are very hygroscopic and decompose into toxic fluorides. Purification using this device requires operators to frequently open the bottles, which poses certain safety hazards. Moreover, the workload of cleaning the equipment and treating the waste liquid when purifying ammonium bifluoride and ammonium fluoride using this method is also very large.

[0017] Experiments showed that adding 150g of ammonium bifluoride reagent to be purified to a reagent bottle in a Savvillex flask sub-boiling distillation apparatus and heating at 170°C for 12 hours yielded 5-10g of high-purity ammonium bifluoride reagent. The apparatus of this invention, by adding 300g of ammonium bifluoride reagent to one reagent bottle and heating at 230°C for 4 hours, yielded 50g of high-purity ammonium bifluoride reagent. If reagent is added to five reagent bottles simultaneously for purification, the purification efficiency of the apparatus of this invention is increased by 75 times compared to the Savvillex flask sub-boiling distillation apparatus.

[0018] Both the base and the cover are made of graphite.

[0019] The PFA tee elbow has a PFA reagent bottle installed at each of its two ends and in the middle.

[0020] A PFA reagent bottle is installed inside the top heating hole, and the PFA reagent bottle contains ammonium bifluoride reagent or ammonium fluoride reagent; the PFA reagent bottle is installed in the central connecting channel of the PFA tee elbow, and two empty PFA reagent bottles are respectively installed in the connecting channels on both sides of the PFA tee elbow.

[0021] The bottom surface of the cover is provided with an elbow heating hole; the elbow heating hole is used to heat the PFA tee elbow installed above the top heating hole.

[0022] The top heating holes and side heating holes are arranged alternately; a PFA reagent bottle is inserted into the side heating hole, and the PFA reagent bottle contains ammonium bifluoride reagent or ammonium fluoride reagent; the PFA reagent bottle is installed in the connecting channel on either side of the PFA tee elbow, and empty PFA reagent bottles are installed in the connecting channel on the other side and the central channel of the PFA tee elbow.

[0023] Each of the side heating holes is also equipped with an elbow heating plate; one side of the cover extends outward from the bottom to form an elbow heating block adapted to the elbow heating plate; the elbow heating plate is used to heat the PFA tee elbow installed on the protruding part of the side heating hole to prevent the condensing reagent from crystallizing and blocking the connecting channel.

[0024] The side heating hole is tilted at an angle of 44-46 degrees to the ground.

[0025] The heating rod is arranged around the top heating hole and the side heating hole.

[0026] The base surface is coated with a Teflon coating.

[0027] The present invention discloses the following technical effects: the purification device of the present invention has high purification efficiency, small footprint and no harsh requirements on the working environment, uniform and stable heating, good safety performance, high efficiency and intelligence, convenient operation, long service life and low maintenance cost, and can meet the needs of pure ammonium bifluoride and ammonium fluoride for scientific research and teaching. Attached Figure Description

[0028] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0029] Figure 1 This is a schematic diagram of the overall structure of the present invention;

[0030] Figure 2 This is a schematic diagram of the structure of the cover of the present invention;

[0031] Figure 3 This is a schematic diagram of the base of the present invention;

[0032] Figure 4 This is a structural perspective view of the base of the present invention;

[0033] Figure 5 This is a perspective view of the PFA tee elbow of the present invention;

[0034] Figure 6 This is a schematic diagram of the structure of the PFA reagent bottle of the present invention;

[0035] The components include: 1. base; 2. cover; 3. heating rod; 4. PFA tee elbow; 5. PFA reagent bottle; 6. controller; 7. elbow heating hole; 8. elbow heating block; 9. side heating hole; 10. elbow heating plate; and 11. top heating hole. Detailed Implementation

[0036] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0037] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0038] The present invention provides a highly efficient purification device for ammonium bifluoride and ammonium fluoride, including a base 1 and a cover 2; a top heating hole 11 is provided on the top surface of the base 1; a side heating hole 9 is also provided inwardly on one side wall of the base 1.

[0039] Each top heating hole 11 and side heating hole 9 is fitted with a PFA canister; the cover 2 is placed on the top surface of the base 1 and completely covers the top heating hole 11; several heating rods 3 are also inserted through the base 1; the heating rods 3 are electrically connected to the controller 6.

[0040] The PFA container includes a PFA reagent bottle 5 and a PFA tee elbow 4; each PFA tee elbow 4 is equipped with three PFA reagent bottles 5, and one of the PFA reagent bottles 5 contains ammonium bifluoride reagent or ammonium fluoride reagent.

[0041] Both the base 1 and the cover 2 are made of graphite.

[0042] A PFA reagent bottle 5 is installed at each end and in the middle of the PFA tee elbow 4;

[0043] A PFA reagent bottle 5 is installed inside the top heating hole 11, and the PFA reagent bottle 5 contains ammonium bifluoride reagent or ammonium fluoride reagent; the PFA reagent bottle 5 is installed in the central connecting channel of the PFA tee elbow 4, and two empty PFA reagent bottles 5 are installed in the connecting channels on both sides of the PFA tee elbow 4 respectively.

[0044] The bottom surface of the cover 2 is provided with an elbow heating hole 7; the elbow heating hole 7 is used to heat the PFA tee elbow 4 installed above the top heating hole 11.

[0045] The top heating hole 11 and the side heating hole 9 are arranged alternately; a PFA reagent bottle 5 is inserted into the side heating hole 9, and the PFA reagent bottle 5 contains ammonium bifluoride reagent or ammonium fluoride reagent to be purified; the PFA reagent bottle 5 is installed in the connecting channel on either side of the PFA tee elbow 4, and empty PFA reagent bottles 5 are installed in the connecting channel on the other side and the central channel of the PFA tee elbow 4 respectively.

[0046] Each side heating hole 9 is also equipped with an elbow heating plate 10; one side bottom of the cover 2 extends outward to form an elbow heating block 8 that is adapted to the elbow heating plate 10; the elbow heating plate 10 is used to heat the PFA tee elbow 4 installed in the protruding part of the side heating hole 9 to prevent the condensed reagent crystallization from blocking the connecting channel.

[0047] The side heating hole 9 is tilted at an angle of 44-46 degrees to the ground.

[0048] Heating rod 3 is arranged around the top heating hole 11 and the side heating hole 9.

[0049] The surface of base 1 is coated with Teflon.

[0050] In one embodiment of the present invention, the base 1 is coated with a Teflon coating to make it corrosion-resistant, oxidation-resistant, and have a longer service life. Its top has two vertical top heating holes 11, and its front has three side heating holes 9 at a 45° angle, with a bent heating plate 10 at each station. This prevents condensation at the top of the PFA tee bend 4 from causing channel blockage during heating and purification. Finally, it forms a highly efficient purification device with five stations and ten reagent purification collection bottles. The base 1 has four 800W heating rods 3 on its side, with a total power of 3200W, which can uniformly reach a maximum temperature of 300 degrees Celsius in all parts within 15 minutes.

[0051] The cover 2, placed on top of the base 1, is also made of highly thermally conductive graphite material. Through heat conduction from the base 1, it heats the PFA tee elbow 4 via two elbow heating holes 7 and three elbow heating blocks 8, preventing excessive condensation at the top of the PFA tee elbow 4 from causing channel blockage. The PFA tee elbow 4 is made of high-purity Teflon, with each adjacent channel having a 45° angle. The threads at the channel openings match the threads of the PFA reagent bottle 5, and a beveled sealing groove is provided at the root of the threads to prevent overflow and leakage. The purification device is timed and heated for purification via the controller 6, and automatically shuts down after completion.

[0052] Furthermore, this device can purify not only ammonium bifluoride and ammonium fluoride, but also commonly used laboratory chemical reagents such as nitric acid, hydrochloric acid, and hydrofluoric acid. Compared to traditional purification devices and methods, this new multifunctional purification device offers advantages such as safety, high efficiency, ease of operation, low cost, small footprint, and no stringent requirements for the working environment.

[0053] After purification using the apparatus of this invention, the background values ​​of elements such as V, Cr, Co, Ni, Cu, Rb, Sr, and Ba detected on the machine reached the level of conventional high-pressure closed digestion methods. In particular, the background values ​​of Cr and Ni decreased significantly: Cr decreased from 23.23 ngg⁻¹ to 0.482 ngg⁻¹, a reduction of 48 times; Ni decreased from 7.847 ngg⁻¹ to 0.103 ngg⁻¹, a reduction of 76 times (Table 1). Furthermore, the apparatus of this invention is highly efficient, has no stringent requirements for the working environment, provides uniform and stable heating, has good safety performance, is easy to operate, highly efficient and intelligent, has a long service life, and low maintenance costs. It can meet the needs of scientific research, teaching, and mass production of pure ammonium bifluoride and ammonium fluoride.

[0054] Table 1. Blank values ​​of ammonium bifluoride before and after purification using the apparatus of the present invention.

[0055]

[0056] In a specific embodiment 1 of the present invention, 400g of ammonium bifluoride reagent to be purified is added to each of five PFA reagent bottles 5. Two of the PFA reagent bottles 5 containing reagent are installed and tightened into the middle PFA threaded channel of the PFA tee elbow 4. The empty PFA reagent bottles 5 are installed and tightened into the two side channels of the PFA tee elbow 4. The two sets of installed PFA reagent bottles 5 containing ammonium bifluoride reagent are placed into the two top heating holes 11 of the graphite base 1. The three empty PFA reagent bottles 5 containing ammonium bifluoride reagent to be purified are then placed into the two top heating holes 11 of the graphite base 1. The PFA reagent bottle 5 containing ammonium bifluoride reagent is installed and tightened with one of the PFA threaded tees on the side of the PFA tee elbow. The empty PFA reagent bottle 5 is installed and tightened with the other two channels of the PFA tee elbow 4. The three sets of PFA reagent bottles 5 containing ammonium bifluoride reagent are placed into the side heating holes 9 of the graphite base 1. Then the cap 2 is installed with the base 1, so that the elbow heating hole 7 and the elbow heating plate 10 heat the PFA tee elbow 4 to prevent the condensed ammonium bifluoride reagent from solidifying and crystallizing and blocking the channels. The controller 6 was set to a temperature of 200 degrees Celsius and a heating time of 6 hours. After purification, 400g of high-purity ammonium bifluoride reagent in powder form was obtained from the PFA reagent bottles 5 on both sides of the two sets of four top heating holes 11. 450g of first-stage high-purity ammonium bifluoride reagent was obtained from the six PFA reagent bottles 5 corresponding to the three sets of side heating holes 9 and the three middle PFA reagent bottles 5. 150g of second-stage ultra-pure ammonium bifluoride reagent in fine needle form with higher purity was obtained from the three adjacent outer PFA reagent bottles 5 after secondary purification.

[0057] In Embodiment 2 of the present invention, 400g of ammonium fluoride reagent to be purified is added to each of the five PFA reagent bottles 5. Two of the PFA reagent bottles 5 containing reagent are installed and tightened into the middle PFA threaded channel of the PFA tee elbow 4. The empty PFA reagent bottles 5 are installed and tightened into the two side channels of the PFA tee elbow 4. The two sets of installed PFA reagent bottles 5 containing ammonium fluoride reagent are placed into the two top heating holes 11 of the graphite base 1. Three of the empty PFA reagent bottles 5 containing ammonium fluoride reagent are then placed into the two top heating holes 11 of the graphite base 1. The PFA reagent bottle 5 is installed and tightened with one of the PFA threaded tees on the side of the PFA tee elbow. The empty PFA reagent bottle 5 is installed and tightened with the other two channels of the PFA tee elbow 4. The three sets of PFA reagent bottles 5 containing ammonium fluoride reagent are placed into the side heating holes 9 of the graphite base 1. Then the cap 2 is installed with the base 1, so that the elbow heating hole 7 and the elbow heating plate 10 heat the PFA tee elbow 4 to prevent the condensed ammonium fluoride reagent from solidifying and crystallizing and blocking the channels. With controller 6 set to 230 degrees Celsius and heating time set to 4 hours, after purification, 400g of high-purity ammonium fluoride reagent in powder form was obtained from the PFA reagent bottles 5 on both sides of the two sets of four top heating holes 11. 450g of first-stage high-purity ammonium fluoride reagent was obtained from the six PFA reagent bottles 5 corresponding to the three sets of side heating holes 9, and 150g of second-stage ultra-pure ammonium fluoride reagent in slender needle-like form after secondary purification from the three adjacent outer PFA reagent bottles 5.

[0058] In the description of this invention, it should be understood that the terms "longitudinal", "lateral", "up", "down", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this invention, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this invention.

[0059] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims

1. A high efficient purification device for ammonium bifluoride and ammonium fluoride, characterized in that, Include: Base (1) and cover (2); the top of the base (1) is provided with a top heating hole (11); one side wall of the base (1) is also provided with an inwardly inclined side heating hole (9); Each of the top heating hole (11) and side heating hole (9) is inserted with a PFA tank; the cover (2) is covered on the top of the base (1), and the top heating hole (11) is completely covered; a plurality of heating rods (3) are also inserted into the base (1); the heating rod (3) is electrically connected with the controller (6); The PFA tank includes a PFA reagent bottle (5) and a PFA three-way elbow (4); each of the PFA three-way elbow (4) is provided with three PFA reagent bottles (5), and one of the PFA reagent bottles (5) is placed with ammonium bifluoride reagent or ammonium fluoride reagent; The bottom of the cover (2) is provided with an elbow heating hole (7) upward; the elbow heating hole (7) is used for heating the PFA three-way elbow (4) installed above the top heating hole (11); The top heating hole (11) and side heating hole (9) are staggered; one of the PFA reagent bottles (5) is inserted into the side heating hole (9), and the PFA reagent bottle (5) is placed with ammonium bifluoride reagent or ammonium fluoride reagent; the PFA reagent bottle (5) is installed in the communication channel on either side of the PFA three-way elbow (4), and the other side communication channel and the center channel of the PFA three-way elbow (4) are respectively provided with empty PFA reagent bottles (5); Each of the side heating hole (9) is also provided with an elbow heating piece (10) at the hole opening; the bottom of one side of the cover (2) extends outward to form an elbow heating block (8) matched with the elbow heating piece (10); the elbow heating piece (10) is used for heating the PFA three-way elbow (4) installed on the protruding part of the side heating hole (9), preventing the condensate from blocking the communication channel.

2. A highly efficient purification device for ammonium bifluoride and ammonium fluoride according to claim 1, characterized in that: The base (1) and cover (2) are both graphite materials.

3. A highly efficient purification device for ammonium bifluoride and ammonium fluoride according to claim 1, characterized in that: The PFA three-way elbow (4) is provided with a PFA reagent bottle (5) at both ends and the middle part; The PFA reagent bottle (5) is installed in the top heating hole (11), and the PFA reagent bottle (5) is placed with ammonium bifluoride reagent or ammonium fluoride reagent; the PFA reagent bottle (5) is installed in the center communication channel of the PFA three-way elbow (4), and two empty PFA reagent bottles (5) are respectively installed in the two side communication channels of the PFA three-way elbow (4).

4. A highly efficient purification device for ammonium bifluoride and ammonium fluoride according to claim 1, characterized in that: The angle of the side heating hole (9) to the ground is 44-46 degrees.

5. A highly efficient purification device for ammonium bifluoride and ammonium fluoride as claimed in claim 1, wherein: The heating rod (3) surrounds the top heating hole (11) and side heating hole (9).

6. A highly efficient purification device for ammonium bifluoride and ammonium fluoride as claimed in claim 1, wherein: The surface of the base (1) is sprayed with a Teflon coating.

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