Resin precipitation washing device

Abstract

The utility model discloses a resin precipitation washing device. The device comprises a two-in-one kettle, a chassis and a water storage tank, the two-in-one kettle is provided with a dispersion mixer, the dispersion mixer is respectively connected with a water storage tank and a feeding pipe, a stirring paddle is arranged in the two-in-one kettle, the bottom of the two-in-one kettle is connected with a chassis, the top of the chassis is provided with a filtering structure, the bottom of the chassis is provided with a water outlet, and the water outlet is connected with an inlet of a water return pump. One water outlet of the tee joint is connected with the water return pipe, the other water outlet of the tee joint is connected with the water drainage pipe, and the water return pipe is connected with the water storage tank. According to the utility model, resin precipitation and washing equipment are integrated, so that the water consumption is low, the occupied area of the equipment is small, the washing effect is good, and the impurity ion content index in the resin completely meets the performance requirements of advanced semiconductor packaging materials.

Description

Technical Field

[0001] The utility model relates to a resin precipitation washing device, in particular to an industrial production device capable of precipitating resin reaction liquid in its poor solvent water to form uniform granular powder and removing intermediate product impurity ions and metal ions by resin washing. Background Art

[0002] Polyimide is a key material in the field of advanced semiconductor packaging. Insulation is one of the key properties of polyimide materials. Semiconductor devices have extremely stringent requirements on the content of metal ions in materials. The synthesis of polyimide precursor resins will produce intermediate impurity ions, and some metal ions will also be introduced into the resin raw materials and the environment. If these impurity ions are not removed, the performance of polyimide material products will be seriously affected.

[0003] Semiconductor devices have stringent requirements on the metal plasma content in polyimide materials, which makes the process steps of polyimide precursor resins more complicated in industrial production. Among them, the resin precipitation step and the washing step are the key steps to remove these impurity ions. The traditional resin precipitation and washing process uses a lot of equipment, the equipment occupies a large area, and the investment cost of equipment and plant is high. In order to ensure that the metal plasma content in the resin meets the product requirements, a large amount of deionized ultrapure water is required, which not only wastes water resources but also brings great pressure on wastewater treatment. The complexity of resin production process and equipment will not only result in low industrial production efficiency and low degree of equipment automation, but also increase the risk of introducing impurity ions into the environment. Utility Model Content

[0004] The utility model aims to provide a resin precipitation washing device, which has a small footprint and a high degree of automation. Precipitation and washing are combined in a two-in-one kettle, which simplifies the number of equipment and solves the problems of low industrial production efficiency of polyimide precursor resins and large investment in equipment and plant land. The device can also be used for the precipitation and washing of other resins.

[0005] In order to achieve the above purpose, the utility model adopts the following technical solutions:

[0006] A resin precipitation washing device comprises a two-in-one kettle for resin precipitation and washing, a chassis and a water storage tank. The two-in-one kettle comprises an inner cavity with openings at both ends and a top cover located at the upper part of the inner cavity, a stirring paddle is arranged in the inner cavity, the upper end of the stirring paddle passes through the two-in-one kettle top cover and is connected to a stirring motor, the stirring motor is fixed on a liftable base, a resin precipitation outlet, a water inlet and a material outlet are arranged on the two-in-one kettle, a disperser is installed at the resin precipitation outlet, the disperser is connected to a water storage tank and a feeding pipe respectively, the bottom of the two-in-one kettle is connected to the chassis, a filtering structure is arranged on the top of the chassis, a water outlet is arranged at the bottom of the chassis, the water outlet is connected to the inlet of a return water pump, the return water pump outlet is connected to the water inlet of a tee, one water outlet of the tee is connected to a return water pipe, the other water outlet is connected to a drain pipe, and the return water pipe is connected to a water storage tank.

[0007] Furthermore, in order to completely remove the impurity ions in the resin, the device uses a disperser to evenly pulverize the resin reaction liquid in its poor solvent water, and the precipitated resin powder particles are uniform in size, with an average particle size of less than 60μm, and there is no phenomenon of resin wrapping the reaction liquid. The resin reaction liquid enters the disperser through a feed pipe, and a feed pump is provided on the feed pipe.

[0008] Furthermore, the liftable base is connected to the top cover via a lifting rod and a stabilizing rod, wherein the lifting rod controls the lifting of the base so that the stirring paddle can be lifted up and down to fully mix and stir, and the lifting rod is connected to a control system. The stabilizing rod stabilizes the base and can maintain stability when the base is lifted or lowered. The lifting rods are arranged vertically, and there are at least two of them, one end of the lifting rods is arranged inside the base, and the other end is fixed on the top cover. The number of lifting rods is at least two, and they are preferably arranged symmetrically. One end of the stabilizing rod is also arranged inside the base, and the other end is also fixed on the top cover. There are at least two stabilizing rods, and the upper ends of the stabilizing rods are preferably connected to each other to achieve better stabilization.

[0009] Furthermore, the water inlet on the two-in-one kettle is connected to an ultrapure water pipeline for introducing washing water into the two-in-one kettle. The ultrapure water pipeline is provided with a flow regulating valve and a flow meter.

[0010] Furthermore, the two-in-one kettle may be provided with an air inlet and an exhaust port, the air inlet being connected to a nitrogen pipeline, and nitrogen may be introduced into the two-in-one kettle through the air inlet, so that filtration is performed under nitrogen pressurized conditions, and washing water may pass through the filtration structure quickly and more thoroughly, achieving efficient and rapid drainage, accelerating filtration speed, and improving washing efficiency. A nitrogen valve is provided on the nitrogen pipeline.

[0011] Furthermore, a pressure gauge and a window may be provided on the two-in-one kettle. The pressure gauge is used to reflect the pressure of the two-in-one kettle, and the window can facilitate observation of the internal conditions of the two-in-one kettle.

[0012] Furthermore, a heat preservation jacket can be provided on the two-in-one kettle to heat the two-in-one kettle, and washing can be performed under heating conditions, thereby increasing the solubility of impurity ions in water, improving the effect and efficiency of washing, and reducing the amount of water used for washing. The heat preservation jacket is provided with a liquid inlet and a liquid outlet, and is connected to a temperature control device for controlling the heating temperature.

[0013] Furthermore, a support structure is provided on the two-in-one kettle to ensure the stability of the two-in-one kettle, and the support structure includes support legs, and a support base may be further connected to the bottom of the support legs.

[0014] Furthermore, the disperser mixer is connected to the water storage tank through a water inlet pipe, and is connected to the feed pump through a feed pipe. The water inlet pipe, the feed pipe and the two-in-one kettle return pipe are all provided with flow regulating valves and flow meters, and the two-in-one kettle drain pipe is provided with a ball valve. The two-in-one kettle and the water storage tank are connected through the water inlet pipe and the return pipe, and the precipitation water and washing water are recycled, reducing the water consumption for resin precipitation and washing.

[0015] Furthermore, the disperser mixer used is the disperser mixer described in patent CN109749099A.

[0016] Furthermore, the stirring paddle includes a stirring rod and a blade. The blade is located on the stirring rod, generally at the lower end of the stirring rod. The blade is a triangular three-dimensional gradient sickle-shaped structure, that is, the cross-section of the blade is a triangle, and the size of the blade gradually decreases from one end connected to the stirring rod to the other end; the blade is at least one, for example, one, two, three or more, preferably at least two.

[0017] Furthermore, by setting the paddle structure, it can play the dual role of stirring and automatic unloading. The width of the paddle gradually narrows from the inside to the outside, and the outermost end of the paddle is less than or equal to two centimeters away from the inner wall of the two-in-one kettle. The stirring paddle can play the role of stirring when it rotates forward, and can automatically unload when it rotates reversely.

[0018] Furthermore, an annular baffle is provided on the side wall of the bottom of the two-in-one kettle, and the annular baffle is located below the discharge port. The annular baffle can be seamlessly fitted with the filtering structure on the bottom plate to prevent leakage, and is fixed on the inner wall of the two-in-one kettle. When the stirring paddle is lowered to the lowest point, the distance between the bottom of the stirring paddle and the annular baffle is less than or equal to one centimeter.

[0019] Furthermore, a discharge port of the two-in-one kettle is extended outwardly to be provided with a discharge pipe, the discharge port is arranged on the side wall of the two-in-one kettle, and the material is discharged through the discharge port and the discharge pipe.

[0020] Furthermore, the shape of the discharge pipe can be various shapes that are convenient for discharge, such as a straight line, a right angle, an arc, etc. A discharge port is provided on the discharge pipe, and the discharge port can be located at the end of the discharge pipe or on its side wall. Preferably, the discharge pipe is arranged in a straight line, and the discharge port is located on the side wall at the bottom of the discharge pipe. More preferably, a discharge rod is provided in the discharge pipe, and a baffle is provided at the top of the discharge rod, and the size of the baffle matches the discharge port and the discharge pipe. The discharge port is closed by the baffle, and the baffle is seamlessly fitted with the discharge port. The end of the discharge rod is located outside the discharge pipe. When discharging, the discharge rod is pulled by the hydraulic control system to open the discharge port and discharge from the discharge port. Preferably, the discharge port and the baffle at the top of the discharge rod are both circular structures, and the ratio of the diameter of the discharge port and the discharge port to the height of the two-in-one kettle cavity is 1:3-4.

[0021] Furthermore, the two-in-one kettle and the chassis are detachably connected, for example, by means of a buckle, a slot, etc. In addition, a lifting rod can be connected between the bottom of the two-in-one kettle and the chassis, and the lifting rod is controlled by the control system to achieve the lifting of the chassis. One end of the lifting rod is connected to the chassis, and the other end is connected to the two-in-one kettle.

[0022] Furthermore, the filtering structure includes a filter plate, which is a planar porous structure, and its shape is consistent with the inner cavity of the two-in-one kettle, for example, a circular shape, and a filter cloth is provided on the upper part of the filter plate for filtering washing water, and a ring-shaped cover plate is provided on the upper part of the filter cloth, which plays a role in fixing the filter cloth and fixes the filter cloth on the filter plate. When the bottom plate is raised to the highest point, the ring-shaped baffle plate on the two-in-one kettle is seamlessly fitted with the cover plate of the filter cloth.

[0023] Furthermore, the chassis is a hollow structure with an opening at the top, a filtering structure is arranged at the opening, and the hollow interior is used to hold washing water. The bottom of the chassis is preferably a pot bottom type structure, and the water outlet is located at the lowest point of the chassis to facilitate drainage.

[0024] Furthermore, universal wheels can be provided on the chassis of the two-in-one kettle to facilitate the movement of the chassis, and the number of universal wheels can be adjusted according to actual needs, for example, it can be 2, 3, 4 or more than 4, preferably at least 3.

[0025] Furthermore, a TDS detection probe is provided on the drain pipe, and the TDS detection probe is connected to a TDS detector (total dissolved solids detector) through a data transmission line, which can monitor the change of impurity ion content in the washing water in real time. The washed water is discharged through the outlet. According to the TDS test, when the washing water reaches a certain index, the washing water is recovered to the water storage tank and reused when it is precipitated next time. When the washing water does not reach the corresponding index, it is directly discharged through the drain pipe.

[0026] Furthermore, the water storage tank is provided with a water return port, a water inlet and a water outlet. The water return port and the water inlet can be located at the upper part or top of the water storage tank, and the water inlet is connected to the ultrapure water pipeline for adding ultrapure water to the water storage tank, and the ultrapure water pipeline is provided with a flow regulating valve and a flow meter. The water return port is connected to the water return pipe for recycling the water that meets the requirements after washing the two-in-one kettle. The water outlet is connected to the water inlet pipe for supplying water to the disperser mixer. The water outlet is preferably set at the lowest point at the bottom of the water storage tank.

[0027] Furthermore, a manhole may be provided on the water storage tank to facilitate cleaning, and a cover plate may be provided at the manhole.

[0028] Furthermore, a liquid level meter may be provided on the water storage tank to detect the water level in the water storage tank, and the liquid level meter is connected to the display screen and the alarm via a data transmission line.

[0029] Furthermore, a pressure balancing port can be provided on the water tank, and the pressure balancing port is used to balance the pressure in the water tank. A movable cover is provided at the pressure balancing port. When the pressure in the water tank is too high, the movable cover can be automatically opened to release the pressure.

[0030] Furthermore, support legs can be provided on the water tank to better stabilize the water tank, and the water tank has at least three support legs.

[0031] Furthermore, there is no special requirement for the shape of the water storage tank, and various shapes are acceptable, such as cylindrical, rectangular, etc. The cavity of the water storage tank can also be a cylindrical structure, with an inverted pot bottom shape at the top and a pot bottom shape at the bottom.

[0032] Furthermore, in order to avoid the introduction of metal ions during the resin precipitation and washing process, preferably, all parts in contact with the resin are coated with a polytetrafluoroethylene coating, such as the stirring paddle body and the surface of the paddle blades, the inner cavity of the two-in-one kettle, the surface of the baffle at the top of the unloading rod, the inner surface of the chassis cavity, the surface of the filtering structure, the inner surface of the water inlet pump, the inner surface of the return pump, the inner surface of the feed pump, etc. are all coated with a polytetrafluoroethylene coating.

[0033] The utility model uses the precipitation washing device to achieve the precipitation and washing of the resin. The device simplifies the resin production process steps, reduces the risk of introducing impurity ions during the resin production process, reduces the amount of water used, and improves the washing effect. The utility model device is suitable for resins that need to be converted from a reaction liquid state to a solid powder state and need to be washed to remove impurities. The resin can be a polyimide resin, a polyimide precursor resin, an epoxy resin, a polyester resin, a phenolic resin, and the like. The polyimide precursor resin can be a polyamic acid resin or a polyamic acid ester resin.

[0034] The method of using the utility model is as follows:

[0035] (1) Start stirring the two-in-one kettle, make the stirring paddle rotate forward to stir, let water and resin reaction liquid enter the disperser mixer through the water inlet pipe and the feed pipe respectively for precipitation, and the material in the disperser mixer enters the two-in-one kettle through the resin precipitation outlet. After the feeding is completed, close the feed pump and the water inlet pipe;

[0036] (2) After the material enters the two-in-one kettle, if the water meets the washing amount requirement, washing will start directly. If the water does not meet the washing amount requirement, water will enter the two-in-one kettle from the water inlet or the resin precipitation outlet, and stop water intake after the washing water amount is met;

[0037] (3) The two-in-one kettle is heated up, and then washed under stirring. After washing, stirring is stopped, nitrogen is introduced into the two-in-one kettle, the water outlet is opened for filtering, the return water pump is turned on, and the water is discharged from the drain pipe. At the same time, the TDS value of the discharged water is detected. If the TDS value meets the requirements, the filtered water enters the water storage tank through the return water pipe for reuse. If the TDS value does not meet the requirements, the filtered water is discharged from the drain pipe. After the filtration is completed, the nitrogen is stopped;

[0038] (4) Repeat the water intake, washing, and filtering steps of steps (2) and (3) until the washing requirements are met;

[0039] (5) After washing is completed, open the exhaust port of the two-in-one kettle, open the discharge port after returning to normal pressure, and start the stirring paddle to reverse and complete automatic discharge.

[0040] Further, the washing water and the precipitation water are preferably deionized ultrapure water, and the precipitation water and the washing water can also be recycled washed water. When in use, first inject water into the water storage tank, if the water amount in the water storage tank has met the water amount required for precipitation, then omit this step.

[0041] Furthermore, if there is still water in the water storage tank, the water can be directly introduced into the two-in-one kettle through the resin precipitation outlet for washing. If there is insufficient water in the water storage tank, ultrapure water can be directly introduced through the water inlet for washing.

[0042] Furthermore, the resin reaction liquid is a reaction liquid containing resin obtained by reaction.

[0043] Furthermore, the resin reaction liquid enters the disperser through a feed pipe, and the concentration of the resin in the resin reaction liquid is 5wt% to 50wt%, for example, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, preferably, the concentration is 10wt% to 45wt%.

[0044] Furthermore, the reaction liquid in the feed pipe and the water in the water inlet pipe enter the disperser at the same time, and the volume flow ratio (Qv) of the reaction liquid and water is 0.02-0.30:1, for example, 0.02:1, 0.05:1, 0.08:1, 0.1:1, 0.15:1, 0.2:1, 0.25:1, 0.3:1. Preferably, the ratio of the feed flow rate to the water inlet flow rate Qv is 0.05-0.15:1.

[0045] Furthermore, the amount of water used for washing can be adjusted according to the type of resin and the content of impurity ions in the resin, so as to ensure that the requirements are met after washing.

[0046] Further, the washing temperature is preferably 50-70° C., such as 50° C., 55° C., 60° C., 65° C., 70° C., preferably 60° C. The washing time is 1-2 h.

[0047] Furthermore, the stirring speed during washing is 70-90 r / min, for example, 70 r / min, 75 r / min, 80 r / min, 85 r / min, 90 r / min, preferably 80 r / min.

[0048] The utility model has the following beneficial effects:

[0049] 1. The utility model combines resin precipitation and washing equipment into one, with low water consumption, small equipment footprint, simple process and good washing effect, which solves the problems of complicated resin precipitation washing equipment, large equipment footprint, large equipment investment, large water consumption and complicated process steps, and solves the problems of low industrial production efficiency and low equipment automation of resins such as polyimide precursor resins.

[0050] 2. The present invention completes the precipitation of the resin in a dispersing mixer, and can better precipitate the resin from the reaction solution and make the particles uniform. The present invention controls the resin precipitation and washing process in a closed environment, and also reduces the risk of introducing impurity ions during the resin production process. The water washing is carried out under heating, and the impurity ions in the resin are completely removed. When the method of the present invention is used to precipitate and wash the polyimide precursor resin, the impurity ion content index in the obtained resin fully meets the performance requirements of advanced semiconductor packaging materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0051] Figure 1 It is a structural schematic diagram of the resin precipitation washing device of the utility model.

[0052] Figure 2 yes Figure 1 Schematic diagram of the structure of the unloading part of the two-in-one kettle.

[0053] Figure 3 yes Figure 1Schematic diagram of the structure of the chassis part of the two-in-one kettle.

[0054] Figure 4 yes Figure 1 Top view of the chassis of the two-in-one kettle.

[0055] Figure 5 yes Figure 1 Schematic diagram of the structure of the middle blade.

[0056] In the figure: 1, two-in-one kettle; 2, inner cavity of two-in-one kettle; 3, stirring paddle; 301, paddle; 4, top cover of two-in-one kettle; 5, stirring motor; 6, base; 61, lifting rod; 7, stabilizing rod; 8, neck; 81, resin precipitation outlet; 82, air inlet; 821, nitrogen pipeline; 822, nitrogen valve; 83, exhaust port; 831, exhaust valve; 84, water inlet; 841, ultrapure water pipeline; 842, flow regulating valve; 843, flow meter; 85, pressure gauge port; 851, pressure gauge; 8 6. Window; 9. Disperser; 10. Water inlet pipe; 101. Flow control valve; 102. Flow meter; 11. Feed pipe; 111. Flow control valve; 112. Flow meter; 12. Water storage tank; 121. Manhole; 1211. Manhole cover; 122. Water return port of water storage tank; 123. Water inlet of water storage tank; 1231. Ultrapure water pipeline; 1232. Flow control valve; 1233. Flow meter; 124. Liquid level gauge port; 125. Pressure balance port; 1251. Movable cover; 12 6. Water outlet of water storage tank; 127. Support legs of water storage tank; 13. Feed pump; 14. Return pump; 15. Discharge port; 16. Annular baffle; 17. Discharge pipe; 18. Discharge rod; 19. Baffle of discharge rod; 20. Discharge port; 21. Chassis; 211. Filter plate; 212. Filter cloth; 213. Filter cloth cover; 214. Water outlet of chassis; 215. Universal wheel; 216. Chassis lifting rod; 217. Chassis extension rod; 22. Return pipe; 221. Flow control valve; 222. Flow meter; 23. Water inlet pump; 24. Drain pipe; 241. Drain pipe ball valve; 25. Jacket of two-in-one kettle; 251. Jacket liquid inlet; 252. Jacket liquid outlet; 26. Liquid inlet pipe; 27. Liquid outlet pipe; 28. Temperature control device; 29. ​​Support legs of two-in-one kettle; 30. Support base of two-in-one kettle; 31. TDS detector; 311. TDS detection probe; 312. Data transmission line; 32. Liquid level meter; 321. Liquid level display screen; 322. Liquid level alarm; 323. Data transmission line. DETAILED DESCRIPTION

[0057] The following will be combined with the drawings in the embodiments of the utility model to describe the technical solutions in the embodiments of the utility model more clearly and completely. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of them. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0058] Example 1

[0059] like Figure 1-5 The resin precipitation washing device of the utility model is shown, which includes a two-in-one kettle 1, a bottom plate 21 and a water storage tank 12. The two-in-one kettle includes a kettle body and a top cover located on the kettle body. There is no special requirement for the overall shape of the kettle body, which can be cylindrical, rectangular, or other shapes. Figure 1 As shown, the upper part of the kettle body is a neck 8, the upper half of the neck is a cylindrical structure, the lower half of the neck is an arc-shaped surface protruding outward, and is an arc-shaped tapered structure. The middle and lower parts of the kettle body are cylindrical. The kettle body is provided with openings at the top and bottom, and its interior is a hollow inner cavity 2, in which there is a stirring paddle 3, and the stirring paddle blade 301 is located at the lower end of the rod body. The paddle plays a stirring role and can be various feasible paddles. Preferably, the paddle is a triangular three-dimensional gradient sickle-shaped structure, the cross section of the paddle is a triangle, and the width of the paddle gradually narrows from the inside to the outside. This structure can achieve both the stirring effect and the automatic discharging effect. The number of paddles is at least one, such as one, two, three, four, four or more, etc., preferably 2 or more. Preferably, the outermost end of the paddle is less than or equal to two centimeters from the inner cavity wall of the two-in-one kettle, such as one centimeter, one and a half centimeters, less than one centimeter, etc. The upper end of the stirring paddle rod body passes through the top cover 4 of the two-in-one kettle and is connected to the stirring motor 5. The stirring motor is fixed on the base 6, and the base and the top cover are connected by the lifting rod 61 and the stabilizing rod 7. The base is a hollow structure surrounded by an outer shell. A plurality of through holes are provided on the outer shell of the base. The through holes are respectively used to install the lifting rod and the stabilizing rod. The lifting rod is connected to the control system to achieve the up and down lifting and stirring of the base, so that the stirring is more sufficient and thorough. The stabilizing rod is to ensure the stability of the base during the lifting process. The lifting rod and the stabilizing rod are both arranged vertically, one end of which is arranged in the through hole of the base, and the other end is fixed on the top cover. There are at least two lifting rods, and they are preferably symmetrically arranged. There are at least two stabilizing rods, and the upper ends of the stabilizing rods are preferably connected to each other to play a better stabilizing role.

[0060] Furthermore, the two-in-one kettle is provided with a resin precipitation outlet 81, an air inlet 82, an exhaust port 83, a water inlet 84, a discharge port 15, and may also be provided with a pressure gauge port 85 and a window 86. Except that the discharge port is arranged at the lower part of the two-in-one kettle, the resin precipitation outlet 81, the air inlet 82, the exhaust port 83, the water inlet 84, the pressure gauge port 85 and the window 86 are all arranged at the upper part or top of the two-in-one kettle, for example, they can be arranged at the lower half of the neck 8. The resin precipitation outlet of the two-in-one kettle is connected to the discharge port of the disperser 9, the water inlet of the disperser is connected to the water inlet pipe 10, a flow regulating valve 101 and a flow meter 102 are installed on the water inlet pipe, the other end of the water inlet pipe is connected to the water outlet of the water inlet pump 23, the water inlet of the water inlet pump is connected to the water outlet 126 of the water storage tank through the water inlet pipe, the feed port of the disperser is connected to the feed pipe 11, the other end of the feed pipe is connected to the discharge port of the feed pump 13, and a flow regulating valve 111 and a flow meter 112 are installed on the feed pipe. The air inlet of the two-in-one kettle is connected to the nitrogen pipeline 821, and a nitrogen valve 822 is provided on the nitrogen pipeline. The exhaust port of the two-in-one kettle is connected to the exhaust pipeline, and an exhaust valve 831 is provided on the exhaust pipeline. The water inlet of the two-in-one kettle is connected to the ultrapure water pipeline 841, and a flow regulating valve 842 and a flow meter 843 are provided on the ultrapure water pipeline. The pressure gauge port of the two-in-one kettle is equipped with a pressure gauge 851.

[0061] Furthermore, a discharge pipe 17 extends outward from the discharge port, and the discharge pipe is arranged horizontally. There is a discharge rod 18 in the discharge pipe, and the end of the discharge rod is located outside the discharge pipe. There is a baffle 19 at the top of the discharge rod. The discharge port and the baffle at the top of the discharge rod are circular structures. Preferably, the baffle and the discharge port are seamlessly fitted. A discharge port 20 is provided at the bottom of the discharge pipe. Preferably, the ratio of the diameter of the discharge port and the discharge port to the height of the two-in-one kettle cavity is 1:3. The baffle of the discharge rod is used to block the discharge port. When no material is discharged, the baffle is moved to the discharge port to block the discharge port. When discharging, the discharge rod is pulled to open the discharge port, and the discharge port and the discharge port are connected to realize discharging. Preferably, the discharge rod is connected to a hydraulic control system to realize automatic unloading.

[0062] Furthermore, the two-in-one kettle is provided with a jacket 25, the lower part of the jacket has a liquid inlet 251, and the upper part has a liquid outlet 252, which are respectively connected to the temperature control device 28 through the liquid inlet pipe 26 and the liquid outlet pipe 27. The two-in-one kettle is also provided with support legs 29 and a support base 30, and the support legs and the support base are connected. The number of the support legs and the support base is at least two.

[0063] Furthermore, the bottom of the two-in-one kettle is connected to the chassis 21, and the two-in-one kettle and the chassis are connected. The upper part of the chassis is a planar structure, the lower part is a pot bottom structure, and the inside of the chassis is a hollow cavity. A filtering structure is provided on the top of the chassis, and the filtering structure includes a filter plate 211, which is a circular flat plate with holes to provide support for the filter cloth. A filter cloth 212 is provided on the filter plate, and a filter cloth cover plate 213 is provided on the upper part of the filter cloth. The filter cloth cover plate is annular and buckled on the filter cloth to fix the filter cloth on the upper part of the filter plate. Two chassis extension rods 217 are symmetrically arranged on the side wall of the chassis, and a chassis lifting rod 216 is connected to the chassis extension rod. The other end of the chassis lifting rod is connected to the two-in-one kettle, and the lifting rod is connected to the hydraulic control system to realize the lifting of the chassis. The chassis is seamlessly fitted with the two-in-one kettle. Preferably, a circle of annular baffles 16 is provided on the bottom side wall of the two-in-one kettle. When the chassis is raised to the highest point, the cover plate 213 of the filter cloth is seamlessly fitted with the annular baffles 16, and the upper edge of the chassis is fixed to the lower edge slot of the two-in-one kettle by a buckle to prevent leakage. When replacing the filter cloth, remove the buckle, lower the chassis to separate it from the two-in-one kettle. The annular baffle is installed below the discharge port, preferably at the lower edge of the discharge port. When the stirring paddle is lowered to the lowest point, the distance between the lowest point of the stirring paddle and the upper edge of the annular baffle 16 is less than or equal to one centimeter.

[0064] Furthermore, a water outlet 214 is provided at the lowest part of the chassis for discharging the water after washing, and a water outlet valve is provided on the water outlet. The water outlet is connected to the inlet of the water return pump 14 through the water return pipe 22, the water outlet of the water return pump is connected to the water inlet of the three-way connection, the three-way water outlet is connected to the water return pipe 22 and the drain pipe 24 respectively, the other end of the water return pipe is connected to the water return port 122 of the water storage tank, the water return pipe is equipped with a flow regulating valve 221 and a flow meter 222, the drain pipe is equipped with a ball valve 241 and a TDS detection probe 311, and the TDS detection probe is connected to the TDS detector 31 through a data transmission line 312. Three universal wheels 215 are also provided at the bottom of the chassis for easy movement.

[0065] Further, the water tank is a hollow structure with a cavity inside. The water tank can be of any shape without special requirements. Preferably, the middle part of the water tank is a cylindrical structure, the upper part is an inverted pot bottom type, and the lower part is a pot bottom type. The top or upper part of the water tank is provided with a manhole 121, a return water port 122, a water inlet 123, a liquid level meter port 124, and a pressure balance port 125. The bottom of the water tank is provided with a water outlet 126 and a support leg 127. The function of the manhole of the water tank is to facilitate cleaning. A cover plate 1211 is provided at the manhole, a movable cover plate 1251 is provided at the pressure balance port, and there are 3 support legs of the water tank. The water inlet 123 of the water tank is connected to an ultrapure water pipeline 1231, and a flow regulating valve 1232 and a flow meter 1233 are provided on the ultrapure water pipeline. A liquid level meter 32 is installed at the liquid level meter port, and the liquid level meter is connected to a display screen 321 and an alarm 322 through a data transmission line 323.

[0066] Preferably, the inner surface of the two-in-one kettle, the surface of the stirring paddle rod and the paddle blades, the surface of the baffle at the top of the discharge rod, the inner surface of the bottom cavity, the surface of the filter plate and the filter cloth cover plate, and the inner surfaces of the water inlet pump, the return pump and the feed pump are all coated with polytetrafluoroethylene.

[0067] In addition to the equipment structure described above, the water pump, feed pump, temperature control device, stirring motor, pressure gauge, flow regulating valve, flow meter, liquid level meter, etc. used in the utility model are all conventional equipment in the field, and will not be described here. The structure of the disperser mixer used in the utility model can refer to the equipment disclosed in CN 109749099 B.

[0068] Example 2

[0069] The resin precipitation and washing device described in Example 1 is used to precipitate and wash the resin reaction liquid, and the steps are as follows:

[0070] (1) Before precipitation, ensure that the flow control valve 842, nitrogen valve 822, flow control valve 101, flow control valve 111, flow control valve 1232, flow control valve 221, and drain pipe ball valve 241 are in the closed state, and the two-in-one kettle exhaust valve is in the open state.

[0071] (2) Open the water inlet valve 1232 on the ultrapure water pipeline of the water storage tank 12, inject deionized ultrapure water into the water storage tank first, and then close the water inlet valve 1232 after injecting the ultrapure water.

[0072] (3) Turn on the stirring motor and make it rotate forward to stir. You can also raise and lower the motor to make the stirring more thorough and adjust it to the appropriate speed.

[0073] (4) When precipitation begins, the water outlet 214 of the two-in-one kettle is closed, the two-in-one kettle water inlet pump 23 and the return pump 14 are turned on, the flow rate of the water inlet pipe 10 is adjusted by the flow regulating valve 101, the flow rate of the return pipe 22 is adjusted by the flow regulating valve 221, the feed pump 13 is turned on, and the flow rate of the feed pipe 11 is adjusted by the flow regulating valve 111.

[0074] (5) After the precipitation is completed, the flow regulating valve 111, the feed pump 13, the flow regulating valve 221, and the return pump 14 are closed in sequence. After the required amount of water for resin washing is added to the two-in-one kettle, the water inlet valve 101 and the water inlet pump 23 are closed.

[0075] (6) Start washing, open the two-in-one kettle jacket temperature control device 28, set the heating temperature, and after heating, stirring and washing, close the stirring paddle 3, close the exhaust valve, open the nitrogen valve 822, pass nitrogen into the two-in-one kettle, start the return pump 14, open the drain valve at the outlet 214, record the TDS detection value of the washing water, and after all the washing water in the two-in-one kettle is discharged, open the exhaust port 83, and close the nitrogen valve 822, the drain valve, and the return pump 14 in turn.

[0076] (7) Turn on the water inlet pump 23 and the flow regulating valve 101. After the required amount of water for resin washing is added to the two-in-one kettle, close the flow regulating valve 101 and the water inlet pump 23, turn on the stirring paddle 3, rotate forward for stirring, and repeat step (6).

[0077] (8) After the precipitated water in the water storage tank is used up, open the flow regulating valve 842 on the ultrapure water pipeline 841 of the two-in-one kettle. After the required amount of water for resin washing is added to the two-in-one kettle, close the flow regulating valve 842, turn on the stirring paddle 3, raise and lower it and rotate it in the forward direction to stir, and continue to repeat step (6).

[0078] (9) Washing water recovery: When the TDS detection value of the washing water reaches 100, close the drain pipe ball valve 241, open the flow regulating valve 221, and recover the washing water to the water storage tank.

[0079] (10) When the TDS value of the washing water reaches below 5, the washing is finished.

[0080] (11) Discharging begins. A receiving container is placed below the discharge port 20. After ensuring that the inner chamber 2 of the two-in-one reactor has returned to normal pressure, the baffle 19 at the discharge port is opened, the stirring paddle 3 is turned on, and reverse rotation is started to complete automatic discharging.

[0081] Example 3

[0082] The resin was precipitated and washed according to the steps of Example 2. The resin reaction liquid used was a reaction liquid containing polyamic acid ester resin obtained by the reaction, and its concentration was 10wt%. The flow rate of the water inlet pipe was 35L / min, the flow rate of the feed pipe was 2L / min, the mass ratio of water to resin was 50:1 during each washing, the washing temperature was 60°C, the stirring speed was 80r / min, and the washing time was 1h. When the washing water was recovered, the flow rate of the return pipe 22 was 25L / min.

[0083] Example 4

[0084] The resin was precipitated and washed according to the method of Example 3, except that the concentration of the reaction solution of the polyamic acid ester resin was 15 wt %.

[0085] Example 5

[0086] The resin was precipitated and washed according to the method of Example 3, except that the concentration of the reaction solution of the polyamic acid ester resin was 20 wt %.

[0087] Example 6

[0088] The resin was precipitated and washed according to the method of Example 3, except that the concentration of the reaction solution of the polyamic acid ester resin was 25 wt %.

[0089] Example 7

[0090] The resin was precipitated and washed according to the method of Example 3, except that the concentration of the reaction solution of the polyamic acid ester resin was 30 wt %.

[0091] Example 8

[0092] The resin was precipitated and washed according to the method of Example 3, except that the concentration of the reaction solution of the polyamic acid ester resin was 35 wt %.

[0093] Example 9

[0094] The resin was precipitated and washed according to the method of Example 3, except that the concentration of the reaction solution of the polyamic acid ester resin was 40 wt %.

[0095] Example 10

[0096] The resin was precipitated and washed according to the method of Example 3, except that the concentration of the reaction solution of the polyamic acid ester resin was 45 wt %.

[0097] Embodiment 11

[0098] The resin was precipitated and washed according to the method of Example 3, except that the flow rate of the feed pipe was 2.5 L / min.

[0099] Example 12

[0100] The resin was precipitated and washed according to the method of Example 3, except that the flow rate of the feed pipe was 3.0 L / min.

[0101] Example 13

[0102] The resin was precipitated and washed according to the method of Example 3, except that the flow rate of the feed pipe was 3.5 L / min.

[0103] Embodiment 14

[0104] The resin was precipitated and washed according to the method of Example 3, except that the flow rate of the feed pipe was 4.0 L / min.

[0105] Embodiment 15

[0106] The resin was precipitated and washed according to the method of Example 3, except that the flow rate of the feed pipe was 4.5 L / min.

[0107] Example 16

[0108] The resin was precipitated and washed according to the method of Example 3, except that the flow rate of the feed pipe was 5.0 L / min.

[0109] After the polyamic acid ester resin obtained in Example 3-16 was dried, the particle size and total ion content of the resin particles were detected, wherein the particle size was detected by a BT-9300S laser particle size distribution analyzer, and the total ion content was detected by an inductively coupled plasma mass spectrometer. The results are shown in Table 1.

[0110]

[0111] It can be seen from the results of the resin particle size and total ion content in Table 1 that the resin precipitation washing device and precipitation washing method of the utility model can better precipitate the polyimide precursor resin from the reaction liquid to form uniform powdered resin particles, and can more thoroughly wash and remove impurity ions in the resin. The resin ion content index fully meets the performance requirements of advanced semiconductor packaging materials.

Claims

1. A resin precipitation washing device, characterized in that: The invention comprises a two-in-one kettle for resin precipitation and washing, a chassis and a water storage tank, wherein the two-in-one kettle comprises an inner cavity with openings at both ends and a top cover located on the upper part of the inner cavity, a stirring paddle is arranged in the inner cavity, the upper end of the stirring paddle passes through the top cover of the two-in-one kettle and is connected with a stirring motor, the stirring motor is fixed on a liftable base, a resin precipitation outlet, a water inlet and a material outlet are arranged on the two-in-one kettle, a disperser is installed at the resin precipitation outlet, the disperser is connected with the water storage tank and the material feeding pipe respectively, the bottom of the two-in-one kettle is connected with the chassis, a filtering structure is arranged on the top of the chassis, a water outlet is arranged at the bottom of the chassis, the water outlet is connected with the inlet of a return water pump, the return water pump outlet is connected with the water inlet of a tee, one water outlet of the tee is connected with the return water pipe, the other water outlet is connected with the drain pipe, and the return water pipe is connected with the water storage tank.

2. The precipitation washing device according to claim 1, characterized in that: An annular baffle is arranged on the bottom side wall of the two-in-one kettle, and the annular baffle is seamlessly fitted with the filtering structure.

3. The precipitation washing device according to claim 1 is characterized in that: The filtering structure comprises a filtering plate, a filtering cloth is arranged on the upper part of the filtering plate, and a covering plate is arranged on the upper part of the filtering cloth.

4. The precipitation washing device according to claim 1 is characterized in that: A lifting rod is connected between the two-in-one kettle and the chassis, and the lifting rod drives the chassis to rise and fall under the control of the control system.

5. The precipitation washing device according to claim 1 is characterized in that: The liftable base is connected to the top cover through a lift rod and a stabilizer rod, one end of the lift rod and the stabilizer rod are both arranged in the base, and the other ends are fixed on the top cover. The lift rod is connected to a control system to control the lifting and lowering of the liftable base.

6. The precipitation washing device according to claim 1 is characterized in that: The stirring paddle comprises a stirring rod and a paddle blade. The paddle blade is located at the lower end of the stirring rod. The cross section of the paddle blade is triangular, and the size of the paddle blade gradually decreases from one end to the other end.

7. The precipitation washing device according to claim 1 is characterized in that: The outermost side of the paddle is less than or equal to two centimeters away from the inner wall of the two-in-one kettle.

8. The precipitation washing device according to claim 1 is characterized in that: A discharge pipe is extended outward from the discharge port, a discharge rod is arranged in the discharge pipe, a baffle is arranged on the top of the discharge rod, the baffle is seamlessly fitted with the discharge port, the end of the discharge rod is located outside the discharge pipe, and a discharge port is arranged at the bottom of the discharge pipe. When discharging, the discharge rod is pulled to discharge the material from the discharge port.

9. The precipitation washing device according to claim 1 is characterized in that: The two-in-one kettle is provided with at least one of an air inlet, an air outlet, a pressure gauge, a viewing window, a heat-insulating jacket, a supporting leg, and a supporting base, and the air inlet is connected to a nitrogen pipeline.

10. The precipitation washing device according to claim 1, characterized in that: The drainage pipe is provided with a TDS detection probe, which is connected to the TDS detector through a data transmission line; the water storage tank is provided with a manhole, a water return port, a water inlet, a liquid level gauge, a pressure balance port, supporting legs, and a water outlet, a cover plate is provided at the manhole, a movable cover plate is provided at the pressure balance port, the water inlet is connected to the ultrapure water pipeline, and the liquid level gauge is connected to the display screen and the alarm through the data transmission line.

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