A preparation device and preparation process for high-purity electronic-grade thionyl fluoride

Abstract

The invention discloses a preparation device for preparing high-purity electronic-grade thionyl fluoride and a preparation process thereof. The device comprises: a mixer, the mixer is communicated with a first preheating device, the first preheating device is communicated with a first distillation tower, the top of the distillation tower is connected with a condenser, the condenser is communicated with a crude product tank, the crude product tank is communicated with a second preheating device, the second preheating device is communicated with a second distillation tower, the second distillation tower is communicated with a third distillation tower, the third distillation tower is connected to a storage tank, the storage tank is connected to a vaporization device, the vaporization device is pressurized and stored in a high-pressure buffer tank, the high-pressure buffer tank is connected to at least three adsorption towers, and the adsorption tower at the rear end is connected to a high-pressure product tank. The invention improves the purity of the finished product while fully utilizing all raw material components.

Description

Technical Field

[0001] The invention relates to the preparation of thionyl fluoride, in particular to a preparation device and a preparation process for preparing high-purity electronic-grade thionyl fluoride. Background Art

[0002] With the continuous development of the semiconductor industry, high-end chip technology has made continuous breakthroughs, among which dry etching technology has been widely used. As the key etching electronic gas and cleaning electronic gas, higher demands have been put forward. Fluorine-based electronic gases have ushered in rapid development. Typical fluorine-based electronic gases currently include sulfur hexafluoride (SF6), carbon tetrafluoride (CF4) and fluorocarbon gases (such as CH3F, CH2F2, CHF3, C2F6, C3F8, etc.). Their GWP values ​​are relatively high and have a greater potential impact on the environment. The development of low-GWP etching and cleaning gases has become the key to the development of the semiconductor industry. While ensuring the etching and cleaning effects, thionyl fluoride (SOF2) is easier to dispose of and more environmentally friendly. Existing technologies usually use anhydrous hydrogen fluoride (AHF) and thionyl chloride (SOCl2) to synthesize thionyl fluoride.

[0003] Although the existing technology also uses anhydrous hydrogen fluoride (AHF) and thionyl chloride (SOCl2) for preparation, the purity of thionyl fluoride obtained after the two are mixed is low. Although the product is distilled through preliminary distillation, the purity of the obtained product does not even reach 99.9%. If the gas obtained in this way is used directly for etching and cleaning, it will lead to poor etching and cleaning effects of the chip, which will directly affect the quality of the chip.

[0004] Therefore, this case aims to provide a preparation device and preparation process for high-purity electronic-grade thionyl fluoride, combining product synthesis and crude product separation in the same equipment, making full use of heat balance, and fully separating the by-product hydrogen chloride gas from the product to obtain higher-purity hydrogen chloride gas, thereby increasing the added value of the by-product and improving the purity of the finished product while fully utilizing all raw material components. Summary of the Invention

[0005] The present invention provides a preparation device and a preparation process for high-purity electronic-grade thionyl fluoride, which can effectively solve the above problems.

[0006] The present invention is achieved in that:

[0007] A preparation device for high-purity electronic-grade thionyl fluoride, comprising: a mixer, the mixer being in communication with a first preheating device, the first preheating device being in communication with a first distillation tower, the top of the distillation tower being connected to a condenser, the condenser being in communication with a crude product tank, the crude product tank being in communication with a second preheating device, the second preheating device being in communication with a second distillation tower, the second distillation tower being in communication with a third distillation tower, the third distillation tower being connected to a storage tank, the storage tank being connected to a vaporization device, the vaporization device being connected to a high-pressure buffer tank, the high-pressure buffer tank being connected to at least three adsorption towers, the adsorption tower at the rear end being connected to a high-pressure product tank, and further comprising:

[0008] The mixer comprises a mixing tube for mixing materials, wherein the mixing tube is provided with an anhydrous hydrogen fluoride feeding end and a thionyl chloride feeding end, and the end of the mixing tube away from the thionyl chloride feeding end is provided with a discharge end.

[0009] A middle material separation structure, wherein the mixing tube includes a front branch pipe provided with an anhydrous hydrogen fluoride feed end and a thionyl chloride feed end, and a rear segment provided with a discharge end, wherein the middle positions of the front branch pipe and the rear segment are connected by a cross-connecting plate, and the middle material separation structure includes a first sealing crank sleeve provided at the upper end of the cross-connecting plate, a second sealing crank sleeve connected to the lower end of the cross-connecting plate, a driving member provided on the side of the first sealing crank sleeve away from the cross-connecting plate, and a dynamic material separation member connected to the output end of the driving member that passes through the cross-connecting plate and is located in the first sealing crank sleeve and the second sealing crank sleeve;

[0010] Axial material distribution structure, the front section branch pipe and the rear section segment are both provided with a mounting groove on one side close to the cross-connecting plate, a static material distribution member is movably provided in the mounting groove, the first sealing crank sleeve and the second sealing crank sleeve are connected to the rear side of the cross-connecting plate and respectively abut against the two static material distribution members, the raw materials entering through the anhydrous hydrogen fluoride feed end and the thionyl chloride feed end are distributed by the front static material distribution member, mixed by the dynamic material distribution member, and then distributed by the rear static material distribution member;

[0011] The vaporization device comprises: a vaporization tank, a thionyl fluoride liquid inlet is provided at the bottom of the vaporization tank, a thionyl fluoride gas outlet is provided at the top of the vaporization tank, a plurality of steam pipes are provided in the vaporization tank, and the steam pipes are connected to the external air inlet and air outlet, and further comprises:

[0012] An isolation and distribution structure includes a middle mounting plate disposed in the middle section of the vaporizer, the middle mounting plate dividing the vaporizer into a vaporization zone and a distribution zone, a plurality of distribution pipes connected to the lower end of the middle mounting plate, a lower distribution assembly disposed on the outer side of the middle portion of the distribution pipes, the lower distribution assembly controlling the opening and closing of all distribution pipes, the bottoms of the distribution pipes connected to a lower pumping pipe extending into the thionyl fluoride liquid at the bottom of the vaporizer, and the lower distribution assembly periodically pumping the thionyl fluoride liquid at the bottom of the vaporizer into the distribution pipes via the lower pumping pipe;

[0013] The segmented vaporization structure includes several accommodating chambers arranged on the central mounting plate. The inlet hole at the bottom of the accommodating chamber is connected to the distribution pipe. The steam pipe is inserted above the accommodating chamber. An inner inclined hole is provided in the middle of the steam pipe. The inner inclined hole is inclined outward to have an outer guide plate. An inner guide component is provided on the inner side of the outer guide plate at a position corresponding to the inner inclined hole. An outer guide component is provided on the outer side of the outer guide plate. Both the inner guide component and the outer guide component are connected to the external exhaust structure.

[0014] As a further improvement, the first preheating device is the same as the second preheating device, and the first preheating device includes: a preheating tank body, the upper end of the preheating tank body is connected to a crude gas inlet, the lower end of the preheating tank body is connected to a crude gas outlet, at least one serpentine coil is connected between the crude gas inlet and the crude gas outlet, the preheating tank body is provided with an inlet pipe and an outflow pipe, and also includes: an internal circulation contact type structure, the serpentine coil includes an upper through portion connected to the crude gas inlet, the upper through portion is connected to a horizontal transmission portion, the end of the horizontal transmission portion is connected to a bending portion, the horizontal transmission portion and the bending portion are alternately arranged, the horizontal transmission portion at the lowest end is connected to a lower through portion communicating with the crude gas outlet, the internal circulation contact type structure includes an upper through portion provided in the bending portion The inner contact piece of the part, the outer side of the inner contact piece is provided with a hollow piece, the inner contact piece is connected to the side of the inner contact piece close to the horizontal transmission part with an outer contact piece, the outer contact piece is located between the two horizontal transmission parts, the inner and outer contact pieces are both connected to the steam inlet pipe, the steam inlet pipe is located on the outside of the preheating tank body, the steam entering through the steam inlet pipe is output from the inner and outer contact pieces and then condenses and falls to the bottom of the preheating tank body; the lower isolation structure comprises an inner heat cover arranged at the lower end of the lower through part, the outer side of the inner heat cover is provided with an outer isolation cover, the outer side of the outer isolation cover is provided with a circulation rack, the outer side of the circulation rack is fixed to the inner side of the preheating tank body and communicates with the outside, and the condensed steam falls to the bottom of the preheating tank body after being guided by the outer isolation cover.

[0015] As a further improvement, the first distillation tower, the second distillation tower and the third distillation tower have the same structure and size, and an air inlet end is provided on one side of the first distillation tower, and further comprises: a packing installation structure, a top tray is provided on the inner side of the distillation tower, the packing installation structure comprises a middle fitting locked on the top tray, a plurality of circular installation cylinders are sleeved on the middle fitting, a packing is provided on the inner side of the circular installation cylinder, a recessed area is provided on the inner side of the circular installation cylinder, the recessed area and the inner wall of the distillation tower form a closed space, a clamping piece is provided on the inner side of the recessed area, the clamping piece comprises a guide cartridge provided in the recessed area, a clamping arm is movably installed on the inner side of the guide cartridge, and a pressing plate is connected to the side of the clamping arm away from the middle fitting. The tensioning arm includes a straight arm portion that cooperates with the guide cartridge, the straight arm portion is movably connected to the push piece, the straight arm portion is connected to a fan-shaped seat on the side away from the guide cartridge, the clamping plate is locked on the fan-shaped seat, the clamping piece abuts against the inner wall of the distillation tower, and when the middle fitting is fixed, a number of circular mounting cylinders are installed on the middle fitting in sequence; the pressurized closing structure includes an outward expansion rod movably installed on the inner wall of the middle fitting, and an outward expansion piece is movably provided on the inner side of the clamping piece, and the outward expansion piece is movably cooperated with the middle fitting piece. When the outward expansion rod is embedded in the middle fitting piece, the outward expansion piece is pushed outward and the clamping piece abuts against the inner wall of the distillation tower, and a sealing piece is provided on the outer periphery of the clamping plate, and the sealing piece is tightly attached to the inner wall of the distillation tower as the clamping piece moves.

[0016] As a further improvement, the cross-connecting plate includes two connecting arc plates connected between the front section branch pipe and the rear section segment, a cross-connecting plate is connected between the two connecting arc plates, a pair of through holes are provided on the cross-connecting plate, a blocking piece is locked on the pair of through holes, the second sealing crank sleeve includes a lower outer sealing sleeve that is fitted with the lower end of the connecting arc plate, the inner side of the lower outer sealing sleeve is connected to a lower inner sealing arc sleeve that is fitted with the inner side wall of the connecting arc plate, the lower inner sealing arc sleeve is provided with a facing empty cylinder, the lateral opening of the facing empty cylinder, the first sealing crank sleeve includes an upper outer sealing sleeve that is fitted with the upper end of the connecting arc plate, the upper outer sealing The inner side of the sleeve is connected to an upper inner closed sleeve arc sleeve that fits with the inner wall of the connecting arc plate. The lower end of the upper inner closed sleeve arc sleeve is provided with a facing column tube, and the lateral opening of the facing column tube. When the first sealing crank sleeve and the second sealing crank sleeve are matched, the facing column tube is embedded in the facing empty cylinder through the facing hole, and the facing column tube and the facing empty cylinder are connected through the facing hole via the blocking piece. The horizontal connecting plate is provided with a horizontal threaded hole in the horizontal direction corresponding to the position of the facing hole. The blocking piece includes a stud portion that passes through the facing column tube and the facing empty cylinder and cooperates with the horizontal threaded hole. The stud portion is provided with an outer blocking portion, and the outer blocking portion blocks the facing hole.

[0017] As a further improvement, a rotating joint is provided in the middle part of the transverse connecting plate, and the dynamic material distribution part includes a circulating ring arranged in the rotating joint, an upper mixing part is provided on the top of the circulating ring, and the lower end of the circulating ring is connected to the lower mixing part, the upper mixing part is connected to the output end of the driving part, and the upper mixing part and the lower mixing part have the same structure and size, the upper mixing part includes an axial column connected to the circulating ring, the axial column is connected to the driving part, a semi-arc-shaped dispersion piece is provided on the axial column, a plurality of dispersion holes are provided on the dispersion piece, and a gasket is provided on the outer side of the dispersion piece, and the gasket is fitted on the inner side of the first sealing crank sleeve.

[0018] As a further improvement, the mounting groove includes an internal cavity, a plurality of external expansion grooves are provided on the inner side of the accommodating cavity, an external spring sheet is provided on the outer edge of the external expansion groove, and the static dividing material component stretches out the external spring sheet and then snaps into the accommodating cavity and the external expansion groove. The static dividing material component includes a clamping ring that cooperates with the internal cavity, a plurality of external expansion pads are provided on the outer side of the clamping ring, a spiral sheet is provided on the inner side of the clamping ring, and the outer edge of the clamping ring is attached to the outer side of the first sealing crank sleeve and the second sealing crank sleeve.

[0019] As a further improvement, the inner and outer sides of the bent portion are both opened, the internal contact part includes an inner air inlet portion embedded in the opening on the outer side of the bent portion, the inner opening on the inner side of the bent portion is provided with an inner air outlet portion, an inner barrier portion is connected between the inner air inlet portion and the inner air outlet portion, the inner air inlet portion is connected to the steam inlet pipe, all the inner barrier portions form a fan-shaped structure, the inner barrier portion includes an inner through pipe connected between the inner air inlet portion and the inner air outlet portion, and a plurality of barbed tubes extend outward from the circumferential outside of the inner through pipe.

[0020] As a further improvement, the inner guide component includes an adsorption pad arranged on the inner inclined hole, the lower end of the adsorption pad is connected to a lower inclined tube, and all the lower inclined tubes are connected through an inner ring, and the lower inclined tube is filled with a barrier group. The outer guide component includes a receiving sleeve arranged under the outer guide plate, and the receiving sleeve is connected to a lower bend pipe, and all the lower bend pipes are connected to an outer ring. The inner ring and the outer ring are connected through a linkage pipe, and the linkage pipe is connected to the external air extraction structure.

[0021] As a further improvement, the circular mounting tube is an I-shaped structure, the middle portion of the circular mounting tube is a hollow ring, the bottom and top surfaces of the circular mounting tube are both mesh plates, and the outer circumferential surface of the circular mounting tube is a closed surface.

[0022] The present invention also provides a preparation process for high-purity electronic-grade thionyl fluoride, which uses the above-mentioned preparation device for high-purity electronic-grade thionyl fluoride, comprising the following steps:

[0023] S1: adding anhydrous hydrogen fluoride to the bottoms of the first distillation tower, the second distillation tower, and the third distillation tower in advance, then metering anhydrous hydrogen fluoride and thionyl chloride in a molar ratio of 2:1 into a mixer, passing the mixed fluid into a first preheating device and preheating it to 50-100° C., and then continuously adding it to the first distillation tower;

[0024] S2: The bottom liquid of the first distillation tower is circulated back to the tower position through the distillation circulation pump, and the materials are controlled to react at 80-150 ° C and 0-0.5 MPa through the tower bottom reboiler. The thionyl fluoride and hydrogen chloride generated by the reaction enter the condenser from the top of the tower in the form of gas for condensation and separation. The thionyl fluoride is condensed into a liquid portion that refluxes to the top of the tower, and the portion is extracted to the crude product tank. The reflux ratio is 3-5, and the hydrogen chloride gas is discharged from the top of the condenser to the first distillation tower;

[0025] S3: The crude thionyl fluoride is preheated to 30-50°C by a second preheating device and then enters a second distillation tower. The material is controlled at 0-30°C by a tower bottom reboiler, and the light components are removed at the top of the tower, and a product free of light components is obtained in the tower bottom;

[0026] S4: The product without light components enters the third distillation tower for purification, and the material is controlled at 30-50° C. by the tower bottom reboiler, and the thionyl fluoride product is obtained at the top of the tower. The reflux ratio is controlled at 5-10, part of it is refluxed to the top of the tower, and part of it is extracted to the product storage tank for storage. The hydrogen fluoride in the tower bottom is recycled back to the mixer for a cyclic reaction;

[0027] S5: The thionyl fluoride product is fully vaporized at 50-100°C in a vaporizer, compressed to 1-1.5 Map by a compressor, and stored in a high-pressure buffer tank. The high-pressure product gas then passes through a three-stage molecular sieve adsorption tower to remove hydrogen fluoride and hydrogen chloride, resulting in 99.999% pure thionyl fluoride, which is then stored in a high-pressure product tank.

[0028] The beneficial effects of the present invention are:

[0029] The present invention realizes continuous synthesis of thionyl fluoride by adopting a reactive distillation tower, combines product synthesis and crude product separation in the same device, fully utilizes heat balance, and adopts a two-stage continuous distillation method in the whole process. First, light components with a great influence on product purity are removed by a first-stage distillation, and then a high-purity product is obtained by a second-stage distillation, thereby ensuring the high efficiency of the device. During the whole distillation process, by-product hydrogen chloride gas is fully separated from the product to obtain hydrogen chloride gas with high purity, thereby increasing the added value of the by-product. At the same time, there is no need to further process the by-product, thereby fully utilizing the product. Finally, the product is vaporized to form a high-pressure gas, and then a three-stage continuous adsorption is performed to remove trace impurities, thereby ensuring a high adsorption rate, thereby allowing the obtained product to have a purity of 99.999%.

[0030] Whether it is a static mixer or a dynamic mixer used in the prior art, the coating needs to be regenerated after a period of use. When the coating is regenerated, the entire mixer needs to be removed from the pipeline and then immersed in the coating, which is not only time-consuming and labor-intensive, but also the connected pipeline needs to be repeatedly tested before it can be used. Therefore, the present invention sets up a middle dividing structure, firstly divides the entire mixer into two parts, namely the front section branch pipe and the rear section segment, and sets a middle dividing structure between the two parts, which can not only achieve the effect of dynamic mixing in the middle part through the dynamic dividing piece, but also the entire mixer can be disassembled at this time, and the regeneration of the mixing structure can be carried out directly in the middle position, thereby effectively allowing the dynamic mixing effect of the mixer to maintain a good dispersion effect, thereby improving the mixing effect of anhydrous hydrogen fluoride and thionyl chloride.

[0031] Although the dynamic material dividing parts are directly installed on the middle material dividing structure to achieve the effect of being removable and regenerated, the static mixing structures in the front branch pipe and the rear segment are also difficult to regenerate. Therefore, the present invention arranges an axial material dividing structure on the basis of the middle material dividing structure, and arranges the two static material dividing parts directly on the side positions of the first sealing crank sleeve and the second sealing crank sleeve, so that the two static material dividing parts can be directly exposed after the first sealing crank sleeve and the second sealing crank sleeve are removed, so that the coating on the static material dividing parts can be directly regenerated from the outside, thereby achieving the regeneration effect of the static and dynamic mixing parts, and no cumbersome operation is required, so that the mixing effect of the mixer can be maintained for a long time.

[0032] The removable packing in the distillation tower in the prior art is difficult to perfectly match with the tower body, which leads to the easy appearance of gaps between the packing and the tower body, so that some gas will directly pass through the packing area along the edge gap and leak through the packing, resulting in some untreated packing directly flowing into the tower bottom or the tower top, making it difficult to purify the distillation product. Therefore, the present invention adopts a unified middle matching part through the packing installation structure set up, and all the circular mounting cylinders are uniformly installed to the middle matching part, which can reduce the inner diameter of the circular mounting cylinder, and then the circular mounting cylinder is fixed to the inner side of the distillation tower by means of a clamp, so that the circular mounting cylinder can be firmly fixed to the distillation tower while being detachable.

[0033] Although reducing the inner diameter of the circular mounting cylinder and setting a clamp can make the installation of the circular mounting cylinder stable, it is still difficult to avoid the gas in the outer circumference moving to the upper and lower ends without being filtered by the packing. Therefore, the present invention provides a pressurized closed structure based on the packing mounting structure, which not only makes the cooperation between the circular mounting cylinder and the distillation tower more stable, but also can seal the gap between the circular mounting cylinder and the distillation tower through the sealing member to prevent the gas from leaking from the outer edge of the circular mounting cylinder, so that the gas moved to the tower bottom and the tower top can meet the conditions better. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. It should be understood that the following drawings only illustrate certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without paying any creative work.

[0035] Figure 1 It is a structural schematic diagram of the present invention.

[0036] Figure 2 It is a structural schematic diagram of the mixer of the present invention.

[0037] Figure 3 This invention Figure 2 Schematic diagram of the top view structure.

[0038] Figure 4 This invention Figure 3 Cross-section view at AA in the middle.

[0039] Figure 5 It is a side view structural diagram of the partial material structure in the present invention.

[0040] Figure 6 This invention Figure 5 Magnified view of area A in center.

[0041] Figure 7 It is a structural schematic diagram of the static material parts of the present invention.

[0042] Figure 8 It is a structural schematic diagram of the first preheating device of the present invention.

[0043] Figure 9 This invention Figure 8 Schematic diagram of the top view structure.

[0044] Figure 10 This invention Figure 9 Cross-section view at the middle BB.

[0045] Figure 11 This invention Figure 10 Magnified view of area B.

[0046] Figure 12 It is a structural schematic diagram of the hollow member of the present invention.

[0047] Figure 13 It is a structural schematic diagram of the lower isolation structure of the present invention.

[0048] Figure 14 It is a structural schematic diagram of the first distillation tower of the present invention.

[0049] Figure 15 This invention Figure 14 Schematic diagram of the top view structure.

[0050] Figure 16 This invention Figure 15 Cross-sectional view at EE.

[0051] Figure 17 It is a structural diagram of the cooperation between the middle matching piece and the outer expansion rod of the present invention.

[0052] Figure 18 It is a structural schematic diagram of the circular mounting cylinder of the present invention.

[0053] Figure 19 It is a schematic structural diagram of the cooperation between the clamping member and the push-out member of the present invention.

[0054] Figure 20 This invention Figure 19 Magnified view of area E in the middle.

[0055] Figure 21 It is a structural schematic diagram of the vaporization device of the present invention.

[0056] Figure 22 This invention Figure 21 Schematic diagram of the top view structure.

[0057] Figure 23 This invention Figure 22 Cross-section of CC.

[0058] Figure 24 This invention Figure 23 Magnified view of area C in the middle.

[0059] Figure 25 It is a structural schematic diagram of the isolation and distribution structure of the present invention.

[0060] Figure 26 This invention Figure 25 Magnified view of area D in the middle.

[0061] In the picture:

[0062] Mixing tube 10, front section branch pipe 11, rear section segment 12, cross-connecting plate 13, connecting arc plate 131, cross-connecting plate 132, rotary joint 1321, through hole 133, plugging piece 135, stud portion 1351, outer plugging portion 1352, anhydrous hydrogen fluoride feed end 20, thionyl chloride feed end 30, discharge end 40, middle material distribution structure 50, first sealing crank sleeve 51, upper outer sealing sleeve 511, upper inner sealing sleeve arc sleeve 512, opposite column pipe 513, second sealing crank sleeve 52, lower outer sealing sleeve 521, lower inner sealing arc sleeve 522, opposite empty cylinder 523, driving member 53, dynamic material distribution member 54, revolving ring 541, upper mixing section 542, axial column 5421, dispersion sheet 5422, gasket 5423, lower mixing section 543, axial Material distribution structure 60, mounting groove 61, built-in cavity 611, external expansion groove 612, external spring piece 613, static material distribution member 62, clamping ring 621, expansion pad 622, spiral piece 623, preheating tank body 1, crude gas inlet 101, crude gas outlet 102, serpentine coil 103, upper through portion 1031, transverse transmission portion 1032, bending portion 1033, lower through portion 1034, internal circulation contact structure 2, internal contact member 201, internal air inlet portion 2011, internal air outlet portion 2012, internal barrier portion 2013, internal through pipe 20131, barbed pipe 20132, hollow member 202, small sleeve 2021, large sleeve 2022, holding bag 2023, external contact member 203, external transverse pipe 2031, external discharge hole 2032, lower guide portion 2033 , steam inlet pipe 204, lower isolation structure 3, inner heat shield 301, long cone 3011, short cone 3012, outer isolation cover 302, separation cover 3021, isolation felt 3022, circulation rack 303, retaining rack 3031, connecting rod 3032, inlet pipe 4, outflow pipe 5, distillation column 90, top tray 911, matching screw seat 9111, inlet end 93, packing mounting structure 95, middle matching piece 951, lower screw segment 9511, connecting shaft 9512, circular mounting cylinder 952, hollow ring 9521, recessed area 953, clamping piece 954, guide clamp 9541, clamping arm 9542, straight arm portion 95421, fan-shaped seat 95422, pressing plate 9543, mounting plate surface 95431, pressing pad 95432 , outward expansion rod 961, outward swing plate 9611, outward push piece 962, outward push portion 9621, guide inclined surface 9622, spring 9623, sealing piece 963, inner arc plate 9631, abutment ring 9632, vaporizer 80, thionyl fluoride liquid inlet 81, thionyl fluoride gas outlet 82, steam pipe 83, isolation and distribution structure 84, middle mounting plate 841, distribution pipe 842, upper separation section 8421, bending pipe 8422, lower separation section 8423, lower distribution assembly 843, back pressure piece 8431, circumferential shaft 84311, torsion spring 84312, folding plate 84313, sealing arc pad 84314, total lifter 8432, hanging bracket 84321, lower punch 84322, auxiliary pipe 84323, lower extraction pipe 844,Segmented vaporization structure 85, accommodating chamber 851, inner inclined hole 831, outer guide plate 853, inner guide assembly 854, adsorption pad 8541, lower inclined tube 8542, inner ring 8543, outer guide assembly 855, receiving sleeve 8551, lower curved tube 8552, outer ring 8553, linkage tube 856. DETAILED DESCRIPTION

[0063] All embodiments of the present invention are within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the present invention. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0064] In the description of the present invention, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as referring to the purpose, technical solutions and advantages of the methods. To be clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work indicate or imply relative importance or implicitly indicate the number of indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "multiple" is two or more, unless otherwise clearly and specifically defined.

[0065] Reference Figures 1 to 26 As shown, a preparation equipment for preparing high-purity electronic-grade thionyl fluoride includes: a mixer, the mixer is communicated with a first preheating device, the first preheating device is communicated with a first distillation tower, the top of the distillation tower is connected to a condenser, the condenser is communicated with a crude product tank, the crude product tank is communicated with a second preheating device, the second preheating device is communicated with a second distillation tower, the second distillation tower is communicated with a third distillation tower, the third distillation tower is connected to a storage tank, the storage tank is connected to a vaporization device, the vaporization device is connected to a high-pressure buffer tank, the high-pressure buffer tank is connected to at least three adsorption towers, and the adsorption tower at the rear end is connected to a high-pressure product tank.

[0066] The mixer of this embodiment includes a mixing tube 10 for mixing, wherein the mixing tube 10 is respectively provided with an anhydrous hydrogen fluoride feed end 20 and a thionyl chloride feed end 30, and the mixing tube 10 is provided with a discharge end 40 at one end away from the thionyl chloride feed end 30, and further includes: a middle material division structure 50, wherein the mixing tube 10 includes a front section branch pipe 11 provided with an anhydrous hydrogen fluoride feed end 20 and a thionyl chloride feed end 30 and a rear section segment 12 provided with the discharge end 40, the middle position of the front section branch pipe 11 and the rear section segment 12 are connected by a cross-connecting plate 13, the middle material division structure 50 includes a first sealing crank sleeve 51 provided at the upper end of the cross-connecting plate 13, the lower end of the cross-connecting plate 13 is connected to a second sealing crank sleeve 52, the first sealing crank sleeve 51 A driving member 53 is provided on the side away from the cross-connecting plate 13, and the output end of the driving member 53 is connected to a dynamic material dividing member 54 that penetrates the cross-connecting plate 13 and is located in the first sealing crank sleeve 51 and the second sealing crank sleeve 52; an axial material dividing structure 60, the front section branch pipe 11 and the rear section segment 12 are provided with a mounting groove 61 on one side close to the cross-connecting plate 13, and a static material dividing member 62 is movably provided in the mounting groove 61, the first sealing crank sleeve 51 and the second sealing crank sleeve 52 are connected to the rear sides of the cross-connecting plate 13 and respectively abut against the two static material dividing members 62, and the raw materials entering through the anhydrous hydrogen fluoride feed end 20 and the thionyl chloride feed end 30 are divided by the static material dividing member 62 at the front end, mixed by the dynamic material dividing member 54, and then divided by the static material dividing member 62 at the rear end.

[0067] Whether it is a static mixer or a dynamic mixer used in the prior art, the coating needs to be regenerated after a period of use. When the coating is regenerated, the entire mixer needs to be removed from the pipeline and then immersed in the coating, which is not only time-consuming and labor-intensive, but also the connected pipeline needs to be repeatedly tested before it can be used. Therefore, the present invention sets a middle dividing structure 50, firstly divides the entire mixer into two parts, namely the front section branch pipe 11 and the rear section 12, and sets a middle dividing structure 50 between the two parts, which can not only achieve the dynamic mixing effect in the middle through the dynamic dividing piece 54, but also the entire mixer can be disassembled at this time, and the regeneration of the mixing structure can be carried out directly in the middle position, thereby effectively maintaining a good dispersion effect of the dynamic mixing effect of the mixer, thereby improving the mixing effect of anhydrous hydrogen fluoride and thionyl chloride.

[0068] If the front branch pipe 11 and the rear section 12 are set as two separate parts, it will be difficult to connect the two sections of the pipeline regardless of the gluing or welding stage. Therefore, the cross-connecting plate 13 of this embodiment includes two connecting arc plates 131 connected between the front branch pipe 11 and the rear section 12, and a cross-connecting plate 132 is connected between the two connecting arc plates 131. The cross-connecting plate 132 is provided with a pair of through holes 133, and a sealing member 135 is locked on the pair of through holes 133. By setting the cross-connecting plate 13 between the front branch pipe 11 and the rear section 12, the two pipelines are connected through the cross-connecting plate 13, and there are connecting surfaces on the side and the middle, so that although the two parts of the structure are set separately, they have a certain connection, so that they can be more stable when the sealing structure is formed again.

[0069] Due to the setting of the cross-connecting plate 13, the middle material distribution structure 50 needs to be divided into two upper and lower sealing settings, and the two parts have different structures. Specifically: first, there is a second sealing crank sleeve 52 at the lower end, and the second sealing crank sleeve 52 includes a lower outer sealing sleeve 521 that fits with the lower end of the connecting arc plate 131, and the inner side of the lower outer sealing sleeve 521 is connected to the lower inner sealing arc sleeve 522 that fits with the inner wall of the connecting arc plate 131, and the lower inner sealing arc sleeve 522 is provided with a facing empty cylinder 523. The lateral opening of the facing empty cylinder 523 has a lower outer sealing sleeve 521 and a lower inner sealing arc sleeve 522 that fit with the connecting arc plate 131, thereby reducing the difficulty of sealing. The first sealing crank sleeve 51 at the upper end also includes an upper outer sealing sleeve 511 and an upper inner sealing sleeve arc sleeve 512 that cooperate with the connecting arc plate 131, but the second sealing crank sleeve 52 and the first sealing crank sleeve 51 The difference is that the second sealing crank sleeve 52 is provided with a facing empty cylinder 523, while the first sealing crank sleeve 51 is provided with a facing column tube 513. The first sealing crank sleeve 51 includes an upper outer sealing sleeve 511 that is in contact with the upper end of the connecting arc plate 131. The inner side of the upper outer sealing sleeve 511 is connected to the upper inner sealing sleeve arc sleeve 512 that is in contact with the inner side wall of the connecting arc plate 131. The lower end of the upper inner sealing sleeve arc sleeve 512 is provided with a facing column tube 513. The lateral opening of the facing column tube 513, when the first sealing crank sleeve 51 and the second sealing crank sleeve 52 are matched, the facing column tube 513 is embedded in the facing empty cylinder 523 through the through-hole 133, and the facing column tube 513 and the facing empty cylinder 523 are connected through the through-hole 133 via the blocking piece 135, so that the two can form a rapid point-to-point connection, thereby ensuring that a relatively complete circular structure can be formed.

[0070] After the second sealed crank sleeve 52 and the first sealed crank sleeve 51 form a circular structure, in order to ensure a stable fit between the two structures, the transverse connecting plate 132 of this embodiment is provided with a transverse threaded hole in the transverse direction corresponding to the position of the through hole 133, and the blocking piece 135 includes a stud portion 1351 that passes through the opposing column tube 513 and the opposing empty cylinder 523 and cooperates with the transverse threaded hole. The stud portion 1351 is provided with an external blocking portion 1352, and the external blocking portion 1352 closes the through hole 133. By providing a transverse threaded hole on the transverse connecting plate 132, a foundation is laid for cooperation with the blocking piece 135, so that the stud portion 1351 can pass through the opposing column tube 513 and the opposing empty cylinder 523, allowing the second sealed crank sleeve 52 and the first sealed crank sleeve 51 to form a whole, reducing the difficulty of subsequent gluing or welding.

[0071] The dynamic mixing stage of the entire mixer occurs at the position of the transverse connecting plate 132. Therefore, after the second sealed crank sleeve 52 and the first sealed crank sleeve 51 form a whole, the entire dynamic material distribution component 54 is also installed. Specifically, a rotating interface 1321 is provided in the middle of the transverse connecting plate 132. The dynamic material distribution component 54 includes a revolving ring 541 arranged in the rotating interface 1321. The top of the revolving ring 541 is provided with an upper mixing part 542. The lower end of the revolving ring 541 is connected to a lower mixing part 543. The upper mixing part 542 is connected to the output end of the driving member 53. The dynamic material distribution component 54 is divided into an upper mixing part 542 and a lower mixing part 543, so that the effect of dynamic uniform mixing can be achieved in two different areas, and can be regenerated as the second sealed crank sleeve 52 and the first sealed crank sleeve 51 are disassembled.

[0072] When the upper mixing section 542 mixes the raw materials, the upper mixing section 542 and the lower mixing section 543 have the same structure and size. The upper mixing section 542 includes a central column 5421 connected to the revolving ring 541. The central column 5421 is connected to the driving member 53. A semi-arc-shaped dispersion sheet 5422 is provided on the central column 5421. A plurality of dispersion holes are opened on the dispersion sheet 5422. The raw materials are dispersed through the small chambers formed by the plurality of dispersion sheets 5422, and then dispersedly disrupted and mixed, thereby achieving an efficient mixing effect. The entire process is in a high-speed operation state, thereby ensuring the uniformity of mixing.

[0073] In order to avoid friction when the dispersion piece 5422 cooperates with the inner wall of the pipe, a gasket 5423 is provided on the outer side of the dispersion piece 5422 , and the gasket 5423 is attached to the inner side of the first sealing crank sleeve 51 .

[0074] Although the dynamic material dividing member 54 is directly installed on the middle material dividing structure 50 to achieve its external detachable regeneration effect, the static mixing structure in the front section branch pipe 11 and the rear section 12 is also difficult to regenerate. Therefore, the present invention provides an axial material dividing structure 60 on the basis of the middle material dividing structure 50, and directly provides two static material dividing members 62 on the side positions of the first sealing crank sleeve 51 and the second sealing crank sleeve 52, so that the two static material dividing members 62 can be directly exposed after the first sealing crank sleeve 51 and the second sealing crank sleeve 52 are removed, so that the coating on the static material dividing member 62 can be directly regenerated from the outside, thereby achieving the regeneration effect of the static and dynamic mixing members without the need for tedious operations, thereby maintaining the mixing effect of the mixer for a long time.

[0075] If the static material part 62 is set at the inner side, it is difficult to infiltrate or spray during the coating regeneration. Therefore, the mounting groove 61 of this embodiment includes an inner cavity 611, and a plurality of outward expansion grooves 612 are provided on the inner side of the inner cavity 611. The outer edge of the outward expansion groove 612 is provided with an outer spring piece 613. After the static material part 62 opens the outer spring piece 613, it is clamped into the inner cavity 611 and the outward expansion groove 612. The static material part 62 includes a clamping ring 621 that cooperates with the inner cavity 611. A plurality of outward expansion pads 622 are provided on the outer side of the clamping ring 621. A spiral sheet 623 is provided on the inner side of 21, and the outer edge of the clamping ring 621 is fitted on the outer side of the first sealing crank sleeve 51 and the second sealing crank sleeve 52. The static material part 62 is fixed on the inner side of the mounting groove 61, and the clamping ring 621 and the outward expansion pad 622 of the static material part 62 are matched with the outer spring piece 613 and the outward expansion groove 612, thereby forming self-fixation, and then the clamping ring 621 on the static material part 62 is squeezed on the side of the middle material part structure 50, so that the static material part 62 is close to the middle material part structure 50 and can achieve the effect of static mixing.

[0076] The first preheating device of this embodiment is the same as the second preheating device. The first preheating device includes: a preheating tank body 1, the upper end of the preheating tank body 1 is connected to a crude gas inlet 101, the lower end of the preheating tank body 1 is connected to a crude gas outlet 102, at least one serpentine coil 103 is connected between the crude gas inlet 101 and the crude gas outlet 102, the preheating tank body 1 is provided with an inlet pipe 4 and an outlet pipe 5, and further includes: an internal circulation contact structure 2, the serpentine coil 1 03 includes an upper through portion 1031 connected to the crude gas inlet 101, the upper through portion 1031 is connected to a horizontal transmission portion 1032, the end of the horizontal transmission portion 1032 is connected to a bending portion 1033, the horizontal transmission portions 1032 and the bending portions 1033 are alternately arranged, and the lowest end of the horizontal transmission portion 1032 is connected to a lower through portion 1034 communicating with the crude gas outlet 102, and the internal circulation contact type structure 2 includes an internal contact member arranged inside the bending portion 1033 201, a hollow member 202 is provided on the outside of the inner contact member 201, and an outer contact member 203 is connected to the side of the inner contact member 201 close to the horizontal transmission part 1032. The outer contact member 203 is located between the two horizontal transmission parts 1032. The inner contact member 201 and the outer contact member 203 are both connected to the steam inlet pipe 204. The steam inlet pipe 204 is located on the outside of the preheating tank body 1. The steam entering through the steam inlet pipe 204 is discharged from the inner contact member 201. After being output from the external contact piece 203, the condensed steam falls to the bottom of the preheating tank body 1; the lower isolation structure 3 includes an inner heat cover 301 arranged at the lower end of the lower through-portion 1034, and an outer isolation cover 302 is arranged on the outer side of the inner heat cover 301, and a circulation rack 303 is arranged on the outer side of the outer isolation cover 302. The outer side of the circulation rack 303 is fixed to the inner side of the preheating tank body 1 and communicates with the outside. The condensed steam falls to the bottom of the preheating tank body 1 after being guided by the outer isolation cover 302.

[0077] In the preheating stage, the crude gas of thionyl fluoride is introduced into the crude gas inlet 101 , and the crude gas is allowed to enter different serpentine coils 103 , and hot steam is introduced into the inlet pipe 4 of the preheating tank 1 .

[0078] In the prior art, during the preheating stage of the crude thionyl fluoride gas, hot steam is introduced into the serpentine coil 103, and then the gas is introduced into the equipment to contact the serpentine coil 103 with a certain temperature, thereby increasing the temperature of the crude gas to meet the distillation conditions. However, the amount of gas that can be introduced in this way is not proportional to the contact area of ​​the heat medium, resulting in some gas passing out of the equipment before being cooled to a suitable temperature, affecting the distillation effect. Therefore, the present invention provides an internal circulation contact structure 2 to directly introduce the crude thionyl fluoride gas into the serpentine coil 103, and through the internal contact member 201, the external contact member 203 and the preheating tank body 1 itself, it can complete all-round contact with the serpentine coil 103, so that the crude gas in the serpentine coil 103 can be uniformly preheated, and its temperature can be raised to 50-100°C, thereby ensuring that the gas entering the distillation system can always maintain a suitable temperature.

[0079] The flow rate of the crude gas at the transverse transmission portion 1032 and the bend portion 1033 is different, which easily leads to uneven preheating at each position. In order to balance the flow rate at each position and ensure that the gas is always kept at an appropriate temperature, the inner and outer sides of the bend portion 1033 of this embodiment are both opened. The inner contact member 201 includes an inner air inlet portion 2011 embedded in the outer opening of the bend portion 1033, and the inner opening of the bend portion 1033 is provided with an inner air outlet portion 2012. An internal barrier portion 2013 is connected between the internal air inlet portion 2011 and the internal air outlet portion 2012. The internal air inlet portion 2011 is connected to the steam inlet pipe 204. The internal contact member 201 is arranged on the inner side of the bent portion 1033, and the internal barrier portion 2013 forms an obstruction in the bent portion 1033, so that the rough gas passing through this place can be heated by the inner side, thereby reducing the flow rate of the gas, and then balancing the problem of excessive transmission of the horizontal transmission portion 1032 at the front end.

[0080] In order to ensure the covering effect, all the inner blocking portions 2013 form a fan-shaped structure, so as to form a relatively complete coverage area inside the bent portion 1033 .

[0081] In order to cover more areas and fully improve the heat exchange effect, the internal barrier part 2013 includes an internal tube 20131 connected between the internal air inlet part 2011 and the internal air outlet part 2012. A plurality of barbed tubes 20132 extend outward from the circumferential outside of the internal tube 20131, so that the gap in the internal tube 20131 can also be closed by the barbed tubes 20132.

[0082] Although the internal contact piece 201 can heat the coarse air from the inside, this also leads to a problem, that is, the coarse air can easily leak from the inner air inlet 2011 and the inner air outlet 2012 of the inner barrier part 2013. Therefore, the hollow piece 202 of this embodiment includes a small sleeve 2021 nested on the outside of the inner air outlet 2012, and a large sleeve 2022 is nested on the outside of the inner air outlet 2012. A holding bag 2023 is connected between the small sleeve 2021 and the large sleeve 2022, and is ringed on the outside of the bending part 1033. The holding bag 2023 is hollow. By arranging the hollow piece 202 at the inner air inlet 2011 and the inner air outlet 2012, the two sleeves of the hollow piece 202 wrap the entire internal heating structure in a chamber, so that even if leakage occurs, there will be a time of saturation. Once saturated, it can continue to flow forward without affecting the overall use.

[0083] Since multiple serpentine coils 103 are used, the spacing between each transverse transfer part 1032 is small, so the heat transfer effect between each transverse transfer part 1032 is not good. Therefore, the external contact piece 203 of this embodiment includes an outer transverse tube 2031 connected to the steam inlet pipe 204. The outer transverse tube 2031 is provided with an outer discharge hole 2032 near the transverse transfer part 1032. Through the provided external contact piece 203, the pipeline is extended to the transverse transfer part 1032, so that the heat medium can be directly extended to the position of the transverse transfer part 1032, thereby ensuring temperature consistency even in a relatively narrow position.

[0084] In order to avoid turbulence at the far end of the outer transverse tube 2031, a lower guide portion 2033 is provided on the side of the outer transverse tube 2031 close to the inner contact piece 201. The steam can be discharged directly from the lower guide portion 2033 to avoid the formation of internal turbulence and allow the steam to flow out more smoothly.

[0085] By adopting an external heat medium, the heat medium will condense into liquid and fall after preheating. If this part is directly deposited at the bottom of the preheating tank body 1, it will significantly affect the temperature of the bottom serpentine coil 103. Therefore, the present invention provides a lower isolation structure 3 on the basis of the internal circulation contact structure 2, extending the bottom of the entire preheating tank body 1, and wrapping the preheated raw gas in the inner heat cover 301. The inner heat cover 301 is isolated from the outside by the outer isolation cover 302, and all the condensed water is passed to the bottom of the preheating tank body 1 for rapid discharge, so that the condensed water can be discharged smoothly while avoiding affecting the temperature of the raw gas in the serpentine coil 103.

[0086] In order to prevent condensed water from accumulating at the position of the serpentine coil 103, it is necessary to drain the condensed water quickly, and the discharged condensed water must not affect the preheated raw air. Therefore, the inner heat cover 301 of this embodiment includes a long cone 3011 connected to the lower through portion 1034, and the lower end of the long cone 3011 is connected to a short cone 3012. The long cone 3011 is spaced apart from the inner wall of the preheating tank 1, and the inner heat cover 301 is configured as a structure that is long at the top and short at the bottom. Through the configuration of the long cone 3011 and the short cone 3012, the condensed water can be drained away with the largest taper while completely isolating the raw air from the influence of the external temperature, thereby ensuring that the raw air temperature inside is always within the required range.

[0087] In this embodiment, the first distillation tower, the second distillation tower, and the third distillation tower have the same structure and size. The first distillation tower, the second distillation tower, and the third distillation tower constitute a purification system. The purification system includes: at least one distillation tower 90, the upper end of the distillation tower 90 is connected to a condenser, the lower end of the distillation tower 90 is connected to a reboiler, and one side of the distillation tower 90 is provided with an air inlet end 93. It also includes: a packing installation structure 95, the inner side of the distillation tower 90 is provided with a top tray 911, and the packing installation structure 95 includes a packing material that is locked on the top tray 911. The middle fitting 951 on the distillation tower 90 is provided with a plurality of circular mounting cylinders 952, the inner side of which is provided with a filler, and the inner side of which is provided with a recessed area 953. The recessed area 953 forms a closed space with the inner wall of the distillation tower 90, and the inner side of the recessed area 953 is provided with a clamping member 954. The clamping member 954 abuts against the inner wall of the distillation tower 90. After the middle fitting 951 is fixed, the plurality of circular mounting cylinders 952 are sequentially installed on the middle fitting 951. 51; the pressurized closed structure includes an outward expansion rod 961 movably mounted on the inner wall of the middle matching piece 951, and the inner side of the clamping piece 954 is movably provided with an outward push piece 962, and the outward push piece 962 is movably matched with the middle matching piece 951. In the process of limiting the circular mounting cylinder 952 by the clamping piece 954, it is necessary to set a limiting structure for the circular mounting cylinder 952 in the recessed area 953. Therefore, the clamping piece 954 of this embodiment includes a guide cartridge 9541 provided in the recessed area 953, and the guide cartridge 954 1 is movably mounted on the inner side of the clamping arm 9542. A clamping plate 9543 is connected to the side of the clamping arm 9542 away from the middle fitting 951. The circular mounting cylinder 952 is supported by the clamping arm 9542 and the clamping plate 9543 through the guide cartridge 9541 disposed in the recessed area 953. The circular mounting cylinder 952 is then restricted to a desired height, thereby forming an intermittent gas filtering effect. The stabilization process is very stable.

[0088] After the outward expansion rod 961 is embedded in the middle fitting 951, the outward pushing member 962 is pushed outward and the clamping member 954 is abutted against the inner wall of the distillation tower 90. A sealing member 963 is provided on the outer periphery of the clamping plate 9543. The sealing member 963 is tightly attached to the inner wall of the distillation tower 90 as the clamping member 954 moves.

[0089] During the purification process of thionyl fluoride, the gas to be purified is fed into the distillation tower 90 through the lateral gas inlet 93 , and the gas gradually passes through the circular mounting cylinder 952 , contacts the packing in the circular mounting cylinder 952 , and is then recycled at the condenser and reboiler.

[0090] The removable packing in the distillation tower 90 in the prior art is difficult to perfectly match with the tower body, which makes it easy for gaps to appear between the packing and the tower body, so that some gas will pass directly through the packing area along the edge seam and leak through the packing, causing some untreated packing to flow directly into the tower bottom or the top of the tower, making it difficult to purify the distillation product. Therefore, the present invention adopts a unified middle fitting 951 through the packing mounting structure 95 set up, and all the circular mounting cylinders 952 are uniformly installed on the middle fitting 951, which can reduce the inner diameter of the circular mounting cylinder 952, and then the circular mounting cylinder 952 is fixed to the inner side of the distillation tower 90 by the fixing method of the clamp 954, so that the circular mounting cylinder 952 can be firmly fixed to the distillation tower 90 while being detachable.

[0091] The circular mounting cylinder 952 is filled with fillers, and the gas needs to pass through the fillers in order to better separate the substances. Therefore, the circular mounting cylinder 952 in the present invention is an I-shaped structure, and the middle part of the circular mounting cylinder 952 is a hollow ring 9521. The bottom and top surfaces of the circular mounting cylinder 952 are both mesh plates, and the outer peripheral surfaces of the circular mounting cylinder 952 are both closed surfaces. The upper and lower ends of the circular mounting cylinder 952 are both in the state of mesh plates. In order to prevent the gas from leaking from the side position, the outer peripheral surface of the circular mounting cylinder 952 is set to a closed surface, thereby closing the side area, laying the foundation for the formation of the recessed area 953.

[0092] The entire middle fitting part 951 can be taken out together with the circular mounting tube 952, so that all the circular mounting tubes 952 can be quickly taken out together. Therefore, the bottom surface of the inner side of the top tray 911 of this embodiment is provided with a mating screw seat 9111, and the bottom of the middle fitting part 951 is a lower screw section 9511, and the lower screw section 9511 is threadedly connected in the mating screw seat 9111. The bottom of the middle fitting part 951 is set as the lower screw section 9511, so that the middle fitting part 951 can be matched with the mating screw seat 9111, and the middle fitting part 951 can be temporarily fixed and detachable.

[0093] The middle fitting part 951 not only serves as a hollow ring 9521 for limiting and fixing the circular mounting cylinder 952, but is also a container. Therefore, the middle fitting part 951 of this embodiment includes a connecting shaft 9512 that cooperates with the mating screw seat 9111. The interior of the connecting shaft 9512 is hollow, and the interior of the connecting shaft 9512 is provided with a number of through cavities for installing the outward push piece 962. The bottom of the connecting shaft 9512 is connected to the lower screw section 9511. By hollowing out the inner side of the connecting shaft 9512, it can cooperate with the outward expansion rod 961 in the pressurized closed structure, thereby making the cooperation between the connecting shaft 9512 and the clamping part 954 more practical.

[0094] When the tensioning arm 9542 cooperates with the inner wall of the distillation tower 90, the tensioning arm 9542 includes a straight arm portion 95421 that cooperates with the guide cartridge 9541. The straight arm portion 95421 is movably connected to the push piece 962. The side of the straight arm portion 95421 away from the guide cartridge 9541 is connected to a fan-shaped seat 95422. The clamping plate 9543 is locked on the fan-shaped seat 95422. First, the fan-shaped seat 95422 is driven by the movement of the straight arm portion 95421, and then the fan-shaped seat 95422 and the inner wall of the distillation tower 90 form abutment effect to allow the straight arm portion 95421 to support the circular mounting cylinder 952, thereby forming a middle lifting effect. Even if a high oscillation effect is formed when high-pressure gas is introduced, no deviation will occur.

[0095] In order to allow the clamping plate 9543 to better fit with the inner wall of the distillation tower 90, the clamping plate 9543 includes a mounting plate surface 95431 connected to the fan-shaped seat 95422, and a plurality of clamping pads 95432 are provided on the side of the mounting plate surface 95431 close to the inner wall of the distillation tower 90. The degree of deformation of the clamping pad 95432 is proportional to the degree of force applied to the clamping member 954, and when the degree of deformation of the clamping pad 95432 is large, it indicates that the circular mounting cylinder 952 is more stable.

[0096] Although reducing the inner diameter of the circular mounting cylinder 952 and providing the clamping member 954 can make the installation of the circular mounting cylinder 952 stable, it is still difficult to prevent the gas in the outer circumference from moving to the upper and lower ends without being filtered by the packing. Therefore, the present invention provides a pressurized closed structure based on the packing mounting structure 95, which not only makes the cooperation between the circular mounting cylinder 952 and the distillation tower 90 more stable, but also can seal the gap between the circular mounting cylinder 952 and the distillation tower 90 through the sealing member 963, thereby preventing the gas from leaking from the outer edge of the circular mounting cylinder 952, so that the gas moved to the bottom of the tower and the top of the tower can meet the conditions better.

[0097] Since the circular mounting cylinder 952 at the bottom is the first to come into contact with the gas, the gas pressure at this time is relatively large, and the pressure exerted on the circular mounting cylinder 952 is relatively large, so the external mounting force exerted on the circular mounting cylinder 952 at the bottom should also be the largest. Therefore, the bottom of the outward expansion rod 961 of this embodiment is screwed to the bottom inside the middle matching piece 951, and a plurality of outward swing plates 9611 are provided on the outside of the outward expansion rod 961. The length of the outward swing plates 9611 gradually increases from top to bottom, and the outward push piece 962 includes an outward push portion 9621 corresponding to the clamping piece 954. The outward push portion 9621 is provided with a guide slope 9622 on the side away from the clamping piece 954. Different The inclination of the guiding slope 9622 is different. The guiding slope 9622 can extend into the through cavity of the connecting shaft 9512. The outward pushing portion 9621 is connected to the clamping member 954 by a connecting spring 9623. The inclination of the guiding slope 9622 in the movable outward pushing member 962 is set to be different, and the outer swing plate 9611 on the outer side of the outward expansion rod 961 is set to be of different lengths, so that after the outward expansion rod 961 is matched with the middle matching member 951, the support force of the circular mounting cylinder 952 closer to the bottom can be more stable, and the setting of the connecting spring 9623 can retract the outward pushing portion 9621 into the guide clamping cylinder 9541 at an appropriate time, so that the middle matching member 951 can be removed.

[0098] The outer expansion rod 961 and the middle matching piece 951 are also movable and disassembled, thus forming a two-stage disassembly, which makes the replacement of the filler easy without affecting the overall use.

[0099] The closer the circular mounting cylinder 952 is to the bottom, the easier it is for the gas to flow out from the side. Therefore, the sealing member 963 of this embodiment includes an inner arc plate 9631 connected to the inner side of the mounting plate surface 95431. The top edge of the inner arc plate 9631 is connected to an abutment ring 9632. The abutment ring 9632 fits against the inner wall of the distillation tower 90, connecting the inner arc plate 9631 of the sealing member 963 to the mounting plate surface 95431. The sealing member 963 is pushed out through the mounting plate surface 95431, and is closer to the inner wall of the distillation tower 90, thereby improving the sealing effect with depth, thereby avoiding gas leakage from the side.

[0100] The vaporization device of this embodiment includes: a vaporization tank 80, a thionyl fluoride liquid inlet 81 is provided at the bottom of the vaporization tank 80, a thionyl fluoride gas outlet 82 is provided at the top of the vaporization tank 80, a plurality of steam pipes 83 are provided in the vaporization tank 80, and the steam pipes 83 are connected to the external air inlet and outlet ends. It also includes: an isolation and distribution structure 84, including a middle mounting plate 841 provided in the middle section of the vaporization tank 80, the middle mounting plate 841 divides the vaporization tank 80 into a vaporization area and a distribution area, a plurality of distribution pipes 842 are connected to the lower end of the middle mounting plate 841, a lower distribution assembly 843 is provided on the outer side of the middle of the distribution pipe 842, and the lower distribution assembly 843 controls the opening and closing of all the distribution pipes 842, and the bottom of the distribution pipe 842 is connected to the lower extraction pipe 844. 4 extends into the thionyl fluoride liquid at the bottom of the vaporizer 80, and the lower distribution component 843 periodically draws the thionyl fluoride liquid at the bottom of the vaporizer 80 into the distribution pipe 842 through the lower suction pipe 844; the segmented vaporization structure 85 includes a plurality of accommodating chambers 851 arranged on the middle mounting plate 841, the inlet holes at the bottom of the accommodating chambers 851 are connected to the distribution pipe 842, the steam pipe 83 is inserted above the accommodating chamber 851, and an inner inclined hole 831 is provided in the middle of the steam pipe 83, and an outer guide plate 853 is inclined outwardly from the inner inclined hole 831. An inner guide component 854 is provided on the inner side of the outer guide plate 853 at a position corresponding to the inner inclined hole 831, and an outer guide component 855 is provided on the outer side of the outer guide plate 853. The inner guide component 854 and the outer guide component 855 are both connected to the external exhaust structure.

[0101] During vaporization, thionyl fluoride liquid is fed into the vaporizer 80 through the thionyl fluoride liquid inlet 81 and gradually divided by the isolation and distribution structure 84. The distribution speed is connected to the feed speed, thereby achieving the purpose of continuous production. The divided thionyl fluoride liquid is transported to the segmented vaporization structure 85 to be vaporized into thionyl fluoride gas and output from the thionyl fluoride gas outlet 82.

[0102] In the prior art, in the process of vaporizing some corrosive gases, a steam pipe is inserted into the liquid, and the liquid is vaporized through the contact between the liquid and the steam pipe. However, this vaporization method is used for the liquid in the entire chamber when vaporizing the liquid, and its vaporization effect is poor, and the rate of gas precipitation is slow. Therefore, the present invention sets an isolation and distribution structure 84, and the purified liquid will accumulate at the bottom of the vaporization tank 80. The liquid is gradually pumped to the position of the vaporization zone through the lower distribution component 843 through the lower suction pipe 844. Moreover, the extraction adopts periodic extraction, that is, new liquid is extracted after the extracted liquid is vaporized, so as to achieve a continuous, small-volume, and stable vaporization effect. Compared with the traditional vaporization furnace, the vaporization effect is good and the vaporization rate is also higher.

[0103] When extracting the liquid at the bottom of the vaporizer 80 through the distribution pipe 842, if a single-strand, linear extraction is adopted, it is difficult to control the feeding intermittently. Therefore, the distribution pipe 842 of this embodiment includes an upper separation section 8421 connected to the accommodating chamber 851, and the upper separation section 8421 is connected to a bent tube 8422 inclined toward the center line of the vaporizer 80, and the lower end of the bent tube 8422 is connected to a lower separation section 8423, and the lower separation section 8423 is connected to the lower suction pipe 844. By dividing the distribution pipe 842 into sections, a bent tube 8422 is provided on each section of the distribution pipe 842, so that the lower distribution assembly 843 can be provided at the position of the bent tube 8422, thereby better controlling the feeding state of the distribution pipe 842.

[0104] A separate liquid extraction control structure needs to be set at the position of each distribution pipe 842 so as to control the liquid state of each accommodating chamber 851 accordingly. Therefore, the lower distribution component 843 of this embodiment includes a back-pressure piece 8431 arranged in the middle of the inner part of the bending tube 8422, and the lower end of the middle mounting plate 841 is provided with a total feeder 8432, and the total feeder 8432 is connected to the upper half of the bending tube 8422. By providing a back-pressure piece 8431 inside each distribution pipe 842, the back-pressure piece 8431 will only open and close according to the total feeder 8432, and will close the inner side of the distribution pipe 842 under normal conditions, thereby avoiding passive feeding of the distribution pipe 842, thereby being able to control the feeding amount of the distribution pipe 842.

[0105] The counter-pressure member 8431 in this embodiment includes a circumferential shaft 84311 that passes through the bending tube 8422, and one end of the circumferential shaft 84311 is sleeved with a torsion spring 84312, and the part of the circumferential shaft 84311 located in the bending tube 8422 is provided with a folding plate 84313, and sealing arc pads 84314 are fixed at both ends of the bending tube 8422. By using the folding plate 84313 that can only be flipped on one side, it is achieved that only the total feeder 8432 can be opened and closed, and once the total feeder 8432 is closed, it is directly reset.

[0106] It is not only difficult to set up a separate control structure on each distribution pipe 842, but also very costly. Therefore, the total material starter 8432 of this embodiment includes a hanger 84321 locked at the lower end of the middle mounting plate 841, and a lower punch 84322 is locked below the hanger 84321. The lower punch 84322 is connected to the inert gas inlet, and the lower punch 84322 is connected to the upper half of the bending pipe 8422 through a sub-pipe 84323. The total material starter 8432 needs to control all the distribution pipes 842 at the same time, so that it is punched into the bending pipe 8422 through different sub-pipes 84323 through a lower punch 84322 with a positive pressure function, so that the open and closed states of different bending pipes 8422 can be controlled, thereby realizing the state of multiple pipes being opened or closed at the same time.

[0107] During segmented vaporization, the steam pipe 83 is inserted into the accommodating chamber 851, and the hot steam in the steam pipe 83 vaporizes the liquid in the accommodating chamber 851. However, during the vaporization process, condensation is likely to occur both inside and outside the steam pipe 83. The condensed water on the outside is likely to affect the purity of thionyl fluoride, while the condensed water on the inside will affect the temperature of the steam. Therefore, the present invention provides a segmented vaporization structure 85, and respectively provides an inner guide component 854 and an outer guide component 855 on the inner and outer sides of the segmented vaporization structure 85. The inner guide component 854 and the outer guide component 855 can respectively guide the condensed water inside and outside to the outside, thereby making the vaporization process smoother and the purity of the vaporized thionyl fluoride higher.

[0108] On the inner side of the steam pipe 83, the condensed liquid generated inside the steam pipe 83 needs to be discharged to avoid lowering the temperature inside the steam pipe 83. Therefore, the inner guide component 854 of this embodiment includes an adsorption pad 8541 arranged on the inner inclined hole 831, and the lower end of the adsorption pad 8541 is connected to a lower inclined tube 8542. All the lower inclined tubes 8542 are connected through an inner ring 8543. By arranging the adsorption pad 8541 in the inner guide component 854, the aperture of the adsorption pad 8541 is extremely small. Although some gas will be exposed, the condensed liquid droplets flowing down will infiltrate from the position of the adsorption pad 8541, and will not flow to the lower end, thereby avoiding affecting the temperature of the steam inside the steam pipe 83.

[0109] In order to further suppress the diffusion effect of the gas, the downward inclined tube 8542 of this embodiment is filled with a barrier mass, which can limit the flow of gas and ensure that the hot steam does not flow to the outside in large quantities.

[0110] On the outside of the steam pipe 83, in order to prevent the condensed water on the outside from flowing down and coming into contact with the liquid at the bottom, thereby reducing the purity of the liquid at the bottom, the outer guide component 855 of this embodiment includes a receiving sleeve 8551 arranged below the outer guide plate 853, and the receiving sleeve 8551 is connected to a lower bend pipe 8552, and all the lower bend pipes 8552 are connected to an outer ring 8553. The outer guide component 855 is drained into the receiving sleeve 8551 through the outer guide plate 853, and is collected and concentrated at the position of the outer ring 8553 through the receiving sleeve 8551, so that the condensed water on the outside can also be concentrated and guided away, thereby avoiding the negative effects such as temperature reduction and purity reduction after the steam pipe 83 is set, and ensuring the smoothness of the entire vaporization process.

[0111] In order to reduce the flow path with the outside world, the inner ring 8543 and the outer ring 8553 of this embodiment are connected by a linkage pipe 856, and the linkage pipe 856 is connected to the external air extraction structure.

[0112] Another embodiment of the present invention further provides a preparation process for high-purity electronic-grade thionyl fluoride, which uses the above-mentioned preparation device for high-purity electronic-grade thionyl fluoride, comprising the following steps:

[0113] S1: adding anhydrous hydrogen fluoride to the bottoms of the first distillation tower, the second distillation tower, and the third distillation tower in advance, then metering anhydrous hydrogen fluoride and thionyl chloride in a molar ratio of 2:1 into a mixer, passing the mixed fluid into a first preheating device and preheating it to 50-100° C., and then continuously adding it to the first distillation tower;

[0114] S2: The bottom liquid of the first distillation tower is circulated back to the tower position through the distillation circulation pump, and the materials are controlled to react at 80-150 ° C and 0-0.5 MPa through the tower bottom reboiler. The thionyl fluoride and hydrogen chloride generated by the reaction enter the condenser from the top of the tower in the form of gas for condensation and separation. The thionyl fluoride is condensed into a liquid portion that refluxes to the top of the tower, and the portion is extracted to the crude product tank. The reflux ratio is 3-5, and the hydrogen chloride gas is discharged from the top of the condenser to the first distillation tower;

[0115] S3: The crude thionyl fluoride is preheated to 30-50°C by a second preheating device and then enters a second distillation tower. The material is controlled at 0-30°C by a tower bottom reboiler, and the light components are removed at the top of the tower, and a product free of light components is obtained in the tower bottom;

[0116] S4: The product without light components enters the third distillation tower for purification, and the material is controlled at 30-50° C. by the tower bottom reboiler, and the thionyl fluoride product is obtained at the top of the tower. The reflux ratio is controlled at 5-10, part of it is refluxed to the top of the tower, and part of it is extracted to the product storage tank for storage. The hydrogen fluoride in the tower bottom is recycled back to the mixer for a cyclic reaction;

[0117] S5: The thionyl fluoride product is fully vaporized at 50-100°C through a vaporization device, compressed to 1-1.5 Map by a compressor, and then stored in a high-pressure buffer tank. The high-pressure product gas is then absorbed by a three-stage molecular sieve adsorption tower to remove hydrogen fluoride and hydrogen chloride, obtaining thionyl fluoride with a purity of 99.999% and stored in a high-pressure product tank.

[0118] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention are intended to be within the scope of protection of the present invention.

Claims

1. A preparation device for preparing high-purity electronic grade thionyl fluoride, characterized in that, The invention comprises: a mixer, the mixer is in communication with a first preheating device, the first preheating device is in communication with a first distillation tower, the top of the distillation tower is connected to a condenser, the condenser is in communication with a crude product tank, the crude product tank is in communication with a second preheating device, the second preheating device is in communication with a second distillation tower, the second distillation tower is in communication with a third distillation tower, the third distillation tower is connected to a storage tank, the storage tank is connected to a vaporization device, the vaporization device is connected to a high-pressure buffer tank, the high-pressure buffer tank is connected to at least three adsorption towers, and the adsorption tower at the rear end is connected to a high-pressure product tank, and further comprises: The mixer comprises a mixing tube (10) for mixing materials, wherein the mixing tube (10) is provided with an anhydrous hydrogen fluoride feed end (20) and a thionyl chloride feed end (30), and a discharge end (40) is provided at one end of the mixing tube (10) away from the thionyl chloride feed end (30). A middle material dividing structure (50), wherein the mixing tube (10) comprises a front section branch pipe (11) provided with an anhydrous hydrogen fluoride feed end (20) and a thionyl chloride feed end (30) and a rear section segment (12) provided with a discharge end (40), wherein the middle positions of the front section branch pipe (11) and the rear section segment (12) are connected via a cross-connecting plate (13), wherein the middle material dividing structure (50) comprises a first sealing crank sleeve (51) provided at the upper end of the cross-connecting plate (13), wherein the lower end of the cross-connecting plate (13) is connected to a second sealing crank sleeve (52), wherein a driving member (53) is provided on a side of the first sealing crank sleeve (51) away from the cross-connecting plate (13), and wherein the output end of the driving member (53) is connected to a dynamic material dividing member (54) which penetrates the cross-connecting plate (13) and is located in the first sealing crank sleeve (51) and the second sealing crank sleeve (52); An axial material distribution structure (60), wherein the front section branch pipe (11) and the rear section segment (12) are both provided with a mounting groove (61) on one side close to the cross-connecting plate (13), and a static material distribution member (62) is movably provided in the mounting groove (61), and the first sealing crank sleeve (51) and the second sealing crank sleeve (52) are connected to the rear sides of the cross-connecting plate (13) and respectively abut against the two static material distribution members (62), and the raw materials entering through the anhydrous hydrogen fluoride feed end (20) and the thionyl chloride feed end (30) are distributed through the front static material distribution member (62), mixed through the dynamic material distribution member (54), and then distributed through the rear static material distribution member (62); The vaporization device comprises: a vaporization tank (80), a thionyl fluoride liquid inlet (81) is provided at the bottom of the vaporization tank (80), a thionyl fluoride gas outlet (82) is provided at the top of the vaporization tank (80), a plurality of steam pipes (83) are provided in the vaporization tank (80), and the steam pipes (83) are connected to an external air inlet and an air outlet, and further comprises: An isolation and distribution structure (84) includes a middle mounting plate (841) disposed in the middle section of the vaporizer (80), the middle mounting plate (841) dividing the vaporizer (80) into a vaporization zone and a distribution zone, a plurality of distribution pipes (842) are connected to the lower end of the middle mounting plate (841), a lower distribution assembly (843) is disposed on the outer side of the middle portion of the distribution pipes (842), the lower distribution assembly (843) controls the opening and closing of all distribution pipes (842), the bottom of the distribution pipes (842) is connected to a lower pumping pipe (844), the lower pumping pipe (844) extends into the thionyl fluoride liquid at the bottom of the vaporizer (80), and the lower distribution assembly (843) periodically pumps the thionyl fluoride liquid at the bottom of the vaporizer (80) into the distribution pipes (842) through the lower pumping pipes (844); The segmented vaporization structure (85) comprises a plurality of accommodating chambers (851) arranged on a central mounting plate (841), wherein the inlet hole at the bottom of the accommodating chamber (851) is communicated with the distribution pipe (842), the steam pipe (83) is plugged into the upper portion of the accommodating chamber (851), an inner inclined hole (831) is provided in the middle of the steam pipe (83), an outer guide plate (853) is tilted outwardly from the inner inclined hole (831), an inner guide assembly (854) is provided on the inner side of the outer guide plate (853) at a position corresponding to the inner inclined hole (831), an outer guide assembly (855) is provided on the outer side of the outer guide plate (853), and both the inner guide assembly (854) and the outer guide assembly (855) are communicated with an external exhaust structure.

2. A preparation device for preparing high-purity electronic grade thionyl fluoride according to claim 1, characterized in that, The first preheating device is the same as the second preheating device, and the first preheating device comprises: a preheating tank body (1), the upper end of the preheating tank body (1) is connected to a crude gas inlet (101), the lower end of the preheating tank body (1) is connected to a crude gas outlet (102), at least one serpentine coil (103) is connected between the crude gas inlet (101) and the crude gas outlet (102), the preheating tank body (1) is provided with an inlet pipe (4) and an outlet pipe (5), and further comprises: an internal circulation contact type structure (2), the serpentine coil (103) includes The invention relates to a method for manufacturing a gas circulation system comprising an upper through-hole (1031) connected to a crude gas inlet (101), wherein the upper through-hole (1031) is connected to a transverse transmission part (1032), and the end of the transverse transmission part (1032) is connected to a bending part (1033). The transverse transmission parts (1032) and the bending parts (1033) are arranged alternately, and the transverse transmission part (1032) at the lowest end is connected to a lower through-hole (1034) communicating with the crude gas outlet (102). The internal circulation contact type structure (2) comprises an internal contact member (2034) arranged inside the bending part (1033). 1), a hollow member (202) is provided on the outer side of the inner contact member (201), an outer contact member (203) is connected to the side of the inner contact member (201) close to the transverse transmission part (1032), the outer contact member (203) is located between the two transverse transmission parts (1032), the inner contact member (201) and the outer contact member (203) are both connected to a steam inlet pipe (204), the steam inlet pipe (204) is located on the outer side of the preheating tank body (1), and the steam entering through the steam inlet pipe (204) is discharged from the inner contact member (201) After being output from the external contact member (203), the steam condenses and falls to the bottom of the preheating tank body (1); the lower isolation structure (3) comprises an inner heat cover (301) arranged at the lower end of the lower through portion (1034), an outer isolation cover (302) is arranged on the outer side of the inner heat cover (301), and a circulation rack (303) is arranged on the outer side of the outer isolation cover (302), and the outer side of the circulation rack (303) is fixed to the inner side of the preheating tank body (1) and communicates with the outside. The condensed steam falls to the bottom of the preheating tank body (1) after being guided by the outer isolation cover (302).

3. A preparation device for preparing high-purity electronic grade thionyl fluoride according to claim 1, characterized in that, The first distillation tower, the second distillation tower, and the third distillation tower have the same structure and size. An air inlet end (93) is provided on one side of the first distillation tower, and the first distillation tower further comprises: a packing installation structure (95). A top tray (911) is provided on the inner side of the distillation tower (90). The packing installation structure (95) comprises a middle fitting (951) locked on the top tray (911). A plurality of circular installation cylinders (952) are sleeved on the middle fitting (951). The inner side of the circular installation cylinder (952) is provided with packing. The inner side of the circular installation cylinder (952) is provided with a recessed area. (953), the recessed area (953) and the inner wall of the distillation tower (90) form a closed space, the inner side of the recessed area (953) is provided with a clamping member (954), the clamping member (954) is in contact with the inner wall of the distillation tower (90), after the middle matching member (951) is fixed, a plurality of circular mounting cylinders (952) are sequentially mounted on the middle matching member (951); the pressurized closed structure comprises an outward expansion rod (961) movably mounted on the inner wall of the middle matching member (951), the inner side of the clamping member (954) is movably provided with an outward push member (962), the The push-out member (962) is movably matched with the middle fitting member (951). When the expansion rod (961) is embedded in the middle fitting member (951), the push-out member (962) is pushed outward to make the clamping member (954) abut against the inner wall of the distillation tower (90). The clamping member (954) includes a guide cartridge (9541) arranged in the recessed area (953). A clamping arm (9542) is movably installed on the inner side of the guide cartridge (9541). A clamping plate (9543) is connected to the side of the clamping arm (9542) away from the middle fitting member (951). The clamping arm (9542) includes a straight arm portion (95421) that cooperates with the guide cartridge (9541), the straight arm portion (95421) is movably connected to the push-out member (962), and the side of the straight arm portion (95421) away from the guide cartridge (9541) is connected to a fan-shaped seat (95422), the clamping plate (9543) is locked on the fan-shaped seat (95422), and a sealing member (963) is provided on the outer periphery of the clamping plate (9543), and the sealing member (963) is tightly attached to the inner wall of the distillation tower (90) as the clamping member (954) moves.

4. A preparation equipment for preparing high-purity electronic grade thionyl fluoride according to claim 1, characterized in that, The transverse connecting plate (13) includes two connecting arc plates (131) connected between the front section branch pipe (11) and the rear section branch pipe (12), a transverse connecting plate (132) is connected between the two connecting arc plates (131), a pair of through holes (133) are opened on the transverse connecting plate (132), a sealing member (135) is locked on the pair of through holes (133), and the second sealing crank sleeve (52) includes a lower outer sealing sleeve that fits with the lower end of the connecting arc plate (131). (521), the inner side of the lower outer sealing sleeve (521) is connected to a lower inner sealing arc sleeve (522) that fits the inner side wall of the connecting arc plate (131), and the lower inner sealing arc sleeve (522) is provided with a facing hollow cylinder (523), and the lateral opening of the facing hollow cylinder (523), the first sealing crank sleeve (51) includes an upper outer sealing sleeve (511) that fits the upper end of the connecting arc plate (131), and the inner side of the upper outer sealing sleeve (511) is connected to the connecting The arc plate (131) is fitted with an upper inner closed arc sleeve (512) on the inner side wall thereof. The lower end of the upper inner closed arc sleeve (512) is provided with a facing column tube (513). The facing column tube (513) has a lateral opening. When the first sealing crank sleeve (51) and the second sealing crank sleeve (52) are matched, the facing column tube (513) is embedded in the facing hollow cylinder (523) through the facing through hole (133), and passes through the blocking member (135) through the facing through hole (133). The opposing column tube (513) and the opposing empty cylinder (523) are connected, and a transverse threaded hole is opened in the transverse direction of the transverse connecting plate (132) corresponding to the position of the through hole (133). The blocking member (135) includes a stud portion (1351) that passes through the opposing column tube (513) and the opposing empty cylinder (523) and cooperates with the transverse threaded hole. An external blocking portion (1352) is provided on the stud portion (1351), and the external blocking portion (1352) closes the through hole (133).

5. A preparation device for preparing high-purity electronic grade thionyl fluoride according to claim 4, characterized in that, A rotary interface (1321) is provided in the middle of the transverse connecting plate (132), and the dynamic material distribution member (54) includes a revolving ring (541) arranged in the revolving ring (1321). An upper mixing portion (542) is provided on the top of the revolving ring (541), and a lower end of the revolving ring (541) is connected to a lower mixing portion (543). The upper mixing portion (542) is connected to the output end of the driving member (53), and the upper mixing portion (542) and the lower mixing portion (543) are of similar size. The upper mixing section (542) includes an axial column (5421) connected to the revolving ring (541), the axial column (5421) is connected to the driving member (53), and a semi-arc-shaped dispersion piece (5422) is provided on the axial column (5421), and a plurality of dispersion holes are opened on the dispersion piece (5422). A gasket (5423) is provided on the outer side of the dispersion piece (5422), and the gasket (5423) is fitted on the inner side of the first sealing crank sleeve (51).

6. A preparation equipment for preparing high-purity electronic grade thionyl fluoride according to claim 1, characterized in that, The mounting groove (61) includes an inner cavity (611), a plurality of outward expansion grooves (612) are provided on the inner side of the inner cavity (611), an outer spring piece (613) is provided on the outer edge of the outward expansion groove (612), the static material part (62) opens the outer spring piece (613) and then snaps into the inner cavity (611) and the outward expansion groove (612), the static material part (62) includes a clamping ring (621) matched with the inner cavity (611), a plurality of outward expansion pads (622) are provided on the outer side of the clamping ring (621), a spiral piece (623) is provided on the inner side of the clamping ring (621), and the outer edge of the clamping ring (621) is attached to the outer sides of the first sealing crank sleeve (51) and the second sealing crank sleeve (52).

7. A preparation equipment for preparing high-purity electronic grade thionyl fluoride according to claim 2, characterized in that, The inner and outer sides of the bending portion (1033) are both opened, the inner contact member (201) comprises an inner air inlet portion (2011) embedded in the opening on the outer side of the bending portion (1033), the inner opening of the bending portion (1033) is provided with an inner air outlet portion (2012), an inner barrier portion (2013) is connected between the inner air inlet portion (2011) and the inner air outlet portion (2012), the inner air inlet portion (2011) is connected to the steam inlet pipe (204), all the inner barrier portions (2013) form a fan-shaped structure, the inner barrier portion (2013) comprises an inner through pipe (20131) connected between the inner air inlet portion (2011) and the inner air outlet portion (2012), and a plurality of barbed tubes (20132) extend outwardly from the circumferential outside of the inner through pipe (20131).

8. A preparation equipment for preparing high-purity electronic grade thionyl fluoride according to claim 1, characterized in that, The inner guide assembly (854) includes an adsorption pad (8541) arranged on the inner inclined hole (831), the lower end of the adsorption pad (8541) is connected to a lower inclined tube (8542), all the lower inclined tubes (8542) are connected through an inner ring (8543), and the lower inclined tubes (8542) are filled with a barrier group. The outer guide assembly (855) includes a receiving sleeve (8551) arranged below the outer guide plate (853), the receiving sleeve (8551) is connected to a lower curved tube (8552), and all the lower curved tubes (8552) are connected to an outer ring (8553). The inner ring (8543) and the outer ring (8553) are connected through a linkage pipe (856), and the linkage pipe (856) is communicated with an external air extraction structure.

9. A preparation equipment for preparing high-purity electronic grade thionyl fluoride according to claim 3, characterized in that, The circular mounting tube (952) is an I-shaped structure, the middle portion of the circular mounting tube (952) is a hollow ring (9521), the bottom surface and the top surface of the circular mounting tube (952) are both mesh plates, and the outer peripheral surface of the circular mounting tube (952) is a closed surface.

10. A process for preparing high-purity electronic-grade thionyl fluoride, using the preparation equipment for preparing high-purity electronic-grade thionyl fluoride according to any one of claims 1 to 9, characterized in that: The following steps are included: S1: adding anhydrous hydrogen fluoride to the bottoms of the first distillation tower, the second distillation tower, and the third distillation tower in advance, then metering anhydrous hydrogen fluoride and thionyl chloride in a molar ratio of 2:1 into a mixer, passing the mixed fluid into a first preheating device and preheating it to 50-100° C., and then continuously adding it to the first distillation tower; S2: The bottom liquid of the first distillation tower is circulated back to the tower position through the distillation circulation pump, and the materials are controlled to react at 80-150 ° C and 0-0.5 MPa through the tower bottom reboiler. The thionyl fluoride and hydrogen chloride generated by the reaction enter the condenser from the top of the tower in the form of gas for condensation and separation. The thionyl fluoride is condensed into a liquid portion that refluxes to the top of the tower, and the portion is extracted to the crude product tank. The reflux ratio is 3-5, and the hydrogen chloride gas is discharged from the top of the condenser to the first distillation tower; S3: The crude thionyl fluoride is preheated to 30-50°C by a second preheating device and then enters a second distillation tower. The material is controlled at 0-30°C by a tower bottom reboiler, and the light components are removed at the top of the tower, and a product free of light components is obtained in the tower bottom; S4: The product without light components enters the third distillation tower for purification, and the material is controlled at 30-50° C. by the tower bottom reboiler, and the thionyl fluoride product is obtained at the top of the tower. The reflux ratio is controlled at 5-10, part of it is refluxed to the top of the tower, and part of it is extracted to the product storage tank for storage. The hydrogen fluoride in the tower bottom is recycled back to the mixer for a cyclic reaction; S5: The thionyl fluoride product is fully vaporized at 50-100°C through a vaporization device, compressed to 1-1.5 Map by a compressor, and then stored in a high-pressure buffer tank. The high-pressure product gas is then absorbed by a three-stage molecular sieve adsorption tower to remove hydrogen fluoride and hydrogen chloride, obtaining thionyl fluoride with a purity of 99.999% and stored in a high-pressure product tank.

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