An apparatus, a method for continuous purification of organic solids and applications

Abstract

The present application relates to the technical field of organic solid purification, and particularly relates to a device for continuous purification of organic solids, a purification method and application, the device comprising a feeding system, a device body, and a discharging system, the device body being sequentially provided with a tower top clarification section, a purification section, and a tower bottom dispersion section from top to bottom, a plurality of baffles being arranged in the tower top clarification section, a plurality of sieve plate assemblies being arranged in the purification section, and a disperser being arranged in the tower bottom dispersion section, the organic phase and the aqueous phase being countercurrently contacted in the device, and the impurity content of the organic solids being less than 100 ppb after being purified by the device, while the personnel operation intensity is reduced and the production time is greatly saved.

Description

Technical Field

[0001] This invention relates to the field of organic solids purification technology, and more particularly to an apparatus, purification method and application for continuous purification of organic solids. Background Technology

[0002] High-purity organic solids used in the electronics industry, especially in integrated circuits and new display technologies, include: tris(8-hydroxyquinoline)aluminum (Alq3), 4,4',4''-tris(carbazole-9-yl)triphenylamine (TCTA), tris(2-phenylpyridine)iridium (Ir(ppy)3), and di(1-phenylisoquinoline)iridium (Ir... (piq)3), N,N'-diphenyl-N,N'-di(1-naphthyl)-1,1'-biphenyl-4,4'-diamine (NPB), 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (BCP), ultraviolet absorbers (such as 2-hydroxy-4-methoxybenzophenone), organic fluorescent whitening agents (such as stilbene biphenyl derivatives); photochromic functional organic solids: such as thienylspiropyran, thienyl styrenic acid anhydride, dithienylethylene photochromic compounds, thienopyran; medium molecular weight photoresist resins and functional monomer solids: such as phenolic resins with molecular weights of 1000-5000, polyhydroxystyrene resins (PHS), acrylate photoresist matrix resins, cyclic olefin copolymer resins, photoresist resins containing ester / hydroxyl protecting groups, etc. In the production of the above organic solids, the purification process is crucial. Removing small molecule impurities and trace metal ions is not only a core requirement for improving product purity, but also plays a crucial role in improving product performance.

[0003] In existing technologies, the removal of such impurities often employs intermittent washing processes, with pure water being the most commonly used washing solvent. This process is also known as water washing. Specifically, the organic solid is dissolved in an organic solvent immiscible with water (such as benzene, toluene, xylene, trimethylbenzene, ethyl acetate, cyclohexanone, cyclohexane, n-hexane, and methyl isobutyl ketone), then placed in a reaction vessel and stirred with water. The transfer of impurities is achieved by utilizing the different solubilities of small molecule impurities and metal ions in water and organic solvents. After settling and separating into layers, the aqueous phase is discharged. This process is repeated approximately 10-15 times to reduce the content of small molecule impurities and metal ions in the organic solid.

[0004] Intermittent water washing purification process has the following significant drawbacks:

[0005] 1. Low efficiency: The water washing and purification operation requires multiple washing, settling and stratification, and draining, which takes a long time and results in low equipment utilization. 2. The operation is cumbersome, involves many manual intervention steps, and is prone to human error; 3. The purity fluctuates greatly, and it is difficult to keep the operating parameters such as the number of washings and stirring intensity completely consistent between batches, resulting in fluctuations in the impurity concentration of different batches of products; 4. High solvent loss: organic solvents are prone to volatilization during multiple drainage processes, and there is material residue loss when switching batches. 5. The labor intensity is high, making it unsuitable for large-scale industrial production.

[0006] Alternatively, CN119569667A discloses a method and system for continuous extraction and washing of crude benzomelamine. This method involves mixing the crude benzomelamine solid with water to form a continuously flowing slurry, which is then continuously fed in fluid form. The slurry is then subjected to countercurrent contact with washing water within a rotary extraction tower to achieve continuous extraction and washing of the crude benzomelamine. Simultaneously, a screw conveyor is installed at the bottom of the rotary extraction tower to facilitate the settling of the washed benzomelamine solid to the lower part of the tower for continuous discharge and subsequent drying. In essence, a rotary extraction tower is used for continuous extraction and washing of crude benzomelamine. The countercurrent contact between pure water and the slurry effectively removes impurities such as benzamide and potassium hydroxide, and the screw conveyor ensures continuous discharge of the solid. The technical solution involves continuous water washing and uses organic solvents, but it is only applicable to crude benzo-melamine products. Furthermore, it does not mention whether metal ions are removed, and the highest impurity removal rate is only 97.8%, which is far from reducing the level to ppb. Therefore, it cannot be applied to the electronics industry, especially the fields of integrated circuits and new displays.

[0007] For example, CN116217354A discloses an efficient and green synthesis method and product for liquid crystal monomers. The synthesis method includes the following steps: S1. In the preparation of biphenyl monomers using the Suzuki coupling reaction or ether monomers using the Williamson reaction, the raw materials used for the Suzuki coupling reaction or Williamson reaction are first added to water, using water as the reaction medium, and a stainless steel autoclave as the reaction equipment; S2. Then, the autoclave is sealed, stirring is started, the stainless steel autoclave is purged with nitrogen, the temperature is raised, the reaction is completed, and then the temperature is lowered and the material is discharged. The solid is obtained by suction filtration and returned to the stainless steel autoclave; S3. Water is added again, stirring is started, the temperature is raised, the mixture is washed with water, cooled, and filtered again to obtain the liquid crystal monomer product. Although this technical solution uses water as the reaction medium, reducing the use of organic solvents, the purity of the product is at most 99.9%, and the impurity content cannot be controlled at the ppb level.

[0008] Based on the above-mentioned existing technology, there are technical problems that existing devices cannot solve, such as low purification efficiency and large purity fluctuations of organic solids. Summary of the Invention

[0009] To solve the above-mentioned technical problems, the present invention provides an apparatus for continuous purification of organic solids, comprising: Feeding system: includes organic phase feeding unit and aqueous phase feeding unit; Equipment body: Vertical closed tower structure, with a clarification section at the top, a purification section, and a dispersion section at the bottom of the tower arranged sequentially from top to bottom; The discharge system includes an organic phase discharge unit and an aqueous phase discharge unit. The top clarification section of the tower is equipped with several baffles; the purification section is equipped with several sieve plate assemblies; and the bottom dispersion section of the tower is equipped with a disperser. The organic phase and the aqueous phase are in countercurrent contact within the equipment, and the organic solid, after being purified by the equipment, has an impurity content of less than 100 ppb.

[0010] Furthermore, the impurities are water-soluble impurities, including but not limited to metal ions.

[0011] Furthermore, after purification by the aforementioned equipment, the impurity content of the organic solid is less than 80 ppb.

[0012] Furthermore, the device also includes a control system connected to the device for monitoring and regulating the operation of the device.

[0013] Furthermore, the organic phase feeding unit includes an organic phase feed pipe.

[0014] Furthermore, the organic phase feed pipe is connected to the side wall of the bottom dispersion section of the tower, and is used to feed the organic solvent phase, which is immiscible with water and contains dissolved organic solids, into the equipment body.

[0015] Furthermore, the organic solvent includes, but is not limited to, one or more of benzene, toluene, xylene, trimethylbenzene, ethyl acetate, cyclohexanone, cyclohexane, n-hexane, and methyl isobutyl ketone.

[0016] Furthermore, the outlet end of the organic phase feed pipe is connected to a disperser installed in the dispersion section at the bottom of the tower to disperse the organic phase into droplets.

[0017] Furthermore, the aqueous phase feeding unit includes an aqueous phase feeding pipe.

[0018] Furthermore, the aqueous feed pipe is connected to the side wall of the clarification section at the top of the tower, and is used to send pure water into the equipment body to achieve countercurrent contact between the organic phase and the aqueous phase within the equipment body.

[0019] Furthermore, a preheating device is installed on the organic phase feed pipe or the aqueous phase feed pipe of the aqueous phase feed unit, with a preheating temperature of 25-40℃, to improve the subsequent impurity removal effect.

[0020] Furthermore, the material of the device body includes, but is not limited to, stainless steel, stainless steel lined with fluoroplastics, and perfluoroplastics.

[0021] Furthermore, the fluoroplastics include, but are not limited to, perfluoroalkoxyalkanes and polytetrafluoroethylene.

[0022] Furthermore, the height ratio of the equipment body, purification section (4), top clarification section (3), and bottom dispersion section (5) is (4-15): (3-10): (0.5-2.5): (0.3-2.5).

[0023] Furthermore, the total height of the device body is 4.0-15.0m.

[0024] Furthermore, the height of the purification section is 3.0-10m.

[0025] Furthermore, the height of the clarification section at the top of the tower and the dispersion section at the bottom of the tower are independently 0.3-2.5m.

[0026] Furthermore, the height of the clarification section at the top of the tower and the dispersion section at the bottom of the tower are preferably 1.0-1.2m.

[0027] Furthermore, the diameter ratio of the purification section (4), the top clarification section (3), and the bottom dispersion section (5) is (0.15-1.6):(0.3-1.8):(0.3-1.7).

[0028] Furthermore, the diameter of the purification section is 0.15-1.6m.

[0029] Furthermore, the diameter of the clarification section at the top of the tower is 0.3-1.8m.

[0030] Furthermore, the diameter of the dispersion section at the bottom of the tower is 0.3-1.7m.

[0031] Furthermore, the diameters of the clarification section at the top of the tower and the dispersion section at the bottom of the tower are preferably 0.45-0.8m.

[0032] Furthermore, the diameters of the clarification section at the top of the column and the dispersion section at the bottom of the column are independently greater than or equal to the diameter of the purification section.

[0033] Furthermore, the screen plate assembly is a vibrating screen plate assembly or a rotating screen plate assembly.

[0034] Furthermore, the vibrating screen plate assembly includes a vibrating screen plate body, a vibrating connecting rod, and a vibration drive mechanism. Furthermore, the vibration drive mechanism is connected to a control system outside the equipment body to drive the liquid inside the tower to vibrate periodically.

[0035] Furthermore, the material of the vibrating screen plate body includes, but is not limited to, stainless steel, stainless steel lined with PFA, PTFE, or pure PTFE.

[0036] Furthermore, the vibrating screen plate body is provided with a number of screen holes.

[0037] Furthermore, the sieve aperture is 2-10 mm to improve the redispersion of droplets and enhance the impurity removal effect.

[0038] Furthermore, the aperture of the sieve holes is preferably 4-6 mm.

[0039] Furthermore, the opening ratio of the vibrating screen plate body is 15-25%.

[0040] Furthermore, the opening ratio of the vibrating screen plate body is preferably 15-18%.

[0041] Furthermore, the spacing between adjacent vibrating screen plates is 100-400mm.

[0042] Furthermore, the spacing between adjacent vibrating screen plates is preferably 120-150 mm.

[0043] Furthermore, the vibrating screen plate body is detachable, making it easy to clean and replace.

[0044] Furthermore, the vibration drive mechanism is either a mechanical vibration type or a pneumatic vibration type.

[0045] Furthermore, the vibration frequency of the vibration drive mechanism is 5-15Hz and the vibration amplitude is 3-10mm. If the vibration frequency is too low, the droplets will re-merge and agglomerate; if it is too high, the droplet atomization efficiency will decrease, both of which will result in the failure of impurity removal.

[0046] Furthermore, the vibration frequency of the vibration drive mechanism is preferably 8-12Hz, and the vibration amplitude is preferably 6-8mm.

[0047] Furthermore, the vibration frequency and amplitude can be adaptively adjusted by the viscosity of the organic phase. That is, the greater the viscosity of the organic phase, the smaller the vibration frequency and amplitude, and the smaller the viscosity of the organic phase, the greater the vibration frequency and amplitude. The two are inversely proportional.

[0048] Furthermore, the rotating screen assembly includes a rotating screen body, a rotating main shaft, and a rotating drive mechanism.

[0049] Furthermore, the rotary drive mechanism is connected to the control system, which drives the rotary spindle to rotate the vibrating screen plate body, randomly disturbing the liquid layer to achieve mixing between the upper and lower phases and enhancing the two-phase mass transfer efficiency.

[0050] Furthermore, the rotating sieve plate body is provided with a plurality of sieve holes.

[0051] Furthermore, the aperture of the sieve holes is 2-10 mm.

[0052] Furthermore, the aperture of the sieve holes is preferably 4-6 mm.

[0053] Furthermore, the opening ratio of the rotating screen plate body is 15-25%.

[0054] Furthermore, the opening ratio of the rotating screen plate body is preferably 15-18%.

[0055] Furthermore, the spacing between adjacent rotating screen plates is 100-400mm.

[0056] Furthermore, the spacing between adjacent rotating screen plates is preferably 120-150 mm.

[0057] Furthermore, the rotational speed of the rotating sieve assembly is 30-120 r / min. If the speed is too low, the droplets will re-merge and agglomerate; if it is too high, the droplet atomization efficiency will decrease, both of which will result in the failure of impurity removal.

[0058] Furthermore, the rotating screen plate body is detachable, making it easy to clean and replace.

[0059] Furthermore, the rotating screen plate body is located on the rotating main shaft, the horizontal inclination angle of the mounting plane of the rotating screen plate body is greater than 0°, and the inclination direction of each layer of the rotating screen plate body is different.

[0060] Furthermore, the horizontal inclination angle of the mounting plane of the rotating screen plate body is preferably 2-5°.

[0061] Furthermore, the rotation drive mechanism of the rotating screen plate assembly is a variable frequency motor driven type with a rotation speed of 30-120 r / min.

[0062] Furthermore, the rotational speed can be adaptively adjusted by the viscosity of the organic phase; that is, the greater the viscosity of the organic phase, the lower the rotational speed, and the lower the viscosity of the organic phase, the greater the rotational speed, and the two are inversely proportional. The tilted rotating screen plate body generates irregular upper and lower liquid layer disturbances, continuously renewing the two-phase contact interface, enhancing the dispersion and aggregation of droplets, and achieving a mass transfer efficiency comparable to that of a vibrating screen plate assembly. Moreover, there is no axial vibration during operation, resulting in more stable equipment operation and lower noise, which can effectively reduce the risk of emulsification caused by excessively fine droplets.

[0063] Furthermore, the spacing between each of the baffles is 200-300 mm. The higher the clarification section at the top of the column, the more baffles there are. This is to prolong the residence time of the organic phase, promote droplet coalescence, and prevent the organic phase from carrying away the aqueous phase, which would lead to a decrease in purity.

[0064] Furthermore, the baffles are arranged in an alternating pattern of circular baffles and annular baffles to prolong the residence time of the organic phase and promote droplet coalescence. At the same time, they also cause the material to follow an S-shaped path in the clarification section at the top of the tower, increasing the residence time and improving the stratification effect.

[0065] Furthermore, the circular baffle is arranged at the center of the cylinder of the clarification section at the top of the tower, and its diameter is 45-55% of the diameter of the clarification section at the top of the tower.

[0066] Furthermore, the annular baffle is connected to the inner wall of the clarification section at the top of the tower, and the diameter of the central circular hole is 40-55% of the diameter of the clarification section at the top of the tower.

[0067] Furthermore, the device body is also wrapped with an insulation layer to maintain a stable temperature inside the tower.

[0068] Furthermore, a first drain outlet is provided below the clarification section at the top of the tower to periodically discharge the deposited trace amounts of solid impurities.

[0069] Furthermore, a guide cone and a disperser are provided in the dispersion section at the bottom of the tower.

[0070] Furthermore, the disperser is connected to the outlet end of the organic phase feed pipe of the organic phase feeding unit, and is used to disperse the organic phase into droplets with a diameter of 0.5-5mm. By controlling the droplet size, the impurity removal effect is enhanced. Meanwhile, as the droplets flow upward within the device body, the droplets dispersed by the disperser may also merge and agglomerate. At this time, the droplets are further dispersed by combining the vibrating screen plate assembly or rotating screen plate assembly with the baffle plate to ensure that the organic phase exists in the form of uniformly dispersed droplets throughout the entire device body, thereby ensuring the final impurity removal effect.

[0071] Furthermore, the disperser is connected to the outlet end of the organic phase feed pipe of the organic phase feed unit, and is used to disperse the organic phase into droplets with a diameter of 1-3 mm.

[0072] Furthermore, the guide cone is inclined at an angle of 15-45° to guide the aqueous phase towards the aqueous phase outlet and prevent the aqueous phase from stagnating.

[0073] Furthermore, a second drain outlet is provided below the flow guide cone.

[0074] Furthermore, the organic phase discharge unit includes an organic phase discharge pipe.

[0075] Furthermore, the aqueous phase discharge unit includes an aqueous phase discharge pipe.

[0076] Furthermore, the top of the clarification section at the top of the tower is connected to an organic phase discharge pipe, and the bottom dispersion section at the bottom of the tower is connected to an aqueous phase discharge pipe.

[0077] Furthermore, the organic phase discharge pipe is located above the horizontal space of the aqueous phase feed pipe.

[0078] Furthermore, the aqueous phase discharge pipe is located below the organic phase feed pipe in the horizontal space.

[0079] Furthermore, the control system includes a monitoring system and a control system.

[0080] Furthermore, the monitoring system includes an interface detector, an online purity detector, a flow sensor, and a temperature sensor, which are used to monitor the phase interface position at the top of the column, the purity of the organic phase output, the inlet and outlet flow rates, and the temperature inside the column, respectively, and feed the monitoring signals back to the control system to realize automatic parameter adjustment.

[0081] Furthermore, the control system includes a programmable logic controller (PLC controller), which is electrically connected to the interface detector, the online purity detector, the flow sensor, the temperature sensor, the vibration drive mechanism, the rotation drive mechanism, and the conveying pump of the feeding unit. When the interface detector detects that the parameters deviate from the preset range, the PLC controller is used to adjust the valve opening at the feeding and discharging ends, and adjust the rotation speed or vibration frequency of the screen plate.

[0082] The present invention also provides a purification method, wherein the purification method involves continuously purifying organic solids using the aforementioned equipment for continuous purification of organic solids.

[0083] Furthermore, the purification method includes the following steps: Step 1: Dissolve the organic solid to be purified in an organic solvent that is immiscible with water to prepare an organic phase solution; Step 2: The organic phase solution is fed into the dispersion section at the bottom of the column and dispersed into droplets, while pure water is fed into the clarification section at the top of the column. The organic phase and the aqueous phase are in countercurrent contact. Step 3: Mass transfer is enhanced by the sieve plate assembly, causing impurities in the organic phase to transfer to the aqueous phase; Step 4: The purified organic phase is separated in the clarification section at the top of the column, and the aqueous phase containing impurities is discharged from the dispersion section at the bottom of the column; Step 5: The purified organic phase is recovered by solvent and dried to obtain a high-purity organic solid.

[0084] Furthermore, the impurity content of the high-purity organic solid is below 100 ppb.

[0085] Furthermore, the organic solvent is selected from one or more of benzene, toluene, xylene, trimethylbenzene, ethyl acetate, cyclohexanone, cyclohexane, n-hexane, and methyl isobutyl ketone.

[0086] Furthermore, in step 2, the organic phase is dispersed into droplets with a diameter of 0.5-5 mm by a disperser; the ratio of the aqueous phase flow rate to the organic phase flow rate is (10-15):1.

[0087] Furthermore, in step 2, the organic phase is dispersed into droplets with a diameter of 0.5-5 mm by a disperser; the preferred ratio of the aqueous phase flow rate to the organic phase flow rate is 15:1.

[0088] Furthermore, the aqueous phase described in step 2 is preheated to 25-40°C before entering the aqueous phase feed pipe.

[0089] Furthermore, the vibration frequency of the vibrating screen plate assembly is 5-15Hz, and the vibration amplitude is 3-10mm; preferably, the vibration frequency is 8Hz and the amplitude is 6mm.

[0090] Furthermore, the rotational speed of the rotating screen assembly is 30-120 r / min; the horizontal inclination angle of the mounting plane of the rotating screen body is 2-5°.

[0091] Furthermore, the adjacent rotating screen plates have alternating opposite tilt directions.

[0092] Furthermore, the clarification section at the top of the tower is equipped with baffles to promote the coalescence and separation of organic phase droplets and prevent the organic phase from carrying water phase.

[0093] Furthermore, the monitoring system detects the interface, purity, flow rate, and temperature, and transmits the data to the control system to adjust the valve opening at the feed and discharge ends, as well as the rotation speed or vibration frequency of the screen plate.

[0094] Furthermore, the organic phase has a residence time of 15-20 minutes in the column and can operate continuously.

[0095] The present invention also provides a high-purity organic solid, which is a product obtained by purification using the above-mentioned equipment for continuous purification of organic solids, wherein the impurity content in the high-purity organic solid is less than 100 ppb.

[0096] Furthermore, the impurities include metal ions.

[0097] Furthermore, the high-purity organic solids include, but are not limited to, high-purity organic solids used in the electronics industry, especially in the fields of integrated circuits and new displays.

[0098] Furthermore, the high-purity organic solids include, but are not limited to, (2-hydroxy-4-methoxybenzophenone), tris(8-hydroxyquinoline)aluminum (Alq3), 4,4',4''-tris(carbazole-9-yl)triphenylamine (TCTA), tris(2-phenylpyridine)iridium (Ir(ppy)3), di(1-phenylisoquinoline)iridium (Ir(piq)3), N,N'-diphenyl-N,N'-di(1-naphthyl)-1,1'-biphenyl-4,4'-diamine (NPB), 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (BCP), ultraviolet absorbers, organic fluorescent whitening agents, photochromic functional organic solids, medium molecular weight photoresist resins, and functional monomer solids.

[0099] Furthermore, the ultraviolet absorber includes, but is not limited to, 2-hydroxy-4-methoxybenzophenone.

[0100] Furthermore, the organic fluorescent whitening agent includes, but is not limited to, stilbene biphenyl derivatives.

[0101] Furthermore, the photochromic functional organic solids include, but are not limited to, thienylspiropyran, thienyl succinic anhydride, dithienylethylene photochromic compounds, and thienopyran.

[0102] Furthermore, the medium molecular weight photoresist resin and functional monomer solids include, but are not limited to, phenolic resins, polyhydroxystyrene resins (PHS), acrylate photoresist matrix resins, cyclic olefin copolymer resins, and photoresist resin solids containing ester / hydroxyl protecting groups, with molecular weights of 1000-5000.

[0103] The beneficial effects of this invention are as follows: 1. This invention provides an apparatus, purification method, and application for continuous purification of organic solids. The apparatus includes a feeding system, an apparatus body, and a discharging system. The apparatus body is arranged from top to bottom as a top clarification section, a purification section, and a bottom dispersion section. The top clarification section is provided with several baffles; the purification section is provided with several sieve plate assemblies; and the bottom dispersion section is provided with a disperser. The organic phase and the aqueous phase are in countercurrent contact within the apparatus. After purification by the apparatus, the impurity content of the organic solids is less than 100 ppb, while simultaneously reducing the intensity of manual operation and significantly saving production time.

[0104] 2. The equipment for continuous purification of organic solids provided by this invention has the following advantages compared with the existing intermittent water washing process: 1) Breakthrough in Purification Efficiency: This invention addresses the problems of low efficiency, large purity fluctuations, and poor adaptability of existing batch processes. For example, existing batch processes require multiple water washing-concentration-resolution cycles in sequence. Processing 100kg of material requires 10 water washing cycles, with a total process time of up to 37 hours, effective purification time of 25 hours, and a daily capacity of only about 65kg. In contrast, this invention enables continuous purification, effectively replacing more than 10 batch washing cycles. It adopts a continuous countercurrent contact purification mode between the organic phase and the aqueous phase, combined with a mass transfer enhancement structure using vibrating or rotating screens. The full purification of 100kg of material can be completed in just 5 hours, with effective purification time only 1 / 5 of that of existing compliant processes. Daily capacity is increased by more than 7 times, solving the industry pain points of low efficiency and low equipment utilization in batch processes, and stably reducing impurity content to the ppb level. It is anti-clogging, has low maintenance costs, is adaptable to organic phase systems of different viscosities, and is suitable for industrial continuous production. 2) Improved Purification Stability: Existing intermittent processes can only reduce the average metal ion content of the product to 215 ppb after 5 water washes, which cannot meet the requirement of below 100 ppb. To meet the standard, another 5 water wash cycles are required, which takes more than 37 hours in total. Moreover, due to uncontrollable factors such as manual operation, stirring intensity, and settling effect, the more water washes, the higher the purity fluctuation between batches. In contrast, this invention continuously breaks and reorganizes droplets and dynamically updates the mass transfer boundary layer through vibration or rotating sieve plates. The mass transfer coefficient is significantly improved compared to ordinary intermittent stirring systems. A single continuous pass can achieve the purification effect equivalent to more than 10 intermittent water washes, stably reducing the metal ion content to below 100 ppb, and realizing the standardized and stable industrial production of high-purity organic solids. 3) Reduced operational intensity: Existing intermittent processes require multiple material transfers and lid openings, and 10 water washing cycles are needed to achieve the purification target. The entire process requires manual monitoring of liquid discharge, with a total on-duty time of up to 16 hours, resulting in high labor intensity and labor costs. This invention adopts a fully enclosed vertical tower structure, eliminating multiple material transfers and lid openings. At the same time, it achieves real-time adaptive control of phase interface, flow rate, purity, and temperature through a fully automatic monitoring and control system. No manual on-duty monitoring is required, and the total manual operation time is less than 0.5 hours, which significantly reduces the labor costs and labor intensity of industrial production. 4) Significantly Optimized Process: Existing batch processes require multiple concentration and reconstitution operations, necessitating 10 concentration and reconstitution cycles to achieve the purification target. This significantly increases the risk of material thermal degradation and is prone to material entrainment losses due to human error. The more washes, the higher the risk of material loss. This invention eliminates the concentration and reconstitution steps, achieving continuous purification in one step and reducing material loss. Furthermore, the detachable sieve structure and the equipment's drain outlet design effectively address the impact of trace solid impurities, preventing equipment blockage and ensuring continuous, trouble-free operation. The rotating sieve design also completely eliminates axial vibration, adapting to easily emulsified systems and further expanding the equipment's applicability. Its operational continuity is far superior to existing batch processes.

[0105] 3. The purification equipment and method of the present invention achieve continuous purification: adopting the countercurrent continuous contact mode of organic phase and aqueous phase, there is no need for batch waiting, the purification time of unit product is reduced by more than 70%, and only 20%-30% of the operation time of intermittent device is required. The dispersion section at the bottom of the tower and the clarification section at the top of the tower are equipped with sewage outlets for periodically discharging the deposited trace solid impurities. The processing capacity is stable and suitable for large-scale continuous industrial production. 4. The purification equipment and method of this invention have high mass transfer efficiency and stable purity: the vibrating or rotating sieve plate assembly enhances mass transfer, and the equivalent theoretical stage height of each sieve plate is 0.3-0.6m. Each theoretical stage is equivalent to one intermittent washing process. Different equipment heights are equivalent to replacing 5-10 traditional intermittent washing processes. Moreover, the parameters are adjusted in real time through the monitoring and control system, which solves the problem of large purity fluctuations in intermittent processes. 5. The purification equipment of this invention is resistant to clogging and has low maintenance costs: the dispersion section at the bottom of the tower has no filling structure, and with the detachable sieve plate and drain port, it can effectively discharge trace solid impurities and avoid clogging; the sieve plate assembly has no complex moving parts, resulting in low maintenance costs. 6. The purification method of this invention has low solvent loss: Compared with the multiple washing of the batch reactor, the closed tower structure reduces the evaporation of organic solvents and significantly reduces production costs. 7. The purification equipment of this invention has strong adaptability: by adjusting the parameters of the sieve plate, it can be adapted to organic phase systems with different viscosities and can cope with the influence of trace solid impurities, with a wide range of applications; 8. The purification equipment of this invention is flexible in selection and has a wider range of application scenarios: the purification section can use a vibrating screen plate assembly or a rotating screen plate assembly, which operates smoothly with low noise and is more adaptable to easily emulsified systems. Attached Figure Description

[0106] Figure 1 This is a schematic diagram of the equipment used for continuous purification of organic solids in Embodiments 1 and 2 of the present invention; Figure 2 These are schematic diagrams of the equipment used for continuous purification of organic solids in Embodiments 3 and 4 of the present invention; The names of the labels in the diagram are: 1. Organic phase feed pipe; 2. Organic phase discharge pipe; 3. Top clarification section; 301. Baffle plate; 4. Purification section; 401. Vibrating screen plate body; 402. Vibrating connecting rod; 403. Vibration drive mechanism; 404. Rotating screen plate body; 405. Rotating main shaft; 406. Rotating drive mechanism; 5. Bottom dispersion section; 501. Disperser; 502. Guide cone; 6. Aqueous phase feed pipe; 7. Aqueous phase discharge pipe; 8. First drain outlet; 9. Second drain outlet. Detailed Implementation

[0107] Example 1 like Figure 1 As shown, this embodiment provides an apparatus for the continuous purification of organic solids (2-hydroxy-4-methoxybenzophenone), comprising: a feeding system, an apparatus body, a discharging system, and a control system, specifically: 1. Feeding system: including organic phase feeding unit and aqueous phase feeding unit; The organic phase feeding unit includes an organic phase feed pipe 1, a storage tank, a transfer pump, and a flow meter. In this embodiment, the flow rate of the transfer pump is 98.3 L / h. The organic phase feed pipe 1 is connected to the side wall of the bottom dispersion section 5 of the tower. The organic solvent is toluene, used to feed the organic solvent phase, which is immiscible with water and dissolves organic solids, into the equipment body. The outlet end of the organic phase feed pipe 1 is connected to a disperser 501 installed in the bottom dispersion section 5 of the tower to disperse the organic phase into droplets.

[0108] The aqueous phase feeding unit includes an aqueous phase feeding pipe 6, a pure water tank, a preheating device (preheated to 30°C), a delivery pump, and a flow meter. The aqueous phase feeding pipe 6 is connected to the side wall of the clarification section 3 at the top of the tower and is used to send pure water into the equipment body to achieve countercurrent contact between the organic phase and the aqueous phase.

[0109] In this embodiment, the flow rate ratio of aqueous phase to organic phase is 15:1.

[0110] 2. Equipment body: Vertical closed tower structure, with a top clarification section 3, a purification section 4, and a bottom dispersion section 5 arranged sequentially from top to bottom, wherein: The main body of the equipment is made of stainless steel lined with PTFE. The total height of the main body is 4.5m. From top to bottom, it consists of a top clarification section 3 (1.0m high), a purification section 4 (3.0m high), and a bottom dispersion section 5 (0.5m high). The diameter of the purification section 4 is 0.15m, the diameter of the top clarification section 3 is 0.38m, and the diameter of the bottom dispersion section 5 is 0.35m. The main body of the equipment is also wrapped with an insulation layer to maintain temperature stability within the equipment.

[0111] The purification section 4 is equipped with a 6-layer vibrating screen assembly (in some embodiments, the number of layers of the vibrating screen assembly can be adjusted to suit the purification of different organic solids), including a vibrating screen body 401, a vibrating connecting rod 402, and a vibration drive mechanism 403. The vibrating screen body 401 is made of pure PTFE, with a pore size of 5mm and an open area ratio of 16%. The spacing between adjacent vibrating screen bodies 401 is 150mm. The vibrating screen bodies 401 are detachable for easy cleaning and replacement. The vibration drive mechanism 403 is a mechanical vibration type with a vibration frequency of 12Hz and an amplitude of 8mm. The above parameters of the vibrating screen body 401 are designed to adapt to the low viscosity organic-aqueous phase system, ensuring that the organic phase is fully dispersed into fine droplets to increase the mass transfer area, while avoiding emulsification caused by excessively fine droplets. At the same time, the pure PTFE material can prevent the adsorption of metal ions and avoid secondary pollution.

[0112] The top clarification section 3 of the column is equipped with three baffles 301 (in some embodiments, the number of baffles 301 can be adjusted to purify different organic solids), with a spacing of 250 mm. The baffles consist of one circular baffle and two annular baffles arranged alternately to prolong the residence time of the organic phase and promote droplet coalescence. The circular baffle is located at the center of the cylinder of the top clarification section 3 and is connected to the vibrating connecting rod 402. The center of the circular baffle coincides with the axis of the vibrating connecting rod 402, and its diameter is 50% of the diameter of the top clarification section 3. The annular baffle is connected to the inner wall of the top clarification section 3, and the diameter of its central hole is 45% of the diameter of the top clarification section 3. The circular baffle is located in the center, and the annular baffle is attached to the wall, forming an interlaced labyrinth flow channel, which enhances the aggregation and separation effect. At the same time, it breaks up the small droplets entrained and promotes the collision and merging of the dispersed organic phase droplets, reducing the water content of the organic phase and further improving the purity of the output, stably meeting the requirement of impurities at the ppb level.

[0113] In this embodiment, the organic phase discharge pipe 2 located in the top clarification section 3 of the tower is connected to the organic phase collection unit, and the outlet of the organic phase collection unit is connected to the solvent recovery branch (including distillation device and drying device); a first drain outlet 8 is also provided below the top clarification section 3 of the tower for periodically discharging the deposited trace solid impurities.

[0114] The bottom dispersion section 5 of the tower is equipped with a guide cone 502 and a disperser 501. The guide cone 502 has an inclination angle of 35° and is used to guide the aqueous phase to flow towards the aqueous phase outlet 7 to avoid water phase stagnation. A second drain outlet 9 is also provided below the guide cone 502. The disperser 501 is connected to the outlet end of the organic phase feed pipe 1 of the organic phase feed unit and is used to disperse the organic phase into droplets with a diameter of 1-3 mm.

[0115] In this embodiment, the aqueous phase discharge pipe 7 of the bottom dispersion section 5 is connected to the wastewater collection unit.

[0116] 3. Discharge system; including organic phase discharge unit and aqueous phase discharge unit.

[0117] In this embodiment, the equipment also includes a control system connected to the equipment for monitoring and regulating its operation. Specifically, it includes an interface detector (installed in the middle of the clarification section 3 at the top of the tower), an online purity detector (installed at the outlet of the organic phase discharge pipe 1, using an inductively coupled plasma mass spectrometer (ICP-MS)), flow sensors (installed at the feed pipes of the organic and aqueous phases respectively), and a temperature sensor (installed in the middle of the purification section 4). All sensors are electrically connected to a PLC controller; the PLC controller is connected to the vibration drive mechanism 403, the organic and aqueous phase transfer pumps, and the aqueous phase discharge valve.

[0118] This embodiment also provides a method for continuous purification of organic solids using the above-mentioned purification equipment, specifically including: Step 1: Dissolve 100 kg of 2-hydroxy-4-methoxybenzophenone (pale yellow crystalline powder) in 250 kg of toluene to prepare an organic phase solution; complete the batching, stirring and dissolving, and system pipeline preheating preparation, which takes a total of 0.5 h. Step 2: Start the equipment. The organic phase solution is sent from the bottom dispersion section 5 of the tower to the disperser 501 via the transfer pump and dispersed into 1-3mm droplets. Pure water is preheated to 30°C and sent from the top clarification section 3 of the tower. The organic phase and the aqueous phase are in countercurrent contact. Step 3: Mass transfer is enhanced under the action of the vibrating screen plate assembly, so that impurities in the organic phase are transferred to the aqueous phase; that is, the organic phase rises along the purification section 4 under the action of vibration and comes into countercurrent contact with the descending aqueous phase, and impurities are transferred from the organic phase to the aqueous phase. The effective purification residence time in the equipment body is 18 minutes. The total operation time of continuous feeding, purification and discharge of 100 kg material + 250 kg solvent is 3.9 hours. Step 4: The purified organic phase is separated in the clarification section 3 at the top of the tower, and the aqueous phase containing impurities is discharged in the dispersion section 5 at the bottom of the tower. That is, after the organic phase rises to the clarification section 3 at the top of the tower and agglomerates and separates, it is discharged from the organic phase discharge pipe 2 to the organic phase collection unit. The aqueous phase containing impurities is guided by the guide cone 502 to the outlet of the aqueous phase discharge pipe 7 and discharged to the wastewater collection unit. Step 5: The purified organic phase is subjected to solvent recovery and drying. After collection, the solvent is evaporated, which takes 0.5 hours, to obtain a high-purity organic solid.

[0119] The results of the above purification method using the relevant equipment are as follows: the total purification time for 100kg of material is nearly 5.0h, of which the pure purification operation takes 3.9h and the feeding and discharging auxiliary operation takes 1h; the impurity content in the product is 42ppb, which stably meets the high purity requirement of less than 100ppb, and the equipment operates continuously.

[0120] Example 2 like Figure 1 As shown, this embodiment provides a device for the continuous purification of organic solids (thiophene-spiropyran), including: a feeding system, a device body, a discharging system, and a control system, specifically: 1. Feeding system: including organic phase feeding unit and aqueous phase feeding unit; The organic phase feeding unit includes an organic phase feed pipe 1, a storage tank, a transfer pump, and a flow meter. In this embodiment, the flow rate of the transfer pump is 190.6 L / h. The organic phase feed pipe 1 is connected to the side wall of the bottom dispersion section 5 of the tower. The organic solvent is ethyl acetate, which is used to feed the organic solvent phase, which is immiscible with water and dissolves organic solids, into the equipment body. The outlet end of the organic phase feed pipe 1 is connected to a disperser 501 installed in the bottom dispersion section 5 of the tower to disperse the organic phase into droplets.

[0121] The aqueous phase feeding unit includes an aqueous phase feeding pipe 6, a pure water tank, a preheating device (preheated to 35°C), a delivery pump, and a flow meter. The aqueous phase feeding pipe 6 is connected to the side wall of the clarification section 3 at the top of the tower and is used to send pure water into the equipment body to achieve countercurrent contact between the organic phase and the aqueous phase.

[0122] In this embodiment, the flow rate ratio of aqueous phase to organic phase is 15:1.

[0123] 2. Equipment body: Vertical closed tower structure, with a top clarification section 3, a purification section 4, and a bottom dispersion section 5 arranged sequentially from top to bottom, wherein: The main body of the equipment is made of stainless steel, and its total height is 5.0m. From top to bottom, it consists of a top clarification section 3 (1.2m high), a purification section 4 (3.5m high), and a bottom dispersion section 5 (0.3m high). The diameter of the purification section 4 is 0.25m, the diameter of the top clarification section 2 is 0.5m, and the diameter of the bottom dispersion section 5 is 0.45m. The main body of the equipment is also wrapped with an insulation layer to maintain temperature stability within the equipment.

[0124] The purification section 4 is equipped with an 8-layer vibrating screen assembly (in some embodiments, the number of layers of the vibrating screen assembly can be adjusted to suit the purification of different organic solids), including a vibrating screen body 401, a vibrating connecting rod 402, and a vibration drive mechanism 403. The vibrating screen body 401 is made of stainless steel lined with PFA, with a pore size of 6mm and an opening ratio of 18%. The spacing between adjacent vibrating screen bodies 401 is 120mm. The vibrating screen bodies 401 are detachable for easy cleaning and replacement. The vibration drive mechanism 403 is a pneumatic vibration type with a vibration frequency of 12Hz and an amplitude of 8mm. The above parameters of the vibrating screen body 401 are designed to adapt to low-viscosity organic-aqueous systems, ensuring that the organic phase is fully dispersed into fine droplets to increase the mass transfer area, while avoiding emulsification caused by excessively fine droplets. At the same time, the stainless steel lining with PFA prevents the adsorption of metal ions and avoids secondary pollution.

[0125] The top clarification section 3 of the column is equipped with three baffles 301 (in some embodiments, the number of baffles 301 can be adjusted to purify different organic solids), with a spacing of 250 mm. The baffles consist of one circular baffle and two annular baffles arranged alternately to prolong the residence time of the organic phase and promote droplet coalescence. The circular baffle is located at the center of the cylinder of the top clarification section 3 and is connected to the vibrating connecting rod 402. The center of the circular baffle coincides with the axis of the vibrating connecting rod 402, and its diameter is 50% of the diameter of the top clarification section 3. The annular baffle is connected to the inner wall of the top clarification section 3, and the diameter of its central hole is 45% of the diameter of the top clarification section 3. The circular baffle is located in the center, and the annular baffle is attached to the wall, forming an interlaced labyrinth flow channel, which enhances the aggregation and separation effect. At the same time, it breaks up the small droplets entrained and promotes the collision and merging of the dispersed organic phase droplets, reducing the water content of the organic phase and further improving the purity of the output, stably meeting the requirement of impurities at the ppb level.

[0126] In this embodiment, the organic phase discharge pipe 2 located in the top clarification section 3 of the tower is connected to the organic phase collection unit, and the outlet of the organic phase collection unit is connected to the solvent recovery branch (including distillation device and drying device); a first drain outlet 8 is also provided below the top clarification section 3 of the tower for periodically discharging the deposited trace solid impurities.

[0127] The bottom dispersion section 5 of the tower is equipped with a guide cone 502 and a disperser 501. The guide cone 502 has an inclination angle of 35° and is used to guide the aqueous phase to flow towards the aqueous phase outlet 7 to avoid water phase stagnation. A second drain outlet 9 is also provided below the guide cone 502. The disperser 501 is connected to the outlet end of the organic phase feed pipe 1 of the organic phase feed unit and is used to disperse the organic phase into droplets with a diameter of 1-3 mm.

[0128] In this embodiment, the aqueous phase discharge pipe 7 of the bottom dispersion section 5 is connected to the wastewater collection unit.

[0129] 3. Discharge system; including organic phase discharge unit and aqueous phase discharge unit.

[0130] In this embodiment, the equipment also includes a control system connected to the equipment for monitoring and regulating its operation. Specifically, it includes an interface detector (installed in the middle of the clarification section 3 at the top of the tower), an online purity detector (installed at the outlet of the organic phase discharge pipe 1, using an inductively coupled plasma mass spectrometer (ICP-MS)), flow sensors (installed at the feed pipes of the organic and aqueous phases respectively), and a temperature sensor (installed in the middle of the purification section 4). All sensors are electrically connected to a PLC controller; the PLC controller is connected to the vibration drive mechanism 403, the organic and aqueous phase transfer pumps, and the aqueous phase discharge valve.

[0131] This embodiment also provides a method for continuous purification of organic solids using the above-mentioned purification equipment, specifically including: Step 1: Dissolve 100 kg of thienylspiropyran in 250 kg of ethyl acetate to prepare an organic phase solution; complete the preparation of ingredients, stirring and dissolving, and preheating of the system pipelines, which takes a total of 0.5 h. Step 2: Start the equipment. The organic phase solution is sent from the bottom dispersion section 5 of the tower to the disperser 501 via the transfer pump and dispersed into 1-3mm droplets. Pure water is preheated to 30°C and sent from the top clarification section 3 of the tower. The organic phase and the aqueous phase are in countercurrent contact. Step 3: Mass transfer is enhanced under the action of the vibrating screen plate assembly, so that impurities in the organic phase are transferred to the aqueous phase; that is, the organic phase rises along the purification section 4 under the action of vibration and comes into countercurrent contact with the descending aqueous phase, and impurities are transferred from the organic phase to the aqueous phase. The effective purification residence time in the equipment body is 15 minutes. The total operation time of continuous feeding, purification and discharge of 100 kg material + 250 kg solvent is 3.9 hours. Step 4: The purified organic phase is separated in the clarification section 3 at the top of the tower, and the aqueous phase containing impurities is discharged in the dispersion section 5 at the bottom of the tower. That is, after the organic phase rises to the clarification section 3 at the top of the tower and agglomerates and separates, it is discharged from the organic phase discharge pipe 2 to the organic phase collection unit. The aqueous phase containing impurities is guided by the guide cone 502 to the outlet of the aqueous phase discharge pipe 7 and discharged to the wastewater collection unit. Step 5: The purified organic phase is subjected to solvent recovery and drying. After collection, the solvent is evaporated, which takes 0.5 hours, to obtain a high-purity organic solid.

[0132] The results of the above purification method using the relevant equipment are as follows: the total purification time for 100kg of material is nearly 5.0h, of which the pure purification operation takes 3.9h and the feeding and discharging auxiliary operation takes 1h; the impurity content in the product is 75ppb, which stably meets the high purity requirement of less than 100ppb, and the equipment operates continuously.

[0133] Example 3 like Figure 2 As shown, this embodiment provides an apparatus for the continuous purification of organic solids (2-hydroxy-4-methoxybenzophenone), comprising: a feeding system, an apparatus body, a discharging system, and a control system, specifically: 1. Feeding system: including organic phase feeding unit and aqueous phase feeding unit; The organic phase feeding unit includes an organic phase feed pipe 1, a storage tank, a transfer pump, and a flow meter. In this embodiment, the flow rate of the transfer pump is 98.3 L / h. The organic phase feed pipe 1 is connected to the side wall of the bottom dispersion section 5 of the tower. The organic solvent is toluene, used to feed the organic solvent phase, which is immiscible with water and dissolves organic solids, into the equipment body. The outlet end of the organic phase feed pipe 1 is connected to a disperser 501 installed in the bottom dispersion section 5 of the tower to disperse the organic phase into droplets.

[0134] The aqueous phase feeding unit includes an aqueous phase feeding pipe 6, a pure water tank, a preheating device (preheated to 30°C), a delivery pump, and a flow meter. The aqueous phase feeding pipe 6 is connected to the side wall of the clarification section 3 at the top of the tower and is used to send pure water into the equipment body to achieve countercurrent contact between the organic phase and the aqueous phase.

[0135] In this embodiment, the flow rate ratio of aqueous phase to organic phase is 15:1.

[0136] 2. Equipment body: Vertical closed tower structure, with a top clarification section 3, a purification section 4, and a bottom dispersion section 5 arranged sequentially from top to bottom, wherein: The main body of the equipment is made of stainless steel, and its inner wall is electropolished (EP). The total height of the main body is 4.5m. From top to bottom, it consists of a top clarification section 3 (1.0m high), a purification section 4 (3.0m high), and a bottom dispersion section 5 (0.5m high). The diameter of the purification section 4 is 0.15m, the diameter of the top clarification section 3 is 0.4m, and the diameter of the bottom dispersion section 5 is 0.35m. The main body of the equipment is also wrapped with an insulation layer to maintain temperature stability within the equipment.

[0137] The purification section 4 is equipped with a 6-layer rotating sieve assembly (in some embodiments, the number of layers of the rotating sieve assembly can be adjusted to suit the purification of different organic solids), including a rotating sieve body 404, a rotating spindle 405, and a rotating drive mechanism 406. The rotating sieve body 404 is made of pure PTFE, with a pore size of 5mm and an opening rate of 16%. The spacing between adjacent rotating sieve bodies 404 is 150mm. The rotating sieve bodies 404 are detachable for easy cleaning and replacement. The rotating sieve bodies are located on the rotating spindle, and the horizontal inclination angle α of the mounting plane of the rotating sieve bodies 404 is 3°. The inclination direction of each layer of the rotating sieve bodies 404 is different. The rotary drive mechanism 406 of the rotary sieve plate assembly 404 is driven by a variable frequency motor with a rotation speed of 60 r / min, and the rotation speed can be adaptively adjusted according to the viscosity of the organic phase and the impurity content. The rotation of the tilted rotating screen plate body 404 creates irregular upper and lower liquid layer disturbances, continuously renewing the two-phase contact interface, enhancing the dispersion and aggregation of droplets, and achieving a mass transfer efficiency comparable to that of the rotating screen plate assembly. Moreover, the operation process is free from axial vibration, resulting in smoother equipment operation and lower noise, which can effectively reduce the risk of emulsification caused by excessively fine droplets.

[0138] The top clarification section 3 of the column is internally equipped with three baffles 301 (in some embodiments, the number of baffles 301 can be adjusted to purify different organic solids), with a spacing of 250 mm. The baffles consist of one circular baffle and two annular baffles arranged alternately to prolong the residence time of the organic phase and promote droplet coalescence. The circular baffle is located at the center of the cylinder of the top clarification section 3 and is connected to the rotating main shaft 405. The center of the circular baffle coincides with the axis of the rotating main shaft 405, and its diameter is 50% of the diameter of the top clarification section 3. The annular baffles are connected to the inner wall of the top clarification section 3, and the diameter of the central circular hole is 45% of the diameter of the top clarification section 3. The circular baffle is located in the center, and the annular baffle is attached to the wall, forming an interlaced labyrinth flow channel, which enhances the aggregation and separation effect. At the same time, it breaks up the small droplets entrained and promotes the collision and merging of the dispersed organic phase droplets, reducing the water content of the organic phase and further improving the purity of the output, stably meeting the requirement of impurities at the ppb level.

[0139] In this embodiment, the organic phase discharge pipe 2 located in the top clarification section 3 of the tower is connected to the organic phase collection unit, and the outlet of the organic phase collection unit is connected to the solvent recovery branch (including distillation device and drying device); a first drain outlet 8 is also provided below the top clarification section 3 of the tower for periodically discharging the deposited trace solid impurities.

[0140] The bottom dispersion section 5 of the tower is equipped with a guide cone 502 and a disperser 501. The guide cone 502 has an inclination angle of 35° and is used to guide the aqueous phase to flow towards the aqueous phase outlet 7 to avoid water phase stagnation. A second drain outlet 9 is also provided below the guide cone 502. The disperser 501 is connected to the outlet end of the organic phase feed pipe 1 of the organic phase feed unit and is used to disperse the organic phase into droplets with a diameter of 1-3 mm.

[0141] In this embodiment, the aqueous phase discharge pipe 7 of the bottom dispersion section 5 is connected to the wastewater collection unit.

[0142] 3. Discharge system; including organic phase discharge unit and aqueous phase discharge unit.

[0143] In this embodiment, the equipment also includes a control system connected to the equipment for monitoring and regulating its operation. Specifically, it includes an interface detector (installed in the middle of the clarification section 3 at the top of the tower), an online purity detector (installed at the outlet of the organic phase discharge pipe 1, using an inductively coupled plasma mass spectrometer (ICP-MS)), flow sensors (installed at the feed pipes of the organic and aqueous phases respectively), and a temperature sensor (installed in the middle of the purification section 4). All sensors are electrically connected to a PLC controller; the PLC controller is connected to the rotary drive mechanism 403, the organic and aqueous phase transfer pumps, and the aqueous phase discharge valve.

[0144] This embodiment also provides a method for continuous purification of organic solids using the above-mentioned purification equipment, specifically including: Step 1: Dissolve 100 kg of 2-hydroxy-4-methoxybenzophenone (pale yellow crystalline powder) in 250 kg of toluene to prepare an organic phase solution; complete the batching, stirring and dissolving, and system pipeline preheating preparation, which takes a total of 0.5 h. Step 2: Start the equipment. The organic phase solution is sent from the bottom dispersion section 5 of the tower to the disperser 501 via the transfer pump and dispersed into 1-3mm droplets. Pure water is preheated to 30°C and sent from the top clarification section 3 of the tower. The organic phase and the aqueous phase are in countercurrent contact. Step 3: Mass transfer is enhanced under the action of the rotating screen plate assembly, so that impurities in the organic phase are transferred to the aqueous phase. The rotation speed of the rotating screen plate body is 85 r / min. That is, the organic phase rises along the purification section 4 under the action of rotation and comes into countercurrent contact with the descending aqueous phase. Impurities are transferred from the organic phase to the aqueous phase. The effective purification residence time in the equipment body is 17 min. The total operation time of continuous feeding of 100 kg material + 250 kg solvent and purification discharge is 3.9 h. Step 4: The purified organic phase is separated in the clarification section 3 at the top of the tower, and the aqueous phase containing impurities is discharged in the dispersion section 5 at the bottom of the tower. That is, after the organic phase rises to the clarification section 3 at the top of the tower and agglomerates and separates, it is discharged from the organic phase discharge pipe 2 to the organic phase collection unit. The aqueous phase containing impurities is guided by the guide cone 502 to the outlet of the aqueous phase discharge pipe 7 and discharged to the wastewater collection unit. Step 5: The purified organic phase is subjected to solvent recovery and drying. After collection, the solvent is evaporated, which takes 0.5 hours, to obtain a high-purity organic solid.

[0145] The results of the above purification method using the relevant equipment are as follows: the total purification time for 100kg of material is nearly 5.0h, of which the pure purification operation takes 3.9h and the feeding and discharging auxiliary operation takes 1h; the impurity content in the product is 79ppb, which stably meets the high purity requirement of less than 100ppb, and the equipment operates continuously.

[0146] Example 4 like Figure 2As shown, this embodiment provides a device for the continuous purification of organic solids (1'-biphenyl-4,4'-diamine), including: a feeding system, a device body, a discharging system, and a control system, specifically: 1. Feeding system: including organic phase feeding unit and aqueous phase feeding unit; The organic phase feeding unit includes an organic phase feed pipe 1, a storage tank, a transfer pump, and a flow meter. In this embodiment, the flow rate of the transfer pump is 98.3 L / h. The organic phase feed pipe 1 is connected to the side wall of the bottom dispersion section 5 of the tower. The organic solvent is methyl isobutyl ketone, used to feed the water-immiscible organic solvent phase containing dissolved organic solids into the equipment body. The outlet end of the organic phase feed pipe 1 is connected to a disperser 501 installed in the bottom dispersion section 5 of the tower to disperse the organic phase into droplets.

[0147] The aqueous phase feeding unit includes an aqueous phase feeding pipe 6, a pure water tank, a preheating device (preheated to 30°C), a delivery pump, and a flow meter. The aqueous phase feeding pipe 6 is connected to the side wall of the clarification section 3 at the top of the tower and is used to send pure water into the equipment body to achieve countercurrent contact between the organic phase and the aqueous phase.

[0148] In this embodiment, the flow rate ratio of aqueous phase to organic phase is 15:1.

[0149] 2. Equipment body: Vertical closed tower structure, with a top clarification section 3, a purification section 4, and a bottom dispersion section 5 arranged sequentially from top to bottom, wherein: The main body of the equipment is made of stainless steel lined with PFA. The total height of the main body is 4.5m. From top to bottom, it consists of a top clarification section 3 (1.0m high), a purification section 4 (3.0m high), and a bottom dispersion section 5 (0.5m high). The diameter of the purification section 4 is 0.15m, the diameter of the top clarification section 3 is 0.4m, and the diameter of the bottom dispersion section 5 is 0.35m. The main body of the equipment is also wrapped with an insulation layer to maintain temperature stability within the equipment.

[0150] The purification section 4 is equipped with a 6-layer rotating sieve assembly (in some embodiments, the number of layers of the rotating sieve assembly can be adjusted to suit the purification of different organic solids), including a rotating sieve body 404, a rotating spindle 405, and a rotating drive mechanism 406. The rotating sieve body 404 is made of pure PTFE, with a pore size of 5mm and an opening rate of 16%. The spacing between adjacent rotating sieve bodies 404 is 150mm. The rotating sieve bodies 404 are detachable for easy cleaning and replacement. The rotating sieve bodies are located on the rotating spindle, and the horizontal inclination angle α of the mounting plane of the rotating sieve bodies 404 is 3°. The inclination direction of each layer of the rotating sieve bodies 404 is different. The rotary drive mechanism 406 of the rotary sieve plate assembly 404 is driven by a variable frequency motor with a rotation speed of 60 r / min, and the rotation speed can be adaptively adjusted according to the viscosity of the organic phase and the impurity content. The rotation of the tilted rotating screen plate body 404 creates irregular upper and lower liquid layer disturbances, continuously renewing the two-phase contact interface, enhancing the dispersion and aggregation of droplets, and achieving a mass transfer efficiency comparable to that of the rotating screen plate assembly. Moreover, the operation process is free from axial vibration, resulting in smoother equipment operation and lower noise, which can effectively reduce the risk of emulsification caused by excessively fine droplets.

[0151] The top clarification section 3 of the column is internally equipped with three baffles 301 (in some embodiments, the number of baffles 301 can be adjusted to purify different organic solids), with a spacing of 250 mm. The baffles consist of one circular baffle and two annular baffles arranged alternately to prolong the residence time of the organic phase and promote droplet coalescence. The circular baffle is located at the center of the cylinder of the top clarification section 3 and is connected to the rotating main shaft 405. The center of the circular baffle coincides with the axis of the rotating main shaft 405, and its diameter is 50% of the diameter of the top clarification section 3. The annular baffles are connected to the inner wall of the top clarification section 3, and the diameter of the central circular hole is 45% of the diameter of the top clarification section 3. The circular baffle is located in the center, and the annular baffle is attached to the wall, forming an interlaced labyrinth flow channel, which enhances the aggregation and separation effect. At the same time, it breaks up the small droplets entrained and promotes the collision and merging of the dispersed organic phase droplets, reducing the water content of the organic phase and further improving the purity of the output, stably meeting the requirement of impurities at the ppb level.

[0152] In this embodiment, the organic phase discharge pipe 2 located in the top clarification section 3 of the tower is connected to the organic phase collection unit, and the outlet of the organic phase collection unit is connected to the solvent recovery branch (including distillation device and drying device); a first drain outlet 8 is also provided below the top clarification section 3 of the tower for periodically discharging the deposited trace solid impurities.

[0153] The bottom dispersion section 5 of the tower is equipped with a guide cone 502 and a disperser 501. The guide cone 502 has an inclination angle of 35° and is used to guide the aqueous phase to flow towards the aqueous phase outlet 7 to avoid water phase stagnation. A second drain outlet 9 is also provided below the guide cone 502. The disperser 501 is connected to the outlet end of the organic phase feed pipe 1 of the organic phase feed unit and is used to disperse the organic phase into droplets with a diameter of 1-3 mm.

[0154] In this embodiment, the aqueous phase discharge pipe of the bottom dispersion section 5 is connected to the wastewater collection unit.

[0155] 3. Discharge system; including organic phase discharge unit and aqueous phase discharge unit.

[0156] In this embodiment, the equipment also includes a control system connected to the equipment for monitoring and regulating its operation. Specifically, it includes an interface detector (installed in the middle of the clarification section 3 at the top of the tower), an online purity detector (installed at the outlet of the organic phase discharge pipe 1, using an inductively coupled plasma mass spectrometer (ICP-MS)), flow sensors (installed at the feed pipes of the organic and aqueous phases respectively), and a temperature sensor (installed in the middle of the purification section 4). All sensors are electrically connected to a PLC controller; the PLC controller is connected to the rotary drive mechanism 406, the organic and aqueous phase transfer pumps, and the aqueous phase discharge valve.

[0157] This embodiment also provides a method for continuous purification of organic solids using the above-mentioned purification equipment, specifically including: Step 1: Dissolve 100 kg of 1'-biphenyl-4,4'-diamine in 250 kg of methyl isobutyl ketone to prepare an organic phase solution; complete the batching, stirring and dissolving, and preheating of the system pipelines, which takes a total of 0.5 h. Step 2: Start the equipment. The organic phase solution is sent from the bottom dispersion section 5 of the tower to the disperser 501 via the transfer pump and dispersed into 1-3mm droplets. Pure water is preheated to 30°C and sent from the top clarification section of the tower. The organic phase and the aqueous phase are in countercurrent contact. Step 3: Mass transfer is enhanced under the action of the rotating screen plate assembly, so that impurities in the organic phase are transferred to the aqueous phase. The rotation speed of the rotating screen plate body is 60 r / min. That is, the organic phase rises along the purification section under the action of rotation and comes into countercurrent contact with the descending aqueous phase. Impurities are transferred from the organic phase to the aqueous phase. The effective purification residence time in the equipment body is 17 min. The total operation time of 100 kg material + 250 kg solvent continuous feeding, purification and discharge is 3.9 h. Step 4: The purified organic phase is separated in the clarification section 3 at the top of the tower, and the aqueous phase containing impurities is discharged in the dispersion section 5 at the bottom of the tower. That is, after the organic phase rises to the clarification section 3 at the top of the tower and agglomerates and separates, it is discharged from the organic phase discharge pipe 2 to the organic phase collection unit. The aqueous phase containing impurities is guided by the guide cone 502 to the outlet of the aqueous phase discharge pipe 7 and discharged to the wastewater collection unit. Step 5: The purified organic phase is subjected to solvent recovery and drying. After collection, the solvent is evaporated, which takes 0.5 hours, to obtain a high-purity organic solid.

[0158] The results of the above purification method using the relevant equipment are as follows: the total purification time for 100kg of material is nearly 5.0h, of which the pure purification operation takes 3.9h and the feeding and discharging auxiliary operation takes 1h; the impurity content in the product is 32ppb, which stably meets the high purity requirement of less than 100ppb, and the equipment operates continuously.

[0159] Comparative Example 1 This comparative example uses a commonly used intermittent water washing process in the field of organic solid purification. The basic parameters of the raw materials used are consistent with those in Example 1 of this invention, as follows: 1. Raw materials and equipment Raw material to be purified: 2-hydroxy-4-methoxybenzophenone, pale yellow crystalline powder, batch total mass 100 kg, initial total metal ion content 1180 ppb; the purification objective is to reduce the total metal ion content in the raw material to below 100 ppb, wherein the metal ions include, but are not limited to, Na+. + K + Ca 2+ Fe 3+ (Water-soluble metal ions of this type).

[0160] Organic solvent: toluene, initial dissolution volume 250 kg; Washing medium: pure water, with a single wash volume ratio of aqueous phase to organic phase of 1:1; Equipment: 800L enamel washing kettle (with agitator, temperature control, and bottom valve discharge port), 500L vacuum heating kettle, vacuum drying oven.

[0161] 2. Purification Operation Steps The process shall be carried out according to the existing intermittent water washing technology, and the specific steps are as follows: Step 1, raw material dissolution: 100 kg of 2-hydroxy-4-methoxybenzophenone to be purified and 250 kg of toluene are put into a water washing kettle and stirred at room temperature for 30 min until the solid is completely dissolved to obtain a homogeneous organic phase liquid. Step 2, Single water wash cycle: Add pure water to the water washing tank according to the preset ratio, turn on the agitator, and stir at a fixed speed at room temperature for 40 minutes to fully transfer impurities to the aqueous phase; stop stirring and let it stand for 40 minutes to ensure that the organic phase and the aqueous phase are completely separated; under full manual monitoring, slowly open the bottom valve of the water washing tank to discharge the lower aqueous phase. Strictly control the flow rate during the discharge process to avoid damaging the interface between the two phases. Each discharge takes 20 minutes to complete the core operation of a single water wash. Step 3, Concentration, Redissolution, and Repeated Washing: Transfer the organic phase solution after one wash to a vacuum heating kettle, and remove 80% of the toluene solvent by vacuum distillation, which takes 30 minutes; transfer the concentrated material back to the washing kettle, and add fresh toluene to the initial solution volume, which takes 20 minutes. This completes a single batch of complete washing cycles, with a total operation time of 2.5 hours. After the 5th washing cycle, a sample was taken and the impurity content in the organic phase was tested to be 215 ppb, which did not meet the purification target of below 100 ppb. The above operation was repeated until a total of 10 washing cycles were completed. Step 4, Final Post-processing: After the 10th water wash, all the organic phase liquid was transferred to a vacuum heating kettle, and the toluene solvent was removed by vacuum distillation to obtain concentrated 2-hydroxy-4-methoxybenzophenone material; the material was transferred to a vacuum oven and vacuum dried at 60°C for 12 hours to obtain the final purified product.

[0162] 3. Results of intermittent process Intermediate parameters for the 5th water washing cycle: impurity content 215 ppb, which did not meet the purification target of below 100 ppb; cumulative water washing and concentration operation time 12.5 h, with a cumulative manual monitoring time of 8 h; in the 5 aqueous phase discharges, 1 batch experienced organic phase entrainment loss due to interface disturbance during the discharge process.

[0163] The total time for 10 water washing cycles is 37 hours (including drying time), of which 25 hours are spent on effective water washing and concentration operations, and 12 hours are spent on drying. The final product had an impurity content of 93 ppb, achieving the purification target. Total duration of fully manual operation: 16 hours; Equipment utilization rate: 22% (water washing tank and heating tank are used alternately in series); Operational stability: In 10 aqueous phase discharges, 2 batches experienced organic phase entrainment loss due to interface disturbance during the discharge process.

[0164] The performance comparison results between Comparative Example 1 and Embodiment 1 of the present invention are shown in Table 1: Table 1. Performance comparison results between Comparative Example 1 and Embodiment 1 of the present invention

[0165] Comparative Example 2 Compared to Example 1, this comparative example has the same hole diameter (10 mm) and opening ratio (25%) as Example 1, but the other parameters of the equipment and the purification method are the same as in Example 1.

[0166] After continuous purification under the same conditions, the purity of the organic phase output was tested. The impurity content in the obtained product was 89 ppb, significantly higher than the 42 ppb in Example 1, indicating a deterioration in separation efficiency. The reason for this is that when the sieve aperture and open area ratio are too large, the shear dispersion effect on the organic phase as it passes through the sieve apertures weakens, resulting in larger organic phase droplet diameters and a significant decrease in the mass transfer surface area. This leads to a decrease in the mass transfer flux of water-soluble metal ions from the organic phase to the aqueous phase. Simultaneously, a larger open area ratio increases the tendency for local short-circuiting and axial backmixing in the organic phase, further weakening the mass transfer driving force for purification and resulting in incomplete impurity removal.

[0167] Comparative Example 3 Compared to Example 1, this comparative example adjusts the spacing between adjacent vibrating screen plates to 200mm, while the remaining equipment parameters and purification methods are the same as in Example 1.

[0168] After continuous purification under the same conditions, the impurity content in the product was found to be 171 ppb, which is much higher than the 42 ppb in Example 1 and significantly exceeds the high purity requirement of 100 ppb. The reason is that as the distance between adjacent vibrating screen plates increases, the aggregation time and degree of organic phase droplets between adjacent vibrating screen plates in each stage are prolonged, and the effective mass transfer interface renewal frequency decreases. At the same time, the increase in distance exacerbates axial backmixing in purification section 4, reduces stage efficiency and the number of mass transfer units, and ultimately significantly reduces the overall purification effect.

[0169] Comparative Example 4 Compared to Example 1, this comparative example adjusts the vibration frequency of the vibration drive mechanism to 5Hz and the amplitude to 3mm, while the remaining equipment parameters and purification methods are the same as in Example 1.

[0170] After continuous purification under the same conditions, the impurity content in the product was found to be 96 ppb, significantly higher than the 42 ppb in Example 1, indicating a deterioration in separation efficiency. The reason for this is that the significantly reduced vibration frequency and amplitude resulted in insufficient mechanical energy input into the liquid-liquid system, weakening the crushing and redispersing effect of the vibrating sieve on the organic phase. This led to the organic phase being dispersed in larger droplets, reducing the mass transfer surface area and decreasing the mass transfer rate of impurities between phases. Simultaneously, the lower vibration intensity also resulted in insufficient turbulence in the droplet group, further reducing the mass transfer coefficient. Therefore, the product purity could not reach the level of Example 1.

[0171] Comparative Example 5 Compared to Example 1, this comparative example differs from Example 1 in that the top clarification section 3 of the tower is not equipped with baffles, while the remaining equipment parameters and purification methods are the same as in Example 1.

[0172] After continuous purification under the same conditions, the impurity content in the product was found to be 93 ppb, significantly higher than the 42 ppb in Example 1, indicating a deterioration in separation efficiency. The reason is that after removing the baffles, the clarification section 3 at the top of the column lost its labyrinthine flow channel structure, which facilitated the collision and aggregation of organic phase droplets and the separation of fine entrained water droplets. The residence time distribution of rising organic phase droplets in the clarification section 3 became wider, making it difficult for fine aqueous phase droplets to aggregate, grow, and settle. This resulted in some tiny water droplets containing water-soluble impurities being entrained into the organic phase discharge, leading to an increase in product moisture content, impurity content, and a reduction in final purity.

[0173] Comparative Example 6 Compared to Example 1, this comparative example differs from Example 1 in that a disperser is not installed in the dispersion section 5 at the bottom of the tower, while the remaining equipment parameters and purification methods are the same as in Example 1.

[0174] After continuous purification under the same conditions, the impurity content in the product was found to be 329 ppb, far higher than the 42 ppb in Example 1, indicating a significant deterioration in separation efficiency. The reason is that after removing the disperser, the organic phase feed entered the bottom of the column directly without dispersion. The organic phase, in the form of large-sized liquid agglomerates or continuous streams, contacted the descending aqueous phase, failing to form small droplet clusters with a diameter of 1-3 mm. This resulted in a sharp decrease in the liquid-liquid mass transfer surface area and a severely insufficient interphase contact area, significantly reducing the rate of impurity migration from the organic phase to the aqueous phase. Simultaneously, the rising behavior of the large-sized organic phase agglomerates disrupted the uniform distribution of droplet clusters in the vibrating screen section, further weakening the mass transfer efficiency of purification section 4, ultimately leading to a significant increase in the product impurity content.

[0175] Comparative Example 7 Compared to Example 1, this comparative example adjusts the flow ratio of the aqueous phase to the organic phase to 8:1, that is, the flow rate of the aqueous phase feed is reduced accordingly. The other parameters of the equipment and the other operating conditions of the purification method are the same as those in Example 1.

[0176] It should be noted that due to the reduced aqueous phase flow rate, the total throughput within the equipment decreases while the organic phase feed flow rate remains constant, resulting in a corresponding decrease in the apparent flow velocity of the aqueous phase in purification section 4. After continuous purification under the same conditions, the impurity content in the product was found to be greater than 1000 ppb, far exceeding the 42 ppb in Example 1, indicating a sharp deterioration in the separation effect. The reason is that the flow ratio (ratio) of the aqueous phase to the organic phase is a key parameter determining the driving force of purification mass transfer and operation. Reducing the ratio from 15:1 to 8:1 significantly reduces the flow rate of the aqueous phase in countercurrent contact with the organic phase per unit time, thereby reducing the total amount of impurities that the aqueous phase can accommodate. The purification operation line moves closer to the equilibrium line, and the driving force of mass transfer is significantly weakened. At the same time, the decrease in the apparent flow velocity of the aqueous phase also reduces the relative motion intensity and interfacial disturbance of the liquid-liquid two phases, further weakening the mass transfer coefficient. This leads to a sharp increase in the concentration of residual impurities in the organic phase, and the product purity fails to meet the requirements.

[0177] Through the above comparison, the purification equipment and purification method of the present invention can effectively overcome the technical defects of the intermittent water washing process in the prior art. Through systematic innovation in structure and process, that is, the settings of each structure and parameter in the equipment are complementary and coordinated with each other, so that the impurities in the product can be stably met to meet the high purity requirements of less than 100 ppb, or even controlled to less than 90 ppb, and continuous production can be achieved, and the purification time per unit product is also greatly reduced.

[0178] It should be understood that the present invention is not limited to what has been described above and shown in the accompanying drawings, and various modifications and changes can be made without departing from its scope. The scope of the invention is limited only by the appended claims.

Claims

1. An apparatus for the continuous purification of organic solids, characterized in that, include: Feeding system: includes organic phase feeding unit and aqueous phase feeding unit; Equipment body: Vertical closed tower structure, with a top clarification section (3), a purification section (4), and a bottom dispersion section (5) arranged sequentially from top to bottom. Discharge system; Includes an organic phase discharge unit and an aqueous phase discharge unit; The top clarification section (3) of the tower is provided with several baffles; the purification section (4) is provided with several sieve plate assemblies; and the bottom dispersion section (5) of the tower is provided with a disperser (501). The organic phase and the aqueous phase are in countercurrent contact within the equipment, and the organic solid, after being purified by the equipment, has an impurity content of less than 100 ppb.

2. The apparatus for continuous purification of organic solids according to claim 1, characterized in that, The height ratio of the equipment body, purification section (4), top clarification section (3), and bottom dispersion section (5) is (4-15): (3-10): (0.5-2.5): (0.3-2.5).

3. The apparatus for continuous purification of organic solids according to claim 1, characterized in that, The diameter ratio of the purification section (4), the top clarification section (3), and the bottom dispersion section (5) is (0.15-1.6):(0.3-1.8):(0.3-1.7).

4. The apparatus for continuous purification of organic solids according to claim 1, characterized in that, The screen plate assembly is a vibrating screen plate assembly or a rotary screen plate assembly.

5. The apparatus for continuous purification of organic solids according to claim 4, characterized in that, The vibrating screen plate assembly includes a vibrating screen plate body (401), a vibrating connecting rod (402), and a vibration drive mechanism (403).

6. The apparatus for continuous purification of organic solids according to claim 4, characterized in that, The rotary screen assembly includes a rotary screen body (404), a rotary spindle (405), and a rotary drive mechanism (406).

7. The apparatus for continuous purification of organic solids according to claim 6, characterized in that, The rotating screen plate body (404) is located on the rotating main shaft (405). The horizontal inclination angle of the mounting plane of the rotating screen plate body (404) is greater than 0°. The inclination direction of each layer of the rotating screen plate body (404) is different.

8. A purification method, characterized in that, The purification method is to continuously purify organic solids using the equipment for continuous purification of organic solids as described in any one of claims 1-7.

9. The purification method according to claim 8, characterized in that, Includes the following steps: Step 1: Dissolve the organic solid to be purified in an organic solvent that is immiscible with water to prepare an organic phase solution; Step 2: The organic phase solution is fed into the dispersion section (5) at the bottom of the tower and dispersed into droplets, while pure water is fed into the clarification section (3) at the top of the tower. The organic phase and the aqueous phase are in countercurrent contact. Step 3: Mass transfer is enhanced by the sieve plate assembly, causing impurities in the organic phase to transfer to the aqueous phase; Step 4: The purified organic phase is separated in the clarification section (3) at the top of the column, and the aqueous phase containing impurities is discharged in the dispersion section (5) at the bottom of the column. Step 5: The purified organic phase is recovered by solvent and dried to obtain a high-purity organic solid.

10. A high-purity organic solid, characterized in that, The high-purity organic solid is a product obtained by purification using the equipment for continuous purification of organic solids as described in any one of claims 1-7.

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