Purification device for electronic-grade chemicals
Through the purification device integrating the dissolution kettle and crystallization dryer, the problem of efficient purification of industrial-grade products is solved, and the stable production of high-purity electronic-grade chemicals is achieved, especially the low-temperature treatment of heat-sensitive compounds, which improves product quality and large-scale production capacity.
Patent Information
- Application Number
- CN202422111153.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-29
- Publication Date
- 2025-10-10
- Estimated Expiration
- 2034-08-29
AI Technical Summary
Existing technologies make it difficult to efficiently purify electronic-grade chemicals, especially heat-sensitive chemicals, from industrial-grade products. Multiple equipment transfers result in substandard product purity, making large-scale production difficult.
An integrated purification device is used, including a dissolving kettle and a crystallization dryer. By concentrating the purification steps in the crystallization dryer, using polytetrafluoroethylene or ceramic inner walls and polypropylene pipelines, controlling low-temperature operation, and combining adjustable stabilizers and hydraulic lifts, stable material transmission and efficient purification are achieved.
It improves the purity of electronic-grade chemicals, avoids contamination caused by multiple transfers, and expands the scope of application. It is particularly effective in purifying heat-sensitive chemicals such as aminosulfonic acid, with a purity of up to 99.99%.
Smart Images
Figure CN223416771U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of purification of chemical substances, in particular to a purification and drying device for electronic-grade chemicals. Background Art
[0002] Electronic-grade chemicals, also known as electronic chemical materials, broadly refer to specialized chemicals and chemical materials used in the electronics industry. They are high-tech products that combine electronic materials with fine chemicals. They can be categorized by application, including substrates, photoresists, electroplating chemicals, packaging materials, high-purity reagents, specialty gases, solvents, pre-cleaning dopants, solder masks, acids and etchants, specialized electronic adhesives, and auxiliary materials.
[0003] There are many varieties of electronic-grade chemicals, but the requirements for product quality and purity are very high, generally requiring a purity of ≥99.99%, and the requirements for the cleanliness of the production and use environment are also very stringent. In actual production, if such high-purity electronic-grade chemicals are directly synthesized, it is difficult to operate, and the synthesis conditions limit the production scale, which is not conducive to industrial promotion. The commonly used method is to purify the industrial-grade products obtained from large-scale industrial production to stably obtain the corresponding electronic-grade chemicals. This method can produce electronic-grade chemicals on a large scale. In the process of preparing electronic-grade chemicals by purification methods, processes such as crystallization, drying and purification are required. These processes require different equipment to implement. If the product passes through too many devices, it will increase the product purity due to insufficient cleanliness of the equipment or the environment of the circulation operation, and the thermal stability of electronic-grade chemicals is different, and some will decompose at lower temperatures. In order to solve the above problems, the present invention provides the following electronic-grade chemical purification device. Summary of the Invention
[0004] In view of the problems existing in the prior art, the present invention provides a purification device for electronic-grade chemicals to improve the purification accuracy of industrial-grade products such as HEDP, citric acid, and aminosulfonic acid.
[0005] In order to achieve the above purpose, the utility model adopts the following technical solutions:
[0006] The utility model provides a purification device for electronic-grade chemicals, comprising a dissolving kettle, a crystallization dryer, and a fixed platform. The upper end of the dissolving kettle is provided with a raw material feed port and a water inlet, the lower section is provided with a dissolving liquid outlet, and the outer wall is provided with a dissolving constant temperature heat exchanger. The raw material feed port is connected to a solid feeding device through a pipeline and is connected in series with a valve. The water inlet is connected to an ultrapure water supply device through a pipeline and is connected in series with a valve, an electronic flow meter, and a transmission pump.
[0007] The left end of the crystallization drier is provided with a solution inlet, a solution outlet and a rotating left shaft, the right end is provided with an air outlet, a rotating right shaft and a crystal discharge port, the outer wall is provided with a constant temperature heat exchanger, the solution inlet is connected to the dissolution kettle dissolution outlet through a pipeline and is connected in series with a valve, a suction pump and an electronic flow meter, the solution outlet is connected to a crystallization water recovery device through a pipeline and is connected in series with a valve and a suction pump, the air outlet is connected to a vacuum pump through a pipeline, and the crystal discharge port is connected to a dust-free packaging machine through a pipeline;
[0008] The base of the fixed platform is placed flat, a support rod is erected at one end of the base, an adjustable stabilizer 2 is embedded in the support rod, a hydraulic lift is fixedly placed at the other end of the base, an adjustable stabilizer 1 is fixedly placed on the hydraulic lift, the adjustable stabilizer 2 is connected to the rotating left axis of the crystallization dryer, and the adjustable stabilizer 1 is connected to the rotating right axis of the crystallization dryer.
[0009] According to the electronic-grade chemical purification device, the crystallization dryer is a hollow cylindrical structure with an aspect ratio of 3 to 5, and the circular surfaces at both ends are perpendicular to the ground; the solution inlet, solution outlet, gas outlet and crystal discharge port of the crystallization dryer are built-in valves and can be separated from the pipelines connected to them.
[0010] According to the purification device for electronic-grade chemicals, the rotating left shaft and the rotating right shaft of the crystallization dryer are both composed of a left shaft fixing tube and a left shaft rotating shaft; the left end of the left shaft fixing tube of the rotating left shaft and the second adjustable stabilizer are fixed by a snap connection, the right end is sleeved on the left end of the left shaft rotating shaft, and the right end of the left shaft rotating shaft is connected and fixed to the center of the left circular surface of the crystallization dryer body; the right end of the right shaft fixing tube of the rotating right shaft and the first adjustable stabilizer are fixed by a snap connection, the left end is sleeved on the right end of the right shaft rotating shaft, and the left end of the right shaft rotating shaft is connected and fixed to the center of the right circular surface of the crystallization dryer body.
[0011] According to the device for purifying electronic-grade chemicals, the adjustable stabilizer is composed of a detachable upper buckle, an adjustable angle lower buckle and a fixed base. The right end of the right shaft fixing tube of the rotating right shaft is fixed by the detachable upper buckle and the adjustable angle lower buckle. The connecting and fixing surface of the adjustable angle lower buckle and the fixed base is an arc surface. The adjustable angle lower buckle can rotate along the arc surface as the hydraulic lift rises and falls to match the angle change caused by the rise and fall of the rotating right shaft of the crystallization dryer.
[0012] According to the device for purifying electronic-grade chemicals, the adjustable stabilizer 2 is composed of upper and lower telescopic buckles and an adjustable angle base. The left end of the left axis fixed tube that engages with the rotating left axis is fixed by the upper and lower telescopic buckles moving up and down. The embedded surface of the adjustable angle base and the support rod is arc-shaped. The adjustable angle base has a built-in motor. The adjustable angle base can rotate vertically along the arc surface to match the angle change caused by the rotating left axis of the crystal drying box following the rotating right axis to rise and fall.
[0013] According to the device for purifying electronic-grade chemicals, the crystallization dryers and the fixed tables are arranged in groups of two, and multiple groups of crystallization dryers are connected in parallel.
[0014] According to the device for purifying electronic-grade chemicals, the inner walls of the dissolving kettle and the crystallization dryer are made of polytetrafluoroethylene or ceramic, and the connecting pipelines are made of polypropylene.
[0015] Beneficial effects of the present invention:
[0016] The electronic-grade chemical purification device provided by the utility model has a simple structure and concentrates the key purification steps in a crystallization dryer, thereby avoiding contamination caused by multiple material transfers and improving the quality of the electronic-grade chemicals. The equipment can be controlled to operate at a low temperature below 60°C, can purify some heat-sensitive electronic-grade chemicals such as aminosulfonic acid, and has a wide range of applications. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Figure 1 This is a schematic diagram of the overall structure of the utility model.
[0018] Figure 2 This is the left view of the adjustable stabilizer 1.
[0019] Figure 3 This is the right side view of the adjustable stabilizer 1.
[0020] Figure 4 This is the left view of the adjustable stabilizer 2.
[0021] Figure 5 This is the front view of the adjustable stabilizer 2.
[0022] Figure 6 This is a schematic diagram of the rotating left axis structure.
[0023] Figure 7 Schematic diagram of the rotating right axis structure.
[0024] Figure numerals: 1 dissolution kettle, 11. raw material feed port, 12. water inlet, 13. dissolution outlet, 14. dissolution constant temperature heat exchanger, 2. crystallization dryer, 21. solution inlet, 22. solution outlet, 23. air outlet, 24. left rotation axis, 25. right rotation axis, 26. crystal outlet, 27. crystallization constant temperature heat exchanger, 3. fixed platform, 31. base, 32. support rod, 33. hydraulic lift, 34. adjustable stabilizer 1, 35. adjustable stabilizer 2, 341. detachable upper buckle, 342. adjustable angle lower buckle, 343. fixed base, 351. upper and lower telescopic buckles, 352. adjustable angle base. DETAILED DESCRIPTION
[0025] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
[0026] The present invention provides a purification device for electronic-grade chemicals, comprising a dissolution vessel 1, a crystallization dryer 2, and a fixed platform 3. The dissolution vessel 1 has a raw material feed port 11 and a water inlet 12 at its upper end, a stirring mechanism within, a dissolution outlet 13 at its lower end, and a dissolution constant-temperature heat exchanger 14 on its outer wall. The raw material feed port 11 is connected to a solid feed device via a pipeline and connected in series with a valve. The water inlet 12 is connected to an ultrapure water supply via a pipeline and connected in series with a valve, an electronic flow meter, and a transmission pump.
[0027] The left end of the crystallization dryer 2 is provided with a solution inlet 21, a solution outlet 22 and a rotating left shaft 24, the right end is provided with an air outlet 23, a rotating right shaft 25 and a crystal discharge port 26, and the outer wall is provided with a constant temperature heat exchanger 27. The solution inlet 21 is connected to the dissolution kettle dissolution outlet 13 through a pipeline and is connected in series with a valve, a suction pump and an electronic flow meter. The solution outlet 22 is connected to the crystallization water recovery device through a pipeline and is connected in series with a valve and a suction pump. The air outlet 23 is connected to a vacuum pump through a pipeline, and the crystal discharge port 26 is connected to a dust-free packaging machine through a pipeline.
[0028] The base 31 of the fixed platform 3 is placed in a plane, and a support rod 32 is erected at one end of the base, and an adjustable stabilizer 2 35 is embedded in the support rod. A hydraulic lift 33 is fixedly placed at the other end of the base, and an adjustable stabilizer 1 34 is fixedly placed on the hydraulic lift. The adjustable stabilizer 2 35 is connected to the rotating left axis 24 of the crystallization dryer, and the adjustable stabilizer 1 34 is connected to the rotating right axis 25 of the crystallization dryer.
[0029] The crystallization dryer 2 of this device is a hollow cylindrical structure with an aspect ratio of 3 to 5, with its two rounded ends perpendicular to the ground. The solution inlet 21, solution outlet 22, gas outlet 23, and crystal discharge port 26 of the crystallization dryer are equipped with built-in valves, allowing disconnection of the connected pipelines. The crystallization dryer 2 is used for purification. Liquid is introduced through the solution inlet 21, heated and crystallized by a constant temperature heat exchanger 27, and then packaged through the crystal discharge port 26.
[0030] The rotating left shaft 24 and the rotating right shaft 25 of the crystallization dryer 2 are both composed of a left shaft fixing tube and a left shaft rotating shaft; the left end of the left shaft fixing tube 241 of the rotating left shaft 24 is fixed to the adjustable stabilizer 2 35 by a snap connection, and the right end is sleeved on the left end of the left shaft rotating shaft 242, and the right end of the left shaft rotating shaft 242 is connected and fixed to the center of the left circular surface of the crystallization dryer body; the right end of the right shaft fixing tube 251 of the rotating right shaft 25 is fixed to the adjustable stabilizer 1 34 by a snap connection, and the left end is sleeved on the right end of the right shaft rotating shaft 252, and the left end of the right shaft rotating shaft 252 is connected and fixed to the center of the right circular surface of the crystallization dryer body.
[0031] Specifically, the adjustable stabilizer 34 is composed of a detachable upper buckle 341, an adjustable angle lower buckle 342 and a fixed base 343. The right end of the right shaft fixing tube 251 of the rotating right shaft is fixed by the detachable upper buckle 341 and the adjustable angle lower buckle 342. The connecting and fixing surface of the adjustable angle lower buckle 342 and the fixed base 343 is an arc surface. The adjustable angle lower buckle 342 can rotate along the arc surface with the rise and fall of the hydraulic lift 33 to match the angle change caused by the rise and fall of the rotating right shaft 25 of the crystallization dryer.
[0032] Furthermore, the adjustable stabilizer 2 35 is composed of an upper and lower telescopic buckle 351 and an adjustable angle base 352. The upper and lower telescopic buckle 351 is moved up and down to fix the left end of the left shaft fixing tube 241 that engages with the rotating left shaft. The embedded surface of the adjustable angle base 352 and the support rod 32 is arc-shaped. The adjustable angle base 352 has a built-in motor. The adjustable angle base 352 can rotate vertically along the arc surface to match the angle change caused by the rotating left shaft 24 of the crystal drying box following the rotating right shaft 25 to rise and fall.
[0033] The inner walls of the dissolving kettle 1 and the crystallization dryer 2 of the device are made of polytetrafluoroethylene or ceramic, and the connecting pipelines are made of polypropylene.
[0034] Example of use:
[0035] The main raw material equipment specifications are as follows: the inner walls of the dissolving kettle and crystallization dryer are made of ceramic material, the dissolving kettle has a capacity of 5000L, the crystallization dryer has a length-to-diameter ratio of 4:1, an inner diameter of 50cm, and a length of 2m; two groups of crystallization dryers are used in parallel.
[0036] The raw materials are commercially available aminosulfonic acid with a purity of 99% (in actual preparation, aminosulfonic acid will begin to decompose at 70°C in the air and will release a large amount of sulfur dioxide at 90°C) and ultrapure water (homemade).
[0037] Step 1: Open the corresponding valves, add 1000kg of aminosulfonic acid to the dissolution kettle 1 through the raw material feed port 11, pump 2000kg of ultrapure water into the dissolution kettle 1 from the water inlet 12, start stirring, control the temperature in the kettle to 60~70℃ through the constant temperature heat exchanger 104, and keep the temperature unchanged after 0.5~1h. The liquid in the kettle is pumped into the crystallization dryer 2 through the dissolution outlet 13 and the solution inlet 21 by the suction pump in sequence. After 1500kg of liquid is pumped in through the electronic flowmeter, the corresponding valves and the suction pump are closed, the pipeline on the solution inlet 21 is removed, and the built-in valves are closed. At this time, the built-in valves of the solution outlet 22, the air outlet 23 and the crystallization outlet 26 are also in a closed state, and the remaining liquid in the dissolution kettle 1 is pumped into the parallel crystallization dryer in the same operation.
[0038] Step 2: Control the temperature in the crystallization dryer 2 at 60~70°C through the crystallization constant temperature heat exchanger 27, then cool it down at a certain rate, and start adding a quantitative amount of aminosulfonic acid seed crystals when the temperature drops to 50~55°C. After keeping warm for 2~3 hours, continue to cool down the temperature and crystallize. After 6 hours, cool it to 25°C, turn on the hydraulic lift 33 to lift the adjustable stabilizer 34, so that the right end of the crystallization dryer rises higher than the left end and forms an angle of 15° with the horizontal plane. Connect the liquid outlet 22 to the suction pump through the pipeline, open the built-in valve, and start filtration. After filtration, add a quantitative amount of ultrapure water through the solution inlet 21 to rinse the filtration.
[0039] Step 3: Remove the pipeline connecting the solution outlet 22, and close the built-in valves of the solution inlet 21 and the solution outlet 22, open the built-in valve of the air outlet 23, connect the buffer chamber with the air filter membrane and the vacuum pump in sequence through the pipeline, control the temperature in the crystallization dryer 2 to 60~70℃ through the crystallization constant temperature heat exchanger 27, turn on the vacuum pump and the motor in the adjustable stabilizer 2 305, control the rotation rate and vacuum degree, dry the aminosulfonic acid in the crystallization dryer 2, and after 3~5h, turn off the vacuum pump and the motor and cool down until the temperature in the crystallization dryer 2 is ≤30℃, close the built-in valve of the air outlet 23, open the hydraulic lift 33 and lower the adjustable stabilizer 1 34, so that the right end of the crystallization dryer drops below the left end and forms a -20° angle with the horizontal plane, connect the discharge port 26 to the dust-free packaging machine through a pipeline, turn on the built-in switch, and take out the product and package it through the packaging machine. The parallel crystallization dryers are also operated as above to obtain electronic grade aminosulfonic acid with a purity of >99.99%.
[0040] The above is a preferred embodiment of the present invention. For ordinary technicians in this field, based on the teachings of the present invention, without departing from the principles and spirit of the present invention, changes, modifications, replacements and variations made to the implementation methods are still within the scope of protection of the present invention.
Claims
1. A purification device for electronic grade chemicals, characterized in that: include: A dissolving kettle (1), a crystallization dryer (2) and a fixed platform (3), wherein the upper end of the dissolving kettle (1) is provided with a raw material feed port (11) and a water inlet (12), the lower section is provided with a dissolving liquid outlet (13), and the outer wall is provided with a dissolving constant temperature heat exchanger (14), the raw material feed port (11) is connected to a solid feeding device through a pipeline and is connected in series with a valve, and the water inlet (12) is connected to an ultrapure water supply device through a pipeline and is connected in series with a valve, an electronic flow meter and a transmission pump; The left end of the crystallization dryer (2) is provided with a solution inlet (21), a solution outlet (22) and a rotating left shaft (24), the right end is provided with an air outlet (23), a rotating right shaft (25) and a crystal discharge port (26), and the outer wall is provided with a constant temperature heat exchanger (27), the solution inlet (21) is connected to the dissolution outlet (13) of the dissolution kettle through a pipeline and is connected in series with a valve, a suction pump and an electronic flow meter, the solution outlet (22) is connected to the crystallization water recovery device through a pipeline and is connected in series with a valve and a suction pump, the air outlet (23) is connected to a vacuum pump through a pipeline, and the crystal discharge port (26) is connected to a dust-free packaging machine through a pipeline; The base (31) of the fixed platform (3) is placed in a plane, a support rod (32) is erected at one end of the base, and an adjustable stabilizer 2 (35) is embedded in the support rod. A hydraulic lift (33) is fixedly placed at the other end of the base, and an adjustable stabilizer 1 (34) is fixedly placed on the hydraulic lift. The adjustable stabilizer 2 (35) is connected to the left rotating shaft (24) of the crystallization dryer, and the adjustable stabilizer 1 (34) is connected to the right rotating shaft (25) of the crystallization dryer.
2. The device for purifying electronic-grade chemicals according to claim 1, wherein: The crystallization dryer (2) is a hollow cylindrical structure with an aspect ratio of 3 to 5, and the circular surfaces at both ends are perpendicular to the ground; the solution inlet (21), solution outlet (22), gas outlet (23) and crystal discharge port (26) of the crystallization dryer are built with valves and can be separated from the pipelines connected thereto.
3. The device for purifying electronic-grade chemicals according to claim 1, wherein: The rotating left shaft (24) and the rotating right shaft (25) of the crystallization dryer (2) are both composed of a left shaft fixing tube and a left shaft rotating shaft; the left end of the left shaft fixing tube (241) of the rotating left shaft (24) is fixed to the second adjustable stabilizer (35) by a snap connection, the right end is sleeved on the left end of the left shaft rotating shaft (242), and the right end of the left shaft rotating shaft (242) is connected and fixed to the center of the left circular surface of the crystallization dryer body; the right end of the right shaft fixing tube (251) of the rotating right shaft (25) is fixed to the first adjustable stabilizer (34) by a snap connection, the left end is sleeved on the right end of the right shaft rotating shaft (252), and the left end of the right shaft rotating shaft (252) is connected and fixed to the center of the right circular surface of the crystallization dryer body.
4. The device for purifying electronic-grade chemicals according to claim 1 or 3, characterized in that: The adjustable stabilizer (34) is composed of a detachable upper buckle (341), an adjustable angle lower buckle (342) and a fixed base (343). The detachable upper buckle (341) and the adjustable angle lower buckle (342) are engaged with the right end of the right shaft fixing tube (251) of the rotating right shaft to fix the right shaft. The connecting and fixing surface of the adjustable angle lower buckle (342) and the fixed base (343) is an arc surface. The adjustable angle lower buckle (342) can rotate along the arc surface as the hydraulic lift (33) rises and falls to match the angle change caused by the rise and fall of the rotating right shaft (25) of the crystallizer dryer.
5. The device for purifying electronic-grade chemicals according to claim 1 or 3, characterized in that: The adjustable stabilizer 2 (35) is composed of an upper and lower telescopic buckle (351) and an adjustable angle base (352). The upper and lower telescopic buckle (351) is fixed to the left end of the left axis fixing tube (241) that is engaged with the rotating left axis by moving up and down. The embedded surface of the adjustable angle base (352) and the support rod (32) is arc-shaped. The adjustable angle base (352) has a built-in motor. The adjustable angle base (352) can rotate vertically along the arc surface to match the angle change caused by the rotating left axis (24) of the crystal drying box following the rotating right axis (25) to rise and fall.
6. The device for purifying electronic-grade chemicals according to claim 1, wherein: The crystallization dryers and the fixing tables are arranged in groups of two, and multiple groups of crystallization dryers are connected in parallel.
7. The device for purifying electronic-grade chemicals according to claim 1, wherein: The inner walls of the dissolving kettle (1) and the crystallization dryer (2) are made of polytetrafluoroethylene or ceramic, and the connecting pipelines are made of polypropylene.