Device for synthesizing and purifying high-purity antimony pentafluoride
By using a synthesis and multi-stage distillation tower device with nitrogen trifluoride and antimony powder, the problems of low purity and safety hazards in the production of antimony pentafluoride have been solved, realizing the safe and simple production of high-purity antimony pentafluoride and meeting the needs of the semiconductor industry.
Patent Information
- Application Number
- CN202520190393.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-07
- Publication Date
- 2026-01-09
- Estimated Expiration
- 2035-02-07
AI Technical Summary
The existing production methods for antimony pentafluoride are complex, the product purity is not high, the separation of impurities is difficult, the equipment requirements are high, and there are safety hazards. In particular, the use of fluorine gas has strict requirements on equipment materials and operators, and hydrogen fluoride is difficult to separate from antimony pentafluoride.
Using nitrogen trifluoride and antimony powder as reaction raw materials, antimony pentafluoride is synthesized and purified through a combination of a synthesis reactor and a multi-stage distillation column. The process includes a combination of a pre-purification section and a distillation section. Low-activity and low-toxicity nitrogen trifluoride is used to avoid the generation of combustible gases. Hydrogen fluoride is removed by an adsorption column, and impurities are removed by a multi-stage distillation column.
It reduces equipment investment and operational complexity, improves safety, ensures product purity of 99.99% or higher, meets semiconductor industry requirements, avoids explosion risks, and simplifies operating procedures.
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Figure CN223774801U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to the production technology field of antimony pentafluoride, and particularly relates to a device for synthesizing and purifying high-purity antimony pentafluoride. BACKGROUND
[0002] In the field of semiconductor manufacturing, antimony pentafluoride is mainly used for doping processes in the production of semiconductor devices and integrated circuits in the electronic industry. With the development of the semiconductor industry, the degree of integration of integrated circuits is increasing, and the purity of antimony pentafluoride is also becoming higher (high-purity antimony pentafluoride requires a purity of more than 99.99% by volume fraction). At present, the method for industrial production of antimony pentafluoride is relatively complex, the purity of the product generated by the reaction is not high, impurity separation is difficult, and high requirements are placed on the equipment, which is not conducive to large-scale production. The invention patent with the publication number CN101531400B obtains antimony pentafluoride products with a purity of 98.5% by reacting fluorine gas with antimony trioxide and then purifying by rectification. This method is simple to operate and can obtain relatively pure antimony pentafluoride. However, element fluorine with high activity is used, fluorine gas has strong oxidizing properties, and the material requirements for the equipment are extremely high, requiring fluorine-resistant materials, which results in high equipment costs. On the other hand, the safety protection and the ability of the operating personnel are extremely high due to the toxicity of fluorine gas. In addition, hydrogen fluoride impurities in the fluorine gas will enter the antimony pentafluoride, which is difficult to separate from the antimony pentafluoride. Moreover, oxygen is generated during the reaction process, and the oxygen has strong flammability, which can easily cause explosions.
[0003] Therefore, how to realize the safe production of antimony pentafluoride has become a technical problem to be solved. CONTENT OF THE UTILITY MODEL
[0004] The utility model aims at providing a device for synthesizing and purifying high-purity antimony pentafluoride to solve the problems in the background technology.
[0005] To achieve the above-mentioned purpose, the utility model provides the following technical scheme.
[0006] A device for synthesizing and purifying high-purity antimony pentafluoride, comprising a raw material adding unit, the raw material adding unit is connected with a high-purity antimony pentafluoride purification unit through an antimony pentafluoride synthesis unit, and the high-purity antimony pentafluoride purification unit is connected with a high-purity antimony pentafluoride filling steel cylinder. The raw material adding unit comprises a nitrogen trifluoride steel cylinder for storing nitrogen trifluoride and a storage tank for storing antimony powder.
[0007] The utility model discloses a beneficial effect is: the utility model discloses a raw material for synthesizing antimony pentafluoride is the nitrogen trifluoride in the nitrogen trifluoride steel bottle and the storage and storage tank's metal antimony powder, specifically, adopt active, and the nitrogen trifluoride of toxic element fluorine is much lower as the reaction raw material, can reduce the requirement to the material quality of synthesis and purification equipment pipeline, to reach the characteristics of reducing equipment investment, simultaneously because the nitrogen trifluoride activity is lower, synthesis and purification reaction to the personnel operating skill requirement is low, further, the nitrogen trifluoride and metal antimony reaction process does not produce combustion-supporting gas, and the reaction is moderate, has the characteristics of high security and not easy to produce the risk of explosion.
[0008] Preferably, the antimony pentafluoride synthesis unit comprises a synthesis reactor connected with the nitrogen trifluoride steel bottle and the storage tank respectively, and a nitrogen gas part for purging the synthesis reactor; the synthesis reactor is externally provided with a heat exchange jacket, the top of the synthesis reactor is provided with a nitrogen trifluoride inlet, a metal antimony powder inlet and a purging inlet connected with the nitrogen gas part; the bottom of the synthesis reactor is provided with a tail gas outlet and a product outlet, the tail gas outlet is provided with a tail gas pipeline, the tail gas pipeline is provided with a first three-way joint, the second end of the first three-way joint is connected with a vacuum pump, and the third end of the first three-way joint is connected with a first tail gas treatment device.
[0009] Preferably, the high-purity antimony pentafluoride purification unit comprises a pre-purification part, the pre-purification part is connected with a buffer tank through a rectification part, and the buffer tank is connected with a high-purity antimony pentafluoride filling steel bottle through a diaphragm pump.
[0010] Preferably, the pre-purification part comprises two sets of parallelly arranged adsorption towers and a condenser connected with the product outlets of the adsorption towers, a second three-way joint is arranged between the product outlets of the adsorption towers and the condenser, and the third end of the second three-way joint is connected with the nitrogen gas part; a third three-way joint is arranged between the inlet of the adsorption tower and the product outlet of the synthesis reactor, and the third end of the third three-way joint is connected with the first tail gas treatment device.
[0011] Preferably, the nitrogen gas part comprises a high-purity nitrogen gas pipeline network, and the high-purity nitrogen gas pipeline network is connected with the purging inlet of the synthesis reactor and the third end of the second three-way joint through a flow meter and a nitrogen gas heater respectively.
[0012] Preferably, the rectification part comprises a first-stage rectification tower connected with the outlet of the condenser in the pre-purification part, the gas phase outlet in the middle and lower part of the first-stage rectification tower is connected with the inlet of a second-stage rectification tower, and the middle and upper part outlet of the second-stage rectification tower is connected with the inlet of the buffer tank.
[0013] Preferably, the outlet of the condenser is connected with the inlet of the first-stage rectification tower through a condensate pump and a fourth three-way joint, and the third end of the fourth three-way joint is connected with the nitrogen trifluoride inlet.
[0014] Preferably, the bottom of the primary rectification tower and the secondary rectification tower is respectively provided with a tower bottom reboiler, the top of the primary rectification tower and the secondary rectification tower is respectively provided with a tower top condenser, the bottom of the primary rectification tower is connected with the second tail gas treatment device through a primary rectification tower tank pump, the bottom of the secondary rectification tower is connected with the second tail gas treatment device through a secondary rectification tower tank pump, and the top gas phase outlet of the condenser, the top gas phase outlet of the primary rectification tower and the top gas phase outlet of the secondary rectification tower are respectively connected with a third tail gas treatment device.
[0015] The device for synthesizing and purifying high-purity antimony pentafluoride is prepared according to the above scheme, raw materials for synthesizing antimony pentafluoride in the device are nitrogen trifluoride and metal antimony powder, nitrogen trifluoride has the characteristics of low activity and toxicity relative to elemental fluorine, so that the device investment is reduced, the operation skill requirement of personnel is lowered, the life safety of on-site personnel is ensured, and the characteristics of high safety and low risk of explosion are achieved during the reaction of nitrogen trifluoride and metal antimony; the hydrogen fluoride content in the nitrogen trifluoride in the device is extremely low, so the technical problem that hydrogen fluoride in antimony pentafluoride is difficult to remove is solved at the source, and the device combines a pre-purification part and a rectification part after synthesis of antimony pentafluoride, the pre-purification part can effectively remove hydrogen fluoride, so that the rectification load of the rectification part and the difficulty of removing impurities are reduced, and the purity of the product is ensured; further, the primary rectification tower and the secondary rectification tower of the device both adopt the form of extracting products from the middle part of the rectification tower, and the two rectification towers can both remove light components and heavy components, so that the purification efficiency is improved, the metal ions in the heavy components do not pollute the product, the final purity of the product is ensured, and the device also innovatively uses the preliminarily purified antimony pentafluoride to flow back to the synthesis reactor as dilution gas, so that the reaction temperature is controlled. BRIEF DESCRIPTION OF DRAWINGS
[0016] Figure 1 It is a structural schematic view of the device.
[0017] Figure 2 It is a structural schematic view of the synthesis reactor.
[0018] In the figure: 1, trifluoride steel cylinder; 2, storage tank; 3, synthesis reactor; 4, heat exchange jacket; 5, trifluoride import; 6, metal antimony powder import; 7, purge import; 8, tail gas export; 9, product export; 10, vacuum pump; 11, first tail gas treatment device; 12, buffer tank; 13, diaphragm pump; 14, adsorption tower; 15, condenser; 16, high-purity nitrogen pipe network; 17, flow meter; 18, nitrogen heater; 19, first rectification tower; 20, second rectification tower; 21, condensate pump; 22, tower bottom reboiler; 23, tower top condenser; 24, first rectification tower kettle pump; 25, second rectification tower kettle pump; 26, second tail gas treatment device; 27, third tail gas treatment device; 28, high-purity antimony pentafluoride filling steel cylinder; 29, first tee; 30, second tee; 31, third tee; 32, fourth tee. DETAILED DESCRIPTION
[0019] The technical solutions in the embodiments of the utility model will be clearly and completely described below with reference to the drawings in the embodiments of the utility model.
[0020] Referring to Figure 1 The utility model discloses a kind of high-purity antimony pentafluoride synthesis and purification device, including raw material adding unit, raw material adding unit is connected with high-purity antimony pentafluoride purification unit by antimony pentafluoride synthesis unit, high-purity antimony pentafluoride purification unit is connected with high-purity antimony pentafluoride filling steel cylinder 28;The raw material adding unit includes trifluoride steel cylinder 1 for storing trifluoride, and storage tank 2 for storing metal antimony powder.The utility model initiatively uses active and low-toxic trifluoride as the raw material of antimony pentafluoride synthesis, to reduce equipment investment (lower the material requirement of pipe and other related equipment), reduce the difficulty of operation and the difficulty of purification feature, to realize the purpose of industrial production high-purity antimony pentafluoride.In addition, the utility model does not produce combustion-supporting gas in the process of aforementioned raw material synthesis, to improve the reliability and safety of reaction from the nature safety.
[0021] Further, as Figure 2The antimony pentafluoride synthesis unit includes a synthesis reactor 3 connected with a nitrogen trifluoride cylinder 1 and a storage tank 2 respectively, and a nitrogen part for purging the synthesis reactor 3; the synthesis reactor 3 is externally provided with a heat exchange jacket 4, the top of the synthesis reactor 3 is provided with a nitrogen trifluoride inlet 5, a metallic antimony powder inlet 6 and a purging inlet 7 communicated with the nitrogen part; the bottom of the synthesis reactor 3 is provided with a tail gas outlet 8 and a product outlet 9, the tail gas outlet 8 is provided with a tail gas pipeline, the tail gas pipeline is provided with a first three-way pipe 29, the second end of the first three-way pipe 29 is connected with a vacuum pump 10, and the third end of the first three-way pipe 29 is connected with a first tail gas treatment device 11. The continuous and stable reaction can be realized through the above-mentioned arrangement, and the purging and replacement of the gas in the synthesis reactor 3 can be realized through the purging inlet 7 communicated with the nitrogen part, the original air (especially oxygen) is replaced by nitrogen, so that the synthesis reaction is carried out under the condition of no combustion-supporting gas, and the synthesis reaction safety is improved. The heat exchange jacket 4 in the utility model can be an electric heating jacket, a heating oil jacket or a steam jacket.
[0022] Further, the high-purity antimony pentafluoride purification unit includes a pre-purification part, the pre-purification part is connected with a buffer tank 12 through a rectification part, and the buffer tank 12 is connected with a high-purity antimony pentafluoride filling cylinder 28 through a diaphragm pump 13. In the conventional technology, hydrogen fluoride is contained in fluorine gas, and after the hydrogen fluoride enters the crude antimony pentafluoride, it is difficult to remove the hydrogen fluoride by only the rectification method due to the close boiling point of the hydrogen fluoride and the antimony pentafluoride, so that the antimony pentafluoride cannot meet the use requirements of semiconductor customers. The pre-purification part and the rectification part are used for purifying the crude antimony pentafluoride when non-fluorine gas raw materials are used, so that the product gas purity is ensured.
[0023] Further, the pre-purification part includes two sets of parallelly arranged adsorption towers 14 and a condenser 15 connected with product outlets of the adsorption towers 14, a second three-way pipe 30 is arranged between the product outlets of the adsorption towers 14 and the condenser 15, and the third end of the second three-way pipe 30 is connected with the nitrogen part; a third three-way pipe 31 is arranged between the inlet of the adsorption tower 14 and the product outlet 9 of the synthesis reactor 3, and the third end of the third three-way pipe 31 is connected with the first tail gas treatment device 11. The adsorption tower 14 in the utility model is used for removing a small amount of hydrogen fluoride, so as to avoid affecting the subsequent impurity removal; and the condenser 15 condenses the antimony pentafluoride into liquid, and removes part of non-condensable gases such as nitrogen, oxygen and carbon dioxide in the antimony pentafluoride.
[0024] Further, the nitrogen part comprises a high-purity nitrogen pipe network 16 connected with the purging inlet 7 of the synthesis reactor 3 and the third end of the second three-way pipe 30 through the flow meter 17 and the nitrogen heater 18 respectively. The nitrogen part arranged in the utility model can be used for purging the synthesis reactor 3 on the one hand, avoiding that the oxygen and moisture in the synthesis reactor 3 affect the synthesis reaction and cause the explosion risk, and can be used for regenerating the adsorption tower to realize the long-time continuous and stable operation of the system on the other hand; further, the nitrogen heater 18 arranged in the utility model can heat the high-purity nitrogen from the high-purity nitrogen pipe network 16, the heated nitrogen entering the synthesis reactor 3 can not only preheat the synthesis reactor 3, but also promote the evaporation of the moisture in the synthesis reactor 3 to ensure the smooth progress of the subsequent synthesis reaction; meanwhile, the heating of the high-purity nitrogen can also improve the regeneration efficiency of the adsorption tower 14.
[0025] Further, the rectification part comprises a first-stage rectification tower 19 connected with the outlet of the condenser 15 in the pre-purification part, the gas phase outlet of the lower part of the first-stage rectification tower 19 is connected with the inlet of the second-stage rectification tower 20, and the upper part outlet of the second-stage rectification tower 20 is connected with the inlet of the buffer tank 12. The rectification part in the utility model adopts two-stage rectification, according to the characteristics of antimony pentafluoride and the characteristics of impurities, the outlet of the first-stage rectification tower 19 is arranged in the lower part of the first-stage rectification tower 19, and the outlet of the second-stage rectification tower 20 is arranged in the upper part of the second-stage rectification tower 20, the above arrangement can make the first-stage rectification tower 19 and the second-stage rectification tower 20 realize the characteristics of simultaneously removing the light components and the heavy components, which can not only improve the rectification efficiency and save energy, but also avoid that the metal particles in the heavy component impurities enter the high-purity antimony pentafluoride filling steel cylinder 28, thereby affecting the purity of the product. The second-stage rectification tower 20 in the utility model is mainly used for removing the heavy component impurities such as antimony trifluoride and metal ions in antimony pentafluoride.
[0026] Further, the outlet of the condenser 15 is connected with the inlet of the first-stage rectification tower 19 through the condensate pump 21 and the fourth three-way pipe 32, and the third end of the fourth three-way pipe 32 is connected with the nitrogen trifluoride inlet 5. The above arrangement of the utility model can realize that a part of the antimony pentafluoride passing through the pre-purification part is transported to the synthesis reactor 3, so as to control the temperature of the synthesis reactor 3 and ensure the mild progress of the synthesis reaction. The condenser 15 in the utility model can pre-purify the antimony pentafluoride on the one hand, and lays a foundation for the mild progress of the synthesis reaction of the synthesis reactor 3.
[0027] Further, the bottoms of the primary rectification tower 19 and the secondary rectification tower 20 are respectively provided with a tower bottom reboiler 22, the tops of the primary rectification tower 19 and the secondary rectification tower 20 are respectively provided with a tower top condenser 23, the tower bottom of the primary rectification tower 19 is connected with the second tail gas treatment device 26 through a primary rectification tower tank pump 24, the tower bottom of the secondary rectification tower 20 is connected with the second tail gas treatment device 26 through a secondary rectification tower tank pump 25; the top gas phase outlet of the condenser 15, the top gas phase outlet of the primary rectification tower 19 and the top gas phase outlet of the secondary rectification tower 20 are respectively connected with a third tail gas treatment device 27.
[0028] A method for synthesizing and purifying high-purity antimony pentafluoride, comprising the following steps:
[0029] Step 1: The metal antimony powder in the storage tank 2 is added into the synthesis reactor 3, high-purity nitrogen in the high-purity nitrogen pipe network 16 is introduced into the synthesis reactor 3 through the flow meter 17, the nitrogen heater 18 and the purging inlet 7 to purge the synthesis reactor 3, and at the same time, the vacuum pump 10 is started to vacuumize the inside of the synthesis reactor 3; after the vacuumization is completed, the heat exchange jacket 4 is used to heat exchange the materials in the synthesis reactor 3, so that the temperature of the materials in the synthesis reactor 3 is 250-350℃; the purging time of the high-purity nitrogen is 5-12h, and the running time of the vacuum pump 10 is 5-12h;
[0030] Step 2: The nitrogen trifluoride in the nitrogen trifluoride cylinder 1 is introduced into the synthesis reactor 3 to carry out a synthesis reaction under the condition that the pressure is 1.5 barg, and the crude antimony pentafluoride is generated after the reaction;
[0031] Step 3: The crude antimony pentafluoride is introduced into the adsorption tower 14 through the inlet of the adsorption tower 14 to carry out adsorption, the adsorbent in the adsorption tower 14 is one or a combination of sodium fluoride, calcium fluoride or magnesium fluoride, which is used to remove trace hydrogen fluoride, and the hydrogen fluoride in the crude antimony pentafluoride is reduced to 0.005ppm or below; the particle size of the adsorbent is 3-5mm, and the adsorption tower 14 is one standby;
[0032] Step 4: The crude antimony pentafluoride passing through the adsorption tower 14 is condensed into a liquid phase in the condenser 15, and the non-condensable gas is introduced into the third tail gas treatment device 27 for treatment; the liquid phase antimony pentafluoride after condensation is introduced into the fourth three-way valve 32 through the condensate pump 21; part of the liquid phase antimony pentafluoride after condensation is refluxed to the synthesis reactor 3 as dilution gas, and the other part of the liquid phase antimony pentafluoride after condensation is introduced into the primary rectification tower 19 for rectification; the operating temperature of the condenser 15 is 10-50℃;
[0033] Step 5: The liquid antimony pentafluoride is introduced into the first rectification column 19 for rectification, the operating temperature at the top of the column is 20-50℃, and the top pressure is 0.5-1 barg; the light component impurity nitrogen and the trace amount of unconverted trifluoride in the heavy component can be removed in the above rectification process; the light component impurity is introduced into the third tail gas treatment device 27 through the top of the first rectification column 19 for treatment, and the heavy component impurity is introduced into the second tail gas treatment device 26 through the bottom of the first rectification column 19 and the first rectification column tank pump 24 for treatment; the gaseous phase after rectification is introduced into the inlet of the second rectification column 20 through the gaseous phase outlet in the middle and lower part of the first rectification column 19;
[0034] Step 6: The gaseous phase passing through the first rectification column 19 is introduced into the second rectification column 20 for rectification, the light component after rectification is introduced into the third tail gas treatment device 27 through the top of the second rectification column 20 for treatment, and the heavy component after rectification is introduced into the second tail gas treatment device 26 through the bottom of the second rectification column 20 and the second rectification column tank pump 25 for treatment; the gaseous phase after rectification is introduced into the buffer tank 12 through the outlet in the upper and middle part of the second rectification column 20; the operating temperature at the top of the second rectification column 20 is 20-50℃, and the top pressure is 0.3-1 barg; the gaseous phase of antimony pentafluoride introduced into the buffer tank 12 has a volume fraction of 99.99% or more;
[0035] Step 7: The product gas in the buffer tank 12 is filled into the high-purity antimony pentafluoride filling steel cylinder 28 by the diaphragm pump 13.
[0036] In the step 3, one adsorption column 14 is in operation, and the other adsorption column 14 is in standby state, which includes regeneration of the adsorption column 14; when the adsorption column 14 needs to be regenerated, the high-purity nitrogen pipe network 16 introduces nitrogen into the regenerated adsorption column 14 through the flow meter 17 and the nitrogen heater 18 for regeneration, and the regenerated nitrogen is introduced into the first tail gas treatment device 11 through the inlet of the adsorption column 14 and the third end of the third three-way valve 31.
[0037] The utility model discloses to the problem of the synthesis and purification of antimony pentafluoride at present, need to find the substance of the element fluorine of strong activity and toxic can be replaced as reaction raw material, can reduce the requirement to the material quality of synthesis and separation purification equipment pipeline etc., reduce the investment, reduce the requirement to operating personnel, and combustion-supporting gas is not produced in the reaction process, improve the reliability and safety of reaction from the nature safety, and fluorine gas and metal antimony or trioxide antimony reaction can emit a large amount of heat, how to control the synthesis reaction temperature is also difficult, in addition, fluorine gas contains hydrogen fluoride, will enter the crude product of antimony pentafluoride, because hydrogen fluoride and antimony pentafluoride boiling point is close, only through the mode of rectification is difficult to remove hydrogen fluoride, makes antimony pentafluoride not reach the requirement of semiconductor customer use, therefore find suitable synthesis and separation method synthesis and purification antimony pentafluoride is imperative, the utility model discloses to adopt nitrogen trifluoride and metal antimony reaction obtains antimony pentafluoride, and the antimony pentafluoride produced in the reaction is purified to 99.99% (volume fraction) and above through adsorption and rectification and meets the purity of semiconductor industry use requirement, and the antimony pentafluoride after purification returns to the synthesis reactor and takes away the heat generated in the reaction, and controls the reaction temperature, the advantage of the utility model is 1. adopt active, the toxicity of nitrogen trifluoride of element fluorine is much lower as reaction raw material, can reduce the requirement to the material quality of synthesis and purification equipment pipeline etc., and the investment is reduced, 2. nitrogen trifluoride is low in activity, and the synthesis and purification reaction is low in operating skill requirement, 3. nitrogen trifluoride and metal antimony reaction process do not produce combustion-supporting gas, and the reaction is moderate, meets the requirement of intrinsic safety, 4. the hydrogen fluoride content in nitrogen trifluoride is extremely low and can be ignored, and the difficult problem that hydrogen fluoride is difficult to remove in antimony pentafluoride is solved from the source, 5. use the antimony pentafluoride of preliminary purification as dilution gas and enter the synthesis reactor, take away the reaction heat very well and control the reaction temperature, and have no influence to subsequent separation.
[0038] Although the embodiments of the utility model have been shown and described, it can be understood by those skilled in the art that various changes, modifications, replacements and variations can be made to these embodiments without departing from the principles and spirits of the utility model, and the scope of the utility model is defined by the appended claims and their equivalents.
Claims
1. An apparatus for the synthesis and purification of high-purity antimony pentafluoride, characterized in that: It includes a raw material addition unit, which is connected to a high-purity antimony pentafluoride purification unit through an antimony pentafluoride synthesis unit, and the high-purity antimony pentafluoride purification unit is connected to a high-purity antimony pentafluoride filling cylinder (28). The raw material addition unit includes a nitrogen trifluoride cylinder (1) for storing nitrogen trifluoride and a storage tank (2) for storing antimony powder.
2. The apparatus for synthesizing and purifying high-purity antimony pentafluoride according to claim 1, characterized in that: The antimony pentafluoride synthesis unit includes a synthesis reactor (3) connected to a nitrogen trifluoride cylinder (1) and a storage tank (2) respectively, and a nitrogen section for purging the synthesis reactor (3); The synthesis reactor (3) is provided with a heat exchange jacket (4) on the outside. The top of the synthesis reactor (3) is provided with a nitrogen trifluoride inlet (5), a metal antimony powder inlet (6) and a purging inlet (7) connected to the nitrogen section. The bottom of the synthesis reactor (3) is provided with a tail gas outlet (8) and a product outlet (9). The tail gas outlet (8) is provided with a tail gas pipe. The tail gas pipe is provided with a first tee (29). The second end of the first tee (29) is connected to a vacuum pump (10), and the third end of the first tee (29) is connected to a first tail gas treatment device (11).
3. The apparatus for synthesizing and purifying high-purity antimony pentafluoride according to claim 2, characterized in that: The high-purity antimony pentafluoride purification unit includes a pre-purification section, which is connected to a buffer tank (12) via a distillation section. The buffer tank (12) is connected to a high-purity antimony pentafluoride filling cylinder (28) via a diaphragm pump (13).
4. The apparatus for synthesizing and purifying high-purity antimony pentafluoride according to claim 3, characterized in that: The pre-purification section includes two sets of adsorption towers (14) arranged in parallel and a condenser (15) connected to the product outlet of the adsorption tower (14). A second tee (30) is provided between the product outlet of the adsorption tower (14) and the condenser (15), and the third end of the second tee (30) is connected to the nitrogen section. A third tee (31) is provided between the inlet of the adsorption tower (14) and the product outlet (9) of the synthesis reactor (3), and the third end of the third tee (31) is connected to the first tail gas treatment device (11).
5. The apparatus for synthesizing and purifying high-purity antimony pentafluoride according to claim 2 or 4, characterized in that: The nitrogen section includes a high-purity nitrogen pipeline (16), which is connected to the purge inlet (7) and the third end of the second tee (30) of the synthesis reactor (3) via a flow meter (17) and a nitrogen heater (18).
6. The apparatus for synthesizing and purifying high-purity antimony pentafluoride according to claim 4, characterized in that: The distillation section includes a primary distillation column (19) connected to the outlet of the condenser (15) in the pre-purification section. The lower gas phase outlet of the primary distillation column (19) is connected to the inlet of the secondary distillation column (20), and the upper outlet of the secondary distillation column (20) is connected to the inlet of the buffer tank (12).
7. The apparatus for synthesizing and purifying high-purity antimony pentafluoride according to claim 6, characterized in that: The outlet of the condenser (15) is connected to the inlet of the first-stage distillation column (19) via a condensate pump (21) and a fourth three-way valve (32), and the third end of the fourth three-way valve (32) is connected to the nitrogen trifluoride inlet (5).
8. The apparatus for synthesizing and purifying high-purity antimony pentafluoride according to claim 7, characterized in that: The bottom of the primary distillation column (19) and the secondary distillation column (20) are respectively provided with bottom reboilers (22), and the top of the primary distillation column (19) and the secondary distillation column (20) are respectively provided with top condensers (23). The bottom of the primary distillation column (19) is connected to the second tail gas treatment device (26) through the primary distillation column bottom pump (24), and the bottom of the secondary distillation column (20) is connected to the second tail gas treatment device (26) through the secondary distillation column bottom pump (25). The top gas outlet of the condenser (15), the top gas outlet of the first-stage distillation column (19), and the top gas outlet of the second-stage distillation column (20) are respectively connected to the third tail gas treatment device (27).
Citation Information
Patent Citations
Method for preparing antimony pentafluoride
CN101531400B