A kind of automatic production equipment of hexafluorodianhydride

Abstract

This invention discloses an automated production equipment for hexafluorodianhydride, relating to the field of chemical production technology. Following the production sequence, it includes a microchannel reactor, a concentration vessel, and a crystallization vessel. The microchannel reactor comprises several reactor groups connected in series. Each reactor group includes a first clamping plate and a second clamping plate, with several guide plates disposed between the first and second clamping plates. A temperature regulating plate is installed between adjacent guide plates. The concentration vessel includes a purification chamber and an MBR membrane concentration chamber. The MBR membrane concentration chamber is piped to the reactor group, and the MBR membrane concentration chamber is piped to the purification chamber. Thus, the microchannel reactor ensures thorough mixing of the reaction solution, guaranteeing complete reaction and reducing material waste.

Description

Technical Field

[0001] The invention relates to the technical field of chemical production, and in particular to automated production equipment for hexafluorodianhydride. Background Art

[0002] Hexafluorodianhydride (6FDA) is an important intermediate for biopharmaceuticals and chemical products. One of its functions is to synthesize fluorinated polyimide, a high-performance polymer widely used in electronics, aerospace, optics and other fields.

[0003] Most of the existing hexafluorodianhydride production methods tend to be laboratory-based small-batch production, such as the Chinese patent with publication number "CN104529965B", which discloses "a method for preparing hexafluorodianhydride", and its technical scheme is: "Having the following steps: ① adding hexafluorotetraacid to anhydrous acetic anhydride, stirring and heating to reflux for the first closed-loop dehydration reaction, and after the reaction, post-processing to obtain a crude hexafluorodianhydride with a closed-loop rate of ≤98.0%; ② adding the crude hexafluorodianhydride obtained in step ① to anhydrous trifluoroacetic anhydride, stirring and heating to reflux for the second closed-loop dehydration reaction, and after the reaction, post-processing to obtain a finished hexafluorodianhydride with a closed-loop rate of ≥99.5%. The polyimide synthesized from hexafluorodianhydride with a high closed-loop rate obtained by the method of the present invention has a high molecular weight, good mechanical properties and thermal properties, and can be widely used in high-tech fields such as optical communications, colorless transparent flexible circuit boards, solar cell substrates, and organic flexible transparent conductive film substrates."

[0004] Although the hexafluorodianhydride product obtained by the above production process has a high closed-loop rate, it requires more manpower input, which makes the above production process unsuitable for large-scale factory automated continuous production.

[0005] Based on the above problems, how to make targeted improvements to the existing hexafluorodianhydride production method so that it can be automated and continuously mass-produced is a difficult problem we are facing now. Summary of the invention

[0006] In view of the above defects, the purpose of the present invention is to provide an automated production equipment for hexafluorodianhydride, aiming to solve the problem that hexafluorodianhydride is difficult to be automated on a large scale in the prior art.

[0007] In order to solve the above technical problems, the technical solution of the present invention is:

[0008] A hexafluorodianhydride automated production equipment comprises, in order of production, a microchannel reactor, a concentration kettle and a crystallization kettle, wherein the microchannel reactor, the concentration kettle and the crystallization kettle are sequentially connected by pipelines, the microchannel reactor comprises a plurality of reactor groups connected in series, the reactor group comprises a first clamping plate and a second clamping plate, a plurality of guide plates are arranged between the first clamping plate and the second clamping plate, and a temperature regulating plate is installed between adjacent guide plates; the concentration comprises an impurity removal bin and an MBR membrane concentration bin, the MBR membrane concentration bin is connected to the reactor group by pipeline, and the MBR membrane concentration bin is connected to the impurity removal bin by pipeline.

[0009] Among them, the side wall of the first splint is equipped with a liquid inlet and a medium inlet, the side wall of the second splint is provided with a liquid outlet and a medium outlet, a plurality of the guide plates are connected in series, the guide plates include a guide inlet pipe, a disturbing flow hole and a guide outlet pipe connected in sequence, the liquid inlet is connected to the guide inlet pipe, the liquid outlet is connected to the guide outlet pipe, and a disturbing flow pipe is provided between adjacent disturbing flow holes.

[0010] Wherein, a serpentine coil is installed on the temperature regulating plate, one end of the serpentine coil is connected to the medium inlet, and the other end of the serpentine coil is connected to the medium outlet.

[0011] Among them, the guide plate is penetrated with a first avoidance hole, the temperature regulating plate is penetrated with a second avoidance hole, the adjacent guide plates are connected through the second avoidance hole pipe, and the two ends of the serpentine coil are respectively connected to the medium inlet and the medium outlet through the first avoidance hole.

[0012] Wherein, an internal thread is arranged on the inner wall of the turbulent flow hole.

[0013] Wherein, the flow-turbulating duct includes a first tube body and a second tube body, one end of the first tube body is connected to the bottom of the flow-turbulating hole, the other end of the first tube body is connected to the second tube body, and the end of the second tube body away from the first tube body is connected to the top of the flow-turbulating hole; an acceleration chamber is arranged in the second tube body, and the acceleration chamber includes a first cavity, a second cavity and a third cavity, and the inner diameters of the first cavity, the second cavity and the third cavity are a, b, c respectively, and a>c>b.

[0014] Among them, the microchannel reactor also includes a secondary reactor, which is located between the reactor group and the concentrator. The secondary reactor includes a catalytic plate and a cover plate. An air inlet and a feed port are installed on the side wall of the catalytic plate. The catalytic plate is recessed from one end facing the cover plate to the end away from the cover plate to form a catalytic groove. The cover plate covers the catalytic groove. A plurality of catalytic holes are installed in the catalytic groove. Pipes are connected between adjacent catalytic holes. A liquid pipeline is installed between the feed port and the catalytic holes. A catalytic material disc is installed in the catalytic hole. A plurality of guide holes are arranged between the top and bottom of the catalytic material disc; an annular air pipe is arranged at the top of the catalytic hole, and a plurality of air outlets are arranged on the side of the annular air pipe facing the catalytic material disc, and the annular air pipe is connected to the air inlet pipe.

[0015] Among them, the concentration kettle includes an MBR membrane concentration bin and an impurity removal bin, the secondary reactor is connected to the MBR membrane concentration bin by a pipeline, an electromagnetic valve is installed between the bottom of the MBR membrane concentration bin and the top of the impurity removal bin, and the impurity removal bin is connected to the crystallization kettle by a pipeline; a temporary storage bin is installed on the side wall of the MBR membrane concentration bin, an upper fixed plate and a lower fixed plate are installed in the MBR membrane concentration bin, a plurality of MBR membrane column assemblies are installed between the upper fixed plate and the lower fixed plate, one end of the upper fixed plate is connected to the MBR membrane column assembly, and the other end of the upper fixed plate is connected to the temporary storage bin; a plurality of ion exchange resin plates are installed in the impurity removal bin.

[0016] Among them, a rotating column is arranged in the concentration kettle, and a first motor is installed on the top of the concentration kettle. The rotating column includes a power section, a connecting section and a stirring section from top to bottom. The power section is hollow, and one end of the power section is connected to the upper fixed disk. A drainage pipe is installed between the other end of the power section and the temporary storage bin, and one end of the drainage pipe is rotatably connected to the power section; a power wheel is arranged on the side wall of the power section, and a driving wheel is installed at the power output end of the first motor, and the power wheel is connected to the driving wheel belt; the upper fixed disk and the lower fixed disk are both arranged around the connecting section; the ion exchange resin plate is arranged around the stirring section.

[0017] After adopting the above technical solution, the beneficial effects of the present invention are:

[0018] First, the reaction liquid is fully mixed through the microchannel reactor, ensuring that the liquid can fully react and reducing the waste of materials. Second, the crude hexafluorodianhydride liquid is concentrated and the metal ion impurities are removed through the concentration kettle, ensuring the purity of the hexafluorodianhydride crystals. Third, the crystallization is carried out step by step through the crystallization cover in the crystallization kettle, which speeds up the crystallization speed and ensures the work efficiency. Fourth, the entire device can be fully automated and continuously operated, which is suitable for large-scale and continuous production of hexafluorodianhydride. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 This is a schematic diagram of the structure of the automated production equipment for hexafluorodianhydride;

[0020] Figure 2 is the connection diagram of the reactor group;

[0021] Figure 3 is a structural diagram of the reactor group;

[0022] Figure 4 is the structural diagram of the guide plate;

[0023] Figure 5 for Figure 4 A partial enlarged view of middle A;

[0024] Figure 6 is a side sectional view of the guide plate;

[0025] Figure 7 It is the structural diagram of the temperature regulating board;

[0026] Figure 8 is the structural diagram of the catalytic plate;

[0027] Fig. 9 for Figure 8 A partial enlarged view of B in the middle;

[0028] Fig.10 is a structural diagram of the secondary reactor;

[0029] Fig.11 is a side sectional view of a catalyst plate;

[0030] Fig.12 It is the structural diagram of the concentration kettle;

[0031] Fig.13 is a structural diagram of an ion exchange resin plate;

[0032] Fig.14 This is the structural diagram of the crystallization kettle.

[0033] In the figure: 1-microchannel reactor, 11-reactor group, 111-first clamping plate, 112-second clamping plate, 113-guide plate, 114-temperature regulating plate, 115-liquid inlet, 116-medium inlet, 117-liquid outlet, 118-medium outlet, 119-flow guide inlet pipe, 120-disturbance flow hole, 121-flow guide outlet pipe, 122-disturbance pipeline, 123-serpentine coil, 124-first avoidance hole, 125-first two avoidance holes, 126-first tube body, 127-second tube body, 128-acceleration chamber, 129-first cavity, 130-second cavity, 131-third cavity, 13-secondary reactor, 132-catalytic plate, 133-cover plate, 135-air inlet, 136-feeding port, 1361-liquid pipeline, 137-catalytic tank, 138-catalytic hole, 139-catalytic material tray, 140-guide hole, 141-annular air pipe,

[0034] 2-concentration kettle, 21-MBR membrane concentration tank, 22-impurity removal tank, 23-temporary storage tank, 24-upper fixed plate, 25-lower fixed plate, 26-MBR membrane column assembly, 27-ion exchange resin plate, 28-rotating column, 281-power section, 282-connecting section, 283-stirring section, 29-first motor, 210-drainage pipe, 211-sleeve, 212-installation frame, 213-fixed frame, 214-second motor, 215-scraping plate,

[0035] 3-crystallization kettle, 31-scraping column, 32-crystallization cover, 33-scraping plate, 34-jacket, 35-temperature regulating coil, 36-inner cavity, 37-first medium pipe, 38-second medium pipe, 39-distribution table, 310-discharging head, 311-third motor, 312-collecting bin, 313-high pressure air outlet, 314-annular hot air pipe. DETAILED DESCRIPTION

[0036] It should be understood that the specific embodiments described herein are only used to explain the present invention, and are not used to limit the present invention.

[0037] Example:

[0038] like Figure 1-14 As shown, an automated production equipment for hexafluorodianhydride includes, in accordance with the production sequence, a microchannel reactor 1, a concentration kettle 2 and a crystallization kettle 3, wherein the microchannel reactor 1, the concentration kettle 2 and the crystallization kettle 3 are sequentially connected by pipelines; various raw materials participating in the reaction are first dissolved in a solvent to form a reaction liquid, and the reaction liquid is mixed and reacted in the microchannel reactor 1, and after the reaction is completed, the liquid is sent to the concentration kettle 2 for concentration, and the concentrated liquid is easier to crystallize. After the concentration is completed, the hexafluorodianhydride liquid is sent to the crystallization kettle 3 for heating and evaporation, and then the hexafluorodianhydride crystals are gradually precipitated, and finally the hexafluorodianhydride crystals are collected to complete the production work.

[0039] The microchannel reactor 1 includes a plurality of reactor groups 11 connected in series, wherein the reactor group 11 includes a first clamp plate 111 and a second clamp plate 112, wherein a plurality of guide plates 113 are arranged between the first clamp plate 111 and the second clamp plate 112, and a temperature regulating plate 114 is installed between adjacent guide plates 113; the concentration kettle 2 includes an MBR membrane concentration tank 21 and an impurity removal tank 22, wherein the MBR membrane concentration tank 21 is connected to the reactor group 11 by a pipeline, and the crystallization kettle 3 is connected to the impurity removal tank 22 by a pipeline. The liquid material participating in the reaction will enter the guide plate 113 from the first clamp plate 111, and will be discharged from the guide plate 113 through the second clamp plate 112 after the reaction is completed. The function of the temperature regulating plate 114 is to regulate the temperature environment suitable for the reaction.

[0040] like Figure 2-7 As shown, in order to facilitate the introduction of the reaction liquid into the reactor group 11, the side wall of the first clamp 111 is provided with a liquid inlet 115 and a medium inlet 116, the side wall of the second clamp 112 is provided with a liquid outlet 117 and a medium outlet 118, and a plurality of the guide plates 113 are connected in series, the guide plates 113 include a guide inlet pipe 119, a flow-interference hole 120 and a guide outlet pipe 121 connected in sequence, the liquid inlet 115 is connected to the guide inlet pipe 119, the liquid outlet 117 is connected to the guide outlet pipe 121, and a flow-interference pipe 122 is provided between adjacent flow-interference holes 120. If one of the flow-interference holes 120 is connected to the guide inlet pipe 119, the reaction liquid passes through the liquid inlet 115, the guide inlet pipe 119, the flow-interference hole 120, and the flow-interference pipe 122 in sequence, and enters the liquid outlet 117 after reaching the last flow-interference hole 120 to complete the reaction.

[0041] In order to facilitate the introduction of temperature regulating medium into the reactor group 11, a serpentine coil 123 is installed on the temperature regulating plate 114, one end of the serpentine coil 123 is connected to the medium inlet 116, and the other end of the serpentine coil 123 is connected to the medium outlet 118. In this solution, adjacent serpentine coils 123 are connected in series.

[0042] In order to facilitate the series connection of the serpentine coils 123, a first avoidance hole 124 is penetrated on the guide plate 113; and in order to facilitate the series connection of the guide plates 113, a second avoidance hole 125 is penetrated on the temperature regulating plate 114. The adjacent guide plates 113 are connected by the second avoidance hole 125 pipeline, and the two ends of the serpentine coils 123 are respectively connected to the medium inlet 116 and the medium outlet 118 through the first avoidance hole 124.

[0043] In order to form turbulence when the reaction liquid enters the turbulent flow hole 120 and accelerate the mixing and reaction of different liquids, the inner wall of the turbulent flow hole 120 is provided with an internal thread.

[0044] In order to make the reaction liquid realize pressure change in the flow disturbance pipe 122 and cause the flow speed to be fast and slow, the flow disturbance pipe 122 includes a first tube body 126 and a second tube body 127, one end of the first tube body 126 is connected to the bottom of the flow disturbance hole 120, the other end of the first tube body 126 is connected to the second tube body 127, and the end of the second tube body 127 away from the first tube body 126 is connected to the top of the flow disturbance hole 120; an acceleration chamber 128 is arranged in the second tube body 127, and the acceleration chamber 128 includes a first cavity 129, a second cavity 130 and a third cavity 131, and the inner diameters of the first cavity 129, the second cavity 130 and the third cavity 131 are a, b and c respectively, and a>c>b. This design accelerates the mixing speed of the reaction liquid by adjusting the flow speed of the liquid, thereby accelerating its reaction speed.

[0045] In order to further speed up the reaction of the liquid, we need to add a catalyst. Figure 8-11 As shown, the microchannel reactor 1 also includes a secondary reactor 13, which is located between the reactor group 11 and the concentration kettle 2. The secondary reactor 13 includes a catalytic plate 132 and a cover plate 133. The side wall of the catalytic plate 132 is provided with an air inlet 135 and a feed inlet 136. The end of the catalytic plate 132 facing the cover plate 133 is recessed toward the end away from the cover plate 133 to form a catalytic groove 137. The cover plate 133 covers the catalytic groove 137. A plurality of catalytic devices are installed in the catalytic groove 137. The catalyst holes 138 are connected by pipelines between the adjacent catalyst holes 138, a liquid pipeline 1361 is installed between the feed port 136 and the catalyst holes 138, a catalyst tray 139 is installed in the catalyst hole 138, and a plurality of guide holes 140 are arranged between the top and the bottom of the catalyst tray 139; an annular air pipe 141 is arranged on the top of the catalyst hole 138, and a plurality of air outlets are arranged on the side of the annular air pipe 141 facing the catalyst tray 139, and the annular air pipe 141 is connected to the air inlet 135 pipeline.

[0046] The cover plate 133 seals the catalyst tank 137 to prevent leakage of the feed liquid. The air inlet 135 delivers oxygen to the air outlet through the annular air pipe 141, and then the oxygen is discharged toward the catalyst tray 139 through the air outlet. At this time, the reaction liquid also reaches the catalyst tray 139 and passes through the catalyst tray 139 through the guide hole 140. In this process, oxygen, reaction liquid, and catalyst are evenly contacted, which ensures the adequacy of the reaction.

[0047] In addition, in the present solution, a plurality of catalytic material trays 139 and annular air pipes 141 are provided, which will allow the material liquid to react gradually to complete, thereby obtaining a crude hexafluorodianhydride liquid and prolonging the service life of the entire device.

[0048] In order to facilitate the subsequent crystallization, we need to concentrate and purify the crude liquid of hexafluorodianhydride first. For this purpose, the concentration kettle 2 includes an MBR membrane concentration bin 21 and an impurity removal bin 22. The secondary reactor 13 is connected to the MBR membrane concentration bin 21 by a pipeline. A solenoid valve is installed between the bottom of the MBR membrane concentration bin 21 and the top of the impurity removal bin 22. The impurity removal bin 22 is connected to the crystallization kettle 3 by a pipeline; a temporary storage bin 23 is installed on the side wall of the MBR membrane concentration bin 21, and an upper fixed plate 24 and a lower fixed plate 25 are installed in the MBR membrane concentration bin 21. A plurality of MBR membrane column assemblies 26 are installed between the upper fixed plate 24 and the lower fixed plate 25. One end of the upper fixed plate 24 is connected to the MBR membrane column assembly 26, and the other end of the upper fixed plate 24 is connected to the temporary storage bin 23; a plurality of ion exchange resin plates 27 are installed in the impurity removal bin 22.

[0049] MBR membranes are often used to concentrate wastewater, and they separate water molecules from high-salinity wastewater through pressure difference. Using the above characteristics, this solution uses MBR membrane column assembly 26 to separate water molecules and other small molecules in the crude hexafluorodianhydride liquid, so that the crude hexafluorodianhydride liquid is purified in the MBR membrane concentration tank 21.

[0050] The MBR membrane assembly is generally used in conjunction with a pump, so that a pressure difference is formed on both sides of the MBR membrane. In this solution, the pump is placed in the temporary storage bin 23, which is connected to the upper fixed plate 24 by a pipeline.

[0051] The catalyst in this solution is a metal or a metal salt, which causes the hexafluorodianhydride concentrate to contain metal ions. In order to remove the metal ions and ensure the purity of the hexafluorodianhydride crystals, this solution introduces an ion exchange resin plate 27.

[0052] like Figure 12-14As shown, in order to speed up the concentration speed, we need to make the hexafluorodianhydride crude liquid in the MBR membrane concentration bin 21 move. For this purpose, a rotating column 28 is provided in the concentration kettle 2. A first motor 29 is installed on the top of the concentration kettle 2. The rotating column 28 includes a power section 281, a connecting section 282 and a stirring section 283 from top to bottom. The power section 281 is hollow, one end of the power section 281 is connected to the upper fixed plate 24, and a drainage pipe 210 is installed between the other end of the power section 281 and the temporary storage bin 23. One end of the drainage pipe 210 is rotatably connected to the power section 281; a power wheel is provided on the side wall of the power section 281, and a driving wheel is installed at the power output end of the first motor 29, and the power wheel is connected to the driving wheel belt; the upper fixed plate 24 and the lower fixed plate 25 are both arranged around the connecting section 282; the ion exchange resin plate 27 is arranged around the stirring section 283. The first motor 29 drives the rotating column 28 to rotate. Since the rotating column 28 is connected to the upper fixed plate 24 and the rotating column 28 is rotatably connected to the top of the MBR membrane concentration tank 21, the rotating column 28 will drive the MBR membrane column assembly 26, the upper fixed plate 24, and the lower fixed plate 25 to rotate together, thereby stirring the crude hexafluorodianhydride liquid.

[0053] This design also allows the ion exchange resin plate 27 to rotate along with the rotating column 28 , thereby stirring the concentrated hexafluorodianhydride concentrate, which speeds up the speed at which the ion exchange resin plate 27 removes metal ions.

[0054] One end of the liquid discharge pipe 210 is rotatably connected to the power section 281 , and the other end thereof is connected to the pump in the temporary storage bin 23 .

[0055] In order to ensure the firmness of the ion exchange resin plate 27, a sleeve 211 is provided on the circumference of the stirring section 283, and a mounting frame 212 is provided between the sleeve 211 and the inner wall of the impurity removal bin 22. The ion exchange resin plate 27 is arranged on the mounting frame 212, and a plurality of exchange holes are opened on the ion exchange resin plate 27.

[0056] In order to further speed up the removal of metal ions, a second motor 214 is provided between the sleeve 211 and the stirring section 283, and a fixing frame 213 is provided on the circumference of a portion of the ion exchange resin plate 27, one end of the fixing frame 213 is connected to the second motor 214, and the other end of the fixing frame 213 is connected to the mounting frame 212. This design enables the second motor 214 to drive the fixing frame 213 and a portion of the ion exchange resin plate 27 to rotate, and the rotation direction of this portion of the ion exchange resin plate 27 is different from the rotation direction of the rotating column 28, which increases the base area of ​​the ion exchange resin plate 27 and the hexafluorodianhydride concentrate.

[0057] The concentrated hexafluorodianhydride liquid is very easy to precipitate crystals. In order to prevent the crystals from adhering to the inner wall of the impurity removal bin 22 , a scraper plate 215 is provided between the mounting frame 212 and the inner wall of the impurity removal bin 22 .

[0058] In order to facilitate the crystallization of hexafluorodianhydride, this scheme adopts a scheme of dispersed crystallization step by step. To this end, a scraper column 31 is rotatably arranged in the crystallization kettle 3, and a plurality of crystallization covers 32 are arranged on the circumference of the scraper column 31, and the plurality of crystallization covers 32 are arranged in sequence from top to bottom along the scraper column 31; a scraper plate 33 cooperating with the crystallization cover 32 is installed on the side wall of the scraper column 31; the crystallization kettle 3 includes a jacket 34, a temperature regulating coil 35 is installed in the jacket 34, and the crystallization cover 32 includes an inner cavity 36, and a first medium pipe 37 and a second medium pipe 38 are arranged between the temperature regulating coil 35 and the inner cavity 36. When the scraper column 31 rotates, it will drive the scraper plate 33 to rotate, which will continuously scrape off the crystals on the crystallization cover 32, so that the crystals fall step by step. The first medium pipe 37 delivers the heating medium of the temperature regulating coil 35 to the inner cavity 36 of the crystallization cover 32 , and then the heating medium is delivered back to the temperature regulating coil 35 through the second medium pipe 38 to complete the heating of the crystallization cover 32 .

[0059] Preferably, the crystallization cover 32 is trumpet-shaped, the top area of ​​the crystallization cover 32 is larger than the bottom area of ​​the crystallization cover 32, and a gap is provided between the bottom of the crystallization cover 32 and the side wall of the scraping column 31. This design facilitates material feeding. At the same time, in order to ensure the firmness of the crystallization cover 32, a plurality of support arms are provided between the crystallization cover 32 and the inner wall of the crystallization kettle 3.

[0060] In order to facilitate the liquid to reach each area of ​​the crystallization cover 32 evenly, a material distribution platform 39 is arranged between adjacent crystallization covers 32, and the material distribution platform 39 is conical.

[0061] In order to facilitate the delivery of the hexafluorodianhydride concentrated liquid to the crystallization cover 32, a discharge head 310 is arranged between the top of the crystallization kettle 3 and the crystallization cover 32, and a plurality of discharge ports are arranged at one end of the discharge head 310 facing the crystallization cover 32; the discharge head 310 is arranged around the scraper column 31, the scraper column 31 is hollow, and the discharge head 310 is connected to the scraper column 31; a concentration pipeline is arranged between the scraper column 31 and the impurity removal bin 22, and one end of the concentration pipeline is rotatably connected to the scraper column 31; a third motor 311 is installed on the top of the crystallization kettle 3, and the power output end of the third motor 311 is belt-connected to the side wall of the scraper column 31.

[0062] In order to further dry the hexafluorodianhydride crystals, a collection bin 312 and an annular hot air pipe 314 are provided at the bottom of the crystallization kettle 3. The annular hot air pipe 314 is arranged around the collection bin 312. A plurality of high-pressure air ports 313 are installed in the collection bin 312. One end of the high-pressure air port 313 is connected to the annular hot air pipe 314, and the other end of the high-pressure air port 313 is arranged toward the crystallization cover 32.

[0063] In summary, this solution has the following advantages: First, the reaction liquid is fully mixed by the microchannel reactor 1, which ensures that the liquid can fully react and reduces the waste of materials. Second, the crude hexafluorodianhydride liquid is concentrated and metal ion impurities are removed by the concentration kettle 2, which ensures the purity of the hexafluorodianhydride crystals. Third, the crystallization is carried out step by step by the crystallization cover 32 in the crystallization kettle 3, which speeds up the crystallization speed and ensures the work efficiency. Fourth, the whole device can be fully automated and continuously operated, which is suitable for large-scale and continuous production of hexafluorodianhydride.

[0064] The present invention is not limited to the above-mentioned specific implementation modes. Various changes made by ordinary technicians in this field based on the above-mentioned concepts without creative work are all within the protection scope of the present invention.

Claims

1. An automated production device for hexafluorodianhydride, comprising, in order of production, a microchannel reactor (1), a concentration kettle (2) and a crystallization kettle (3), wherein the microchannel reactor (1), the concentration kettle (2) and the crystallization kettle (3) are connected in order by pipelines, characterized in that: The microchannel reactor (1) comprises a plurality of reactor groups (11) connected in series, wherein the reactor group (11) comprises a first clamping plate (111) and a second clamping plate (112), a plurality of guide plates (113) are arranged between the first clamping plate (111) and the second clamping plate (112), and a temperature regulating plate (114) is installed between adjacent guide plates (113); the concentration kettle (2) comprises an impurity removal bin (22) and an MBR membrane concentration bin (21), wherein the MBR membrane concentration bin (21) is connected to the reactor group (11) via a pipeline, and the MBR membrane concentration bin (21) is connected to the impurity removal bin (22) via a pipeline; The side wall of the first clamping plate (111) is provided with a liquid inlet (115) and a medium inlet (116), the side wall of the second clamping plate (112) is provided with a liquid outlet (117) and a medium outlet (118), a plurality of the guide plates (113) are connected in series, the guide plates (113) comprising a guide inlet pipe (119), a flow disturbance hole (120) and a guide outlet pipe (121) connected in sequence, the liquid inlet (115) is connected to the guide inlet pipe (119), the liquid outlet (117) is connected to the guide outlet pipe (121), and a flow disturbance pipe (122) is provided between adjacent flow disturbance holes (120); A serpentine coil (123) is installed on the temperature regulating plate (114), one end of the serpentine coil (123) is connected to the medium inlet (116), and the other end of the serpentine coil (123) is connected to the medium outlet (118); The guide plate (113) is provided with a first avoidance hole (124), the temperature adjustment plate (114) is provided with a second avoidance hole (125), the adjacent guide plates (113) are connected via the second avoidance hole (125) pipeline, and the two ends of the serpentine coil (123) are respectively connected to the medium inlet (116) and the medium outlet (118) via the first avoidance hole (124); An internal thread is provided on the inner wall of the turbulent flow hole (120); The flow-turbulating duct (122) comprises a first tube body (126) and a second tube body (127); one end of the first tube body (126) is connected to the bottom of the flow-turbulating hole (120); the other end of the first tube body (126) is connected to the second tube body (127); one end of the second tube body (127) away from the first tube body (126) is connected to the top of the flow-turbulating hole (120); an acceleration chamber (128) is arranged in the second tube body (127); the acceleration chamber (128) comprises a first chamber (129), a second chamber (130) and a third chamber (131); the inner diameters of the first chamber (129), the second chamber (130) and the third chamber (131) are a, b and c respectively, and a>c>b; The microchannel reactor (1) further comprises a secondary reactor (13), wherein the secondary reactor (13) is located between the reactor group (11) and the concentration kettle (2), and the secondary reactor (13) comprises a catalytic plate (132) and a cover plate (133). An air inlet (135) and a feed inlet (136) are installed on the side wall of the catalytic plate (132). An end of the catalytic plate (132) facing the cover plate (133) is recessed toward an end away from the cover plate (133) to form a catalytic groove (137). The cover plate (133) covers the catalytic groove (137), and a plurality of catalytic devices are installed in the catalytic groove (137). Catalytic holes (138), adjacent catalytic holes (138) are connected by pipelines, a liquid pipeline (1361) is installed between the feed port (136) and the catalytic hole (138), a catalytic material disc (139) is installed in the catalytic hole (138), and a plurality of guide holes (140) are arranged between the top and the bottom of the catalytic material disc (139); an annular air pipe (141) is arranged at the top of the catalytic hole (138), and a plurality of air outlets are arranged on the side of the annular air pipe (141) facing the catalytic material disc (139), and the annular air pipe (141) is connected to the air inlet (135) pipeline.

2. The automated production equipment for hexafluorodianhydride according to claim 1, characterized in that: The concentration tank (2) comprises an MBR membrane concentration tank (21) and an impurity removal tank (22); the secondary reactor (13) is connected to the MBR membrane concentration tank (21) by a pipeline; a solenoid valve is installed between the bottom of the MBR membrane concentration tank (21) and the top of the impurity removal tank (22); the impurity removal tank (22) is connected to the crystallization tank (3) by a pipeline; a temporary storage tank (23) is installed on the side wall of the MBR membrane concentration tank (21); an upper fixed plate (24) and a lower fixed plate (25) are installed in the MBR membrane concentration tank (21); a plurality of MBR membrane column assemblies (26) are installed between the upper fixed plate (24) and the lower fixed plate (25); one end of the upper fixed plate (24) is connected to the MBR membrane column assembly (26); and the other end of the upper fixed plate (24) is connected to the temporary storage tank (23); and a plurality of ion exchange resin plates (27) are installed in the impurity removal tank (22).

3. A hexafluorodianhydride automated production equipment according to claim 2, characterized in that: A rotating column (28) is arranged in the concentration kettle (2). A first motor (29) is installed on the top of the concentration kettle (2). The rotating column (28) comprises, from top to bottom, a power section (281), a connecting section (282) and a stirring section (283). The power section (281) is hollow. One end of the power section (281) is in communication with an upper fixed disk (24). A drainage pipe (210) is installed between the other end of the power section (281) and the temporary storage bin (23). One end of the drainage pipe (210) is rotatably connected to the power section (281). A power wheel is arranged on the side wall of the power section (281). A driving wheel is installed at the power output end of the first motor (29). The power wheel is connected to the driving wheel by a belt. The upper fixed disk (24) and the lower fixed disk (25) are both arranged around the connecting section (282). The ion exchange resin plate (27) is arranged around the stirring section (283).

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