CN113358436A - Device and method for purifying ammonium bifluoride - Google Patents
Device and method for purifying ammonium bifluoride Download PDFInfo
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Abstract
The present disclosure provides a device and a method for purifying ammonium bifluoride, comprising: the heating bottle is used for placing ammonium bifluoride to be purified; the heating jacket is at least partially positioned in the heating bottle, so that the heating jacket carries out sub-boiling distillation on the ammonium bifluoride to be purified in the heating bottle; the condensation bottle is positioned outside the heating sleeve; the two ends of the connecting elbow are respectively communicated with the heating bottle and the condensing bottle, the part of the connecting elbow connected with the heating bottle is provided with an ascending section, and the part of the connecting elbow connected with the condensing bottle is provided with a descending section, so that the ammonium bifluoride subjected to sub-boiling distillation in the heating bottle flows into the condensing bottle through the ascending section and the descending section. The ammonium bifluoride purification device disclosed by the invention is simple in structure, simple to operate, low in cost and easy to obtain the ultrahigh-purity ammonium bifluoride.
Description
Technical Field
The disclosure relates to the technical field of chemical analysis, in particular to a device and a method for purifying ammonium bifluoride.
Background
The ammonium bifluoride has strong corrosivity and strong acidity, and can be used as a digestion reagent and a surface treating agent to be applied to a geological sample digestion agent, a surface treating agent in high-end electronic industry and the like. For example, when a geological sample is used for determining the content of trace elements and the isotope ratio, the geological sample needs to be digested by a chemical treatment method, and a solid geological sample is converted into a solution sample which can be tested. Ammonium bifluoride digestion geological sample is a novel chemical sample dissolving method developed in the last decade, can digest indissolvable minerals in the geological sample at higher temperature, is low in cost, is simple and quick to operate, and can more efficiently and accurately obtain the trace element content and isotope ratio of the geological sample such as rock, sediment or soil.
Currently, the commonly used reagent of ammonium bifluoride superior purity (98%) and analytical purity (99.8%) usually contains mg.g-1Metal ion impurities (such as Li, V, Cr, Mn, Cu, Zn, Sr, Zr, Ba, Nd, Pb, and the like) in grades or higher, which seriously affect the accurate determination of these low-content trace elements and isotope ratios in geological samples, sometimes even make the test impossible. The purity of the commercially available ammonium bifluoride is up to 99.99%, the price is high (about 80 yuan for 25 g), and the requirement of accurately testing the geological sample with the ultra-low trace element content cannot be met due to the fact that the content of impurities such as metal ions is still high. Therefore, the problem to be solved is to obtain the ultra-high purity ammonium bifluoride.
The common purification method of ammonium bifluoride is sub-boiling distillation, wherein impure ammonium bifluoride powder is heated to a temperature close to the boiling point (160-240 ℃), and then ammonium bifluoride vapor is cooled to obtain purified crystals. Chinese patent (publication No. CN 103566606B) discloses a purification method of ammonium bifluoride, which comprises the steps of adding ammonium bifluoride powder into a self-made purification device, raising the temperature to 180-200 ℃ for sub-boiling distillation, and crystallizing in a condensation pipe to obtain purified ammonium bifluoride crystals. The purification device has a relatively complex composition structure, and because the crystallization temperature of the ammonium bifluoride is high (the melting point is 125 ℃), the ammonium bifluoride vapor is easy to crystallize locally in a transmission pipeline inside the purification device, even blocks the pipeline, influences the purification efficiency and is difficult to clean. Chinese patent (application publication No. CN 112090106a) discloses a method for purifying ammonium bifluoride, which obtains purified ammonium bifluoride by vertically raising the temperature of the whole bottle and then lowering the temperature step by step, and because the inside of the collection bottle is divided into three layers by PTFE baffles, the ammonium bifluoride after crystallization has higher hardness and is more difficult to collect and clean. The purification equipment used by the two methods is self-developed, has no large-scale commercialization all the time, and cannot meet the requirement of large-scale use at present.
Disclosure of Invention
Technical problem to be solved
In order to solve the problems, the disclosure provides a device and a method for purifying ammonium bifluoride, which are used for at least partially solving the technical problems that the traditional purifying device is complex in structure, ammonium bifluoride crystals easily block pipelines and the like.
(II) technical scheme
The present disclosure provides an ammonium bifluoride purification apparatus, including: the heating bottle is used for placing ammonium bifluoride to be purified; the heating jacket is at least partially positioned in the heating bottle, so that the heating jacket carries out sub-boiling distillation on the ammonium bifluoride to be purified in the heating bottle; the condensation bottle is positioned outside the heating sleeve; the two ends of the connecting elbow are respectively communicated with the heating bottle and the condensing bottle, the part of the connecting elbow connected with the heating bottle is provided with an ascending section, and the part of the connecting elbow connected with the condensing bottle is provided with a descending section, so that the ammonium bifluoride subjected to sub-boiling distillation in the heating bottle flows into the condensing bottle through the ascending section and the descending section.
Furthermore, the connecting elbow is provided with an exhaust hole, and the exhaust hole is provided with an exhaust valve.
Furthermore, the heating bottle and the condensing bottle are meltable polytetrafluoroethylene wide-mouth bottles, and the inner diameters of bottle mouths of the wide-mouth bottles are larger than 4 cm.
Furthermore, the connecting elbow is made of polytetrafluoroethylene, and the connecting elbow is respectively connected with the heating bottle and the condensing bottle through threads.
Furthermore, the heating bottle and the heating sleeve are inclined by 30-60 degrees.
Further, the initial purity of the ammonium acid fluoride to be purified is not less than 98%.
Further, the initial purity of the ammonium bifluoride to be purified is not less than 99.99%.
In another aspect of the present disclosure, there is provided a method for purifying ammonium bifluoride by using the purification apparatus for ammonium bifluoride as described above, including: putting ammonium bifluoride to be purified into a heating bottle; the condensing bottle and the heating bottle are connected through a connecting elbow; placing the heating bottle at least partially in the heating jacket with the condensation bottle outside the heating jacket; the ammonium bifluoride is subjected to sub-boiling distillation through the heating sleeve, and the sub-boiling distilled ammonium bifluoride flows into a condensation bottle through a connecting elbow and is condensed and crystallized to obtain purified ammonium bifluoride.
Further, the sub-boiling distillation of ammonium acid fluoride by means of a heating jacket comprises: heating the temperature in the heating sleeve to 100 ℃ for about half an hour to discharge water through the exhaust holes on the connecting elbow; continuously heating to 200-220 ℃, and carrying out sub-boiling distillation on the ammonium bifluoride.
Further, the flowing of the ammonium bifluoride into the condensation bottle through the connecting elbow and the condensation crystallization comprises the following steps: the rate of condensation crystallization of ammonium bifluoride is about 20 g/hr.
(III) advantageous effects
According to the purification device and method for ammonium bifluoride provided by the embodiment of the disclosure, the ammonium bifluoride is purified by adopting a bottle distillation mode, the device is simple in structure and low in cost, and an interface is not easy to be blocked by the ammonium bifluoride; further, through set up the exhaust hole on connecting the elbow, it makes the ammonium bifluoride crystal granularity who obtains even to eliminate moisture earlier, has avoided the ammonium bifluoride crystal to form the hard piece, is favorable to taking out of ammonium bifluoride after the purification process.
Drawings
FIG. 1 schematically illustrates a schematic structural view of an apparatus for purifying ammonium acid fluoride according to an embodiment of the present disclosure;
FIG. 2 schematically illustrates a flow diagram of a method for purifying ammonium acid fluoride by an ammonium acid fluoride purification apparatus according to an embodiment of the present disclosure;
FIG. 3 is a schematic diagram showing a comparison of metal ion content in an analytical pure ammonium acid fluoride reagent and a purified ammonium acid fluoride according to an embodiment of the present disclosure;
description of reference numerals:
1-PFA bottle 12-PFA bottle 2
3-elbow connection 4-heating jacket
5-exhaust port.
Detailed Description
For the purpose of promoting a better understanding of the objects, aspects and advantages of the present disclosure, reference is made to the following detailed description taken in conjunction with the accompanying drawings.
The invention discloses a device and a method for purifying ammonium bifluoride, in particular to a device and a method for purifying ultra-high-purity ammonium bifluoride from a low-purity particle crude product.
An embodiment of the present disclosure provides an apparatus for purifying ammonium bifluoride, referring to fig. 1, including: the heating bottle 1 is used for placing ammonium bifluoride to be purified; a heating jacket 4, in which the heating bottle is at least partially positioned, so that the heating jacket performs sub-boiling distillation on the ammonium bifluoride to be purified in the heating bottle; the condensation bottle 2 is positioned outside the heating jacket; and the two ends of the connecting elbow 3 are respectively communicated with the heating bottle and the condensing bottle, the part of the connecting elbow connected with the heating bottle is provided with an ascending section, and the part of the connecting elbow connected with the condensing bottle is provided with a descending section, so that the ammonium bifluoride subjected to sub-boiling distillation in the heating bottle flows into the condensing bottle through the ascending section and the descending section.
This ammonium bifluoride purification device includes one to the bottle, including heating bottle 1, condensation bottle 2, and heating bottle 1 is placed in heating jacket 4, and heating jacket 4 carries out the sub-boiling distillation to the ammonium bifluoride in the heating bottle 1, and ammonium bifluoride steam circulates to condensation bottle 2 through connecting elbow 3 to the condensation crystallization in condensation bottle 2. Here, the portion of the connecting elbow 3 connected to the heating bottle 1 is an ascending portion, and the portion connected to the condensing bottle 2 is a descending portion, so that the vapor is condensed and deposited on the bottom of the condensing bottle 2 through the connecting elbow 3. The heating bottle can be arranged in the heating jacket mostly or completely, so as to avoid the crystallization of the ammonium bifluoride on the upper part of the heating bottle. The device has simple structure and low cost, is not easy to be blocked by ammonium bifluoride, and is easy to obtain the ammonium bifluoride with ultra-high purity.
On the basis of the embodiment, the connecting elbow is provided with the exhaust hole, and the exhaust hole is provided with the exhaust valve.
Please continue to refer to fig. 1, a vent hole 5 is disposed at a position of the connecting elbow 3 opposite to the heating bottle 1, and a vent valve (not shown) is further disposed on the vent hole 5, because the ammonium bifluoride powder to be purified usually contains a certain amount of moisture, the presence of the moisture after purification can make the ammonium bifluoride to be hard and hard, and is not easy to take out, therefore, before the ammonium bifluoride is subjected to sub-boiling distillation, the water vapor is firstly discharged through the vent hole 5 at 100 ℃, which is beneficial to obtaining ammonium bifluoride crystals with uniform particles, and is convenient to take out and use.
On the basis of the embodiment, the heating bottle and the condensation bottle are meltable polytetrafluoroethylene wide-mouth bottles, and the inner diameters of the mouths of the wide-mouth bottles are larger than 4 cm.
The heating bottle and the condensing bottle adopt a meltable Polytetrafluoroethylene (PFA) wide-mouth bottle, have good chemical resistance and can play a role in corrosion prevention. The inner diameter of the bottle mouth of the wide-mouth bottle is larger than 4 cm, so that the blockage of the interface by ammonium bifluoride crystallization can be avoided.
On the basis of the above embodiment, the connecting elbow is made of Polytetrafluoroethylene (PTFE), and the connecting elbow is connected with the heating bottle and the condensation bottle respectively through threads.
The polytetrafluoroethylene elbow has excellent corrosion resistance, high flexibility and long service life. The connecting elbow 3 is simple to connect with the heating bottle 1 and the condensing bottle 2, and can be connected or taken down by rotation through threaded connection.
On the basis of the embodiment, the heating bottle and the heating sleeve are inclined by 30-60 degrees.
The connecting elbow 3 is 90 ℃, the heating bottle and the heating sleeve are inclined for 30-60 degrees, and ammonium bifluoride steam is beneficial to rising by being heated firstly through the connecting elbow 3 and then falling and crystallizing at the bottom of the condensing bottle 2 when meeting cold.
On the basis of the above examples, the initial purity of the ammonium acid fluoride to be purified was not less than 98%.
The reagent usually has a purity of 98% and usually contains mg.g-1Metal ion impurities (such as Li, V, Cr, Mn, Cu, Zn, Sr, Zr, Ba, Nd, Pb) of grade or higher, which seriously affect geological samplesThe accurate determination of these low trace element and isotope ratios in medium to medium amounts sometimes even fails to perform the test. The analytically pure ammonium bifluoride can be directly purified by accurate testing.
On the basis of the above examples, the initial purity of the ammonium acid fluoride to be purified was not less than 99.99%.
And the reagent with analytical purity (99.8%) can be directly purified to obtain the ammonium bifluoride with ultra-high purity.
Another embodiment of the present disclosure provides a method for purifying ammonium bifluoride by using the aforementioned purification apparatus for ammonium bifluoride, referring to fig. 2, including: putting ammonium bifluoride to be purified into a heating bottle; the condensing bottle and the heating bottle are connected through a connecting elbow; placing the heating bottle at least partially in the heating jacket with the condensation bottle outside the heating jacket; the ammonium bifluoride is subjected to sub-boiling distillation through the heating sleeve, and the sub-boiling distilled ammonium bifluoride flows into a condensation bottle through a connecting elbow and is condensed and crystallized to obtain purified ammonium bifluoride.
S1, adding ammonium bifluoride powder into a PFA bottle 1;
s2, the PTFE connecting elbow 3 is 90 ℃, one end is connected with the PFA bottle 1, the other end is connected with the PFA reagent bottle 2, and the PFA bottle 2 is placed at room temperature (as shown in figure 1).
S3, putting the PFA bottle 1 into a heating sleeve in an inclined way at 45 degrees;
s4, heating the heating jacket 4 to 200-220 ℃. Ammonium bifluoride is distilled in a heating jacket 4 in a sub-boiling state in a PFA bottle 1, and vapor enters a PFA bottle 2 through a PTFE elbow 3 to be condensed and crystallized into white solid ammonium bifluoride crystals. And (4) turning off the power supply, cooling the heating jacket 4, and taking out the PFA bottle 2 to obtain purified ammonium bifluoride.
The PFA bottle 1, the PFA bottle 2 and the PTFE connecting elbow 3 are made of high-temperature resistant PFA and PTFE respectively, and the inner through hole diameter is larger than 4 cm. The PTFE connecting elbow 3 is connected to the PFA bottle 1 and the PFA bottle 2 by a screw.
In addition to the above examples, the sub-boiling distillation of ammonium acid fluoride by means of a heating jacket comprises: heating the temperature in the heating sleeve to 100 ℃ for about half an hour to discharge water through the exhaust holes on the connecting elbow; continuously heating to 200-220 ℃, and carrying out sub-boiling distillation on the ammonium bifluoride.
The connecting elbow 3 is provided with an exhaust hole 5, an exhaust valve is arranged, and water vapor is easy to remove. Before S4, the temperature of the heating jacket 4 was increased to 100 ℃ to discharge the water in the ammonium acid fluoride powder.
On the basis of the above embodiment, flowing ammonium bifluoride into a condensation bottle through a connecting elbow and condensing and crystallizing comprises: the rate of condensation crystallization of ammonium bifluoride is about 20 g/hr.
The rate of obtaining purified ammonium bifluoride is about 20 g/h at 200-220 deg.C, which is favorable to obtain ammonium bifluoride crystal with homogeneous grain size.
According to the method, impurities are removed by utilizing a sub-boiling distillation principle to obtain the ultra-pure ammonium bifluoride, water in the ammonium bifluoride is discharged to obtain ammonium bifluoride crystals with uniform fine particles, and the purification rate of the ammonium bifluoride is controlled by different heating temperatures. The ammonium bifluoride purification equipment has a very simple structure, a group of near-closed purification systems can be formed only by the PFA bottle 1, the PTFE connecting elbow 3, the PFA bottle 2 and the heating sleeve 4, and the equipment is easy to disassemble and assemble. The connecting elbow 3 is provided with an exhaust hole 5, an exhaust valve is installed, and water in the ammonium bifluoride is easily discharged. Because the inner diameter of the through hole of the purification structure is thicker (about 5 cm), the crystallization of ammonium bifluoride does not block the elbow 3 and the opening of the PFA bottle 2 during the purification process. The PFA bottle 1 is easy to take out from the heating jacket, and the residual impure ammonium bifluoride in the PFA bottle 1 can be easily cleaned after being slightly heated by the electric heating plate after being added with dilute nitric acid. The ultra-pure ammonium bifluoride obtained by the method can meet the requirements of trace element composition and isotope analysis in geological samples with ultra-low element content, and is simple to operate and low in cost.
The present disclosure is described in detail below with specific examples.
In the following examples, the raw materials and equipment sources selected were:
high-grade pure ammonium bifluoride (98%, Shanghai Aladdin Biotechnology Co., Ltd.)
Analytically pure ammonium bifluoride (99.99%, Shanghai Aladdin Biotechnology Co., Ltd.)
Sub-boiling distiller (with three groups of purification bottles)
Analytically pure nitric acid (purified by secondary sub-boiling distillation, chemical reagents of national drug group Co., Ltd.)
Ultrapure water (Millipore-Academic pure Water System, Millipore, USA, effluent conductivity 18.2M omega. em)-1)
Example 1
In this example, the method described above was used to purify guaranteed ammonium bifluoride (98%).
(1) Taking out 3 raw material bottles PFA bottles 1, putting 300g of ammonium bifluoride powder into the bottles, screwing the bottles and connecting elbows by screw threads, and putting the bottles into a heating sleeve; (2) the connecting elbows are respectively connected with three PFA bottles 2, and the heating jacket is slowly heated to 100 ℃ for half an hour to discharge water. Then slowly raising the temperature to 220 ℃, distilling the ammonium bifluoride in the PFA bottle 1 in a sub-boiling state, and leading vapor to enter the PFA bottle 2 through the PTFE connecting elbow 3 for condensation to crystallize white solid ammonium bifluoride crystals. (3) And (4) turning off the power supply, cooling to room temperature, and taking out the PFA bottle 2 to obtain purified ammonium bifluoride. ICP-MS detection is carried out on the ammonium bifluoride prepared in the embodiment, the detection results are shown in figure 3 and table 1, figure 3 shows a comparison schematic diagram of the content of metal ions of the ammonium bifluoride purified by an analytical pure ammonium bifluoride reagent and the ammonium bifluoride purified in the embodiments 1, 2 and 3, and a comparison list of the content of the metal ions is shown in table 1. The contents of metal ions Li, Sc, V, Cr, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, Pb, Th and U are all less than 10ng g-1Besides Sc and Ta, the content of other metal ions is lower than or far lower than that of the commercially available 99.99 percent analytically pure ammonium bifluoride.
TABLE 1
Note: nd indicates no detection.
Example 2
Analytically pure ammonium bifluoride (99.99%) was purified in this example using the method described above.
(1) Taking out 3 raw material bottles PFA bottles 1, putting 300g of ammonium bifluoride powder into the bottles, screwing the bottles and connecting elbows by screw threads, and putting the bottles into a heating sleeve; (2) the connecting elbows are respectively connected with three PFA bottles 2, and the heating jacket is slowly heated to 100 ℃ for half an hour to discharge water. Then slowly raising the temperature to 220 ℃, distilling the ammonium bifluoride in the PFA bottle 1 in a sub-boiling state, and leading vapor to enter the PFA bottle 2 through the PTFE connecting elbow 3 for condensation to crystallize white solid ammonium bifluoride crystals. (3) And (4) turning off the power supply, cooling to room temperature, and taking out the PFA bottle 2 to obtain purified ammonium bifluoride. The ammonium bifluoride prepared in this example was measured by ICP-MS and the results are shown in FIG. 3 and Table 1. The contents of metal ions Li, Sc, V, Cr, Ni, Cu, Ga, Rb, Sr, Y, Zr, Nb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, Pb, Th and U are all less than 1 ng.g-1The content of part of the elements was too low to be detected. Except for Zn and Rb, the content of other metal ions is lower than that of the 98 percent purified ammonium bifluoride in example 1.
Example 3
In this example, the purified ammonium acid fluoride obtained in example 1 was purified for the second time by the method described above.
(1) Taking out 3 raw material bottles PFA bottles 1, putting 300g of each purified ammonium bifluoride powder in the embodiment 1, screwing the raw material bottles and connecting elbows, and putting the bottles into a heating sleeve; (2) the connecting elbows are respectively connected with three PFA bottles 2, and the heating jacket is slowly heated to 100 ℃ for half an hour to discharge water. Then slowly raising the temperature to 220 ℃, distilling the ammonium bifluoride in the PFA bottle 1 in a sub-boiling state, and leading vapor to enter the PFA bottle 2 through the PTFE connecting elbow 3 for condensation to crystallize white solid ammonium bifluoride crystals. (3) And (4) turning off the power supply, cooling to room temperature, and taking out the PFA bottle 2 to obtain purified ammonium bifluoride. The ammonium bifluoride prepared in this example was measured by ICP-MS and the results are shown in FIG. 3 and Table 1. The contents of metal ions Li, Sc, V, Cr, Ni, Cu, Ga, Rb, Sr, Y, Zr, Nb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, and,Tm, Yb, Lu, Hf, Ta, Pb, Th and U are all less than 1ng g-1The content of part of the elements was too low to be detected. The contents of metal ions Cr, Ni, Cu, Ga, Sr, Y, Zr, Cs, La, Ce, Pr, Nd and U are slightly higher than those of the ammonium bifluoride purified in example 2, and the contents of other metal ions are all obviously lower than those of the ammonium bifluoride purified in example 2. This shows that after twice purification of the analytically pure ammonium bifluoride in example 1, ultra-high purity ammonium bifluoride can be obtained, meeting the requirements of trace element and isotope analysis of geological samples.
The above-mentioned embodiments are intended to illustrate the objects, aspects and advantages of the present disclosure in further detail, and it should be understood that the above-mentioned embodiments are only illustrative of the present disclosure and are not intended to limit the present disclosure, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present disclosure should be included in the scope of the present disclosure.
Claims (10)
1. An apparatus for purifying ammonium bifluoride, comprising:
the heating bottle is used for placing ammonium bifluoride to be purified;
a heating jacket, wherein the heating bottle is at least partially positioned in the heating jacket, so that the heating jacket performs sub-boiling distillation on the ammonium bifluoride to be purified in the heating bottle;
the condensation bottle is positioned outside the heating sleeve;
and the two ends of the connecting elbow are respectively communicated with the heating bottle and the condensing bottle, the connecting elbow is provided with an ascending section at the part connected with the heating bottle, and the part connected with the condensing bottle is provided with a descending section, so that the ammonium bifluoride subjected to sub-boiling distillation in the heating bottle flows into the condensing bottle through the ascending section and the descending section.
2. The apparatus for purifying ammonium bifluoride according to claim 1, wherein the connecting elbow is provided with an exhaust hole, and the exhaust hole is provided with an exhaust valve.
3. The apparatus for purifying ammonium bifluoride according to claim 1, wherein the heating bottle and the condensing bottle are meltable polytetrafluoroethylene wide-mouth bottles, and the inner diameter of the mouth of each wide-mouth bottle is greater than 4 cm.
4. The apparatus for purifying ammonium bifluoride according to claim 3, wherein the connecting elbow is made of polytetrafluoroethylene, and the connecting elbow is connected with the heating bottle and the condensing bottle respectively through threads.
5. The purification apparatus of ammonium bifluoride according to claim 1, wherein the heating bottle and the heating jacket are inclined at an angle of 30-60 degrees.
6. The apparatus of any one of claims 1 to 5, wherein the initial purity of the ammonium acid fluoride to be purified is not less than 98%.
7. The apparatus for purifying ammonium acid fluoride according to claim 6, wherein the initial purity of the ammonium acid fluoride to be purified is not less than 99.99%.
8. A method for purifying ammonium bifluoride by using the purification apparatus of ammonium bifluoride as claimed in any one of claims 1 to 7, comprising:
putting ammonium bifluoride to be purified into a heating bottle;
connecting the condensing bottle and the heating bottle through a connecting elbow;
placing the heating vials at least partially within a heating jacket with the condensation vials outside of the heating jacket;
and (3) carrying out sub-boiling distillation on the ammonium bifluoride through the heating sleeve, wherein the sub-boiling distilled ammonium bifluoride flows into the condensation bottle through the connecting elbow and is condensed and crystallized to obtain purified ammonium bifluoride.
9. The method of purifying ammonium acid fluoride according to claim 8, wherein said subjecting of said ammonium acid fluoride to sub-boiling distillation by said heating jacket comprises:
heating the temperature in the heating sleeve to 100 ℃ for about half an hour to discharge water through the exhaust holes on the connecting elbow;
and continuously heating to 200-220 ℃, and performing sub-boiling distillation on the ammonium bifluoride.
10. The method for purifying ammonium bifluoride by using the purification apparatus of ammonium bifluoride according to claim 8, wherein flowing the ammonium bifluoride into the condensation bottle through the connecting elbow and condensing and crystallizing the ammonium bifluoride comprises:
the rate of condensation crystallization of ammonium bifluoride is about 20 g/hr.
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