A process for extracting electronic-grade isopropanol from industrial isopropanol
Through the combination process of multi-stage filtration and distillation combined with the dehydration tower and auxiliary dehydrator, the design of heat heat exchange and oozing vaporization membrane tubes has been solved, and the goal of efficient production of electronic grade isopropanol is achieved.
Patent Information
- Application Number
- CN202510055985.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-14
- Publication Date
- 2025-07-29
- Estimated Expiration
- 2045-01-14
AI Technical Summary
The prior art has high energy consumption when producing electronic grade isopropanol, making it difficult to effectively reduce the water content to below 100 ppm, and the equipment investment is large.
The combination process of multi-stage filtration and distillation combined with dehydration tower and auxiliary dehydrator is adopted to use the heat of the distillate of the dehydration tower for heat exchange, and combined with the design of the exudate vaporized membrane tube and the vibrating plate to promote moisture condensation and uniform distribution and improve dehydration efficiency.
It reduces the energy consumption of the refining process, improves the production efficiency and product quality of electronic grade isopropanol, and reduces equipment investment.
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Figure CN119798043B_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of isopropanol production, and specifically relates to a process for extracting electronic-grade isopropanol from industrial isopropanol. Background Art
[0002] Electronic-grade isopropanol is mainly used as a super-clean cleaning, drying organic solvent for precision electronic components such as chips, liquid crystals, magnetic heads, and circuit boards during processing, and as a super-clean cleaning organic solvent for tools in the clean room. Among them, the product quality of electronic-grade isopropanol seriously affects the yield of tight electronic components. When isopropanol contains trace metal elements, it is very easy to cause the breakdown of integrated circuits or semiconductor components, affecting the product life.
[0003] At present, the price difference between electronic-grade isopropanol and industrial-grade isopropanol is significant. Usually, industrial-grade isopropanol is used as the raw material, and after more refined separation, purification, and refinement, electronic-grade isopropanol is obtained. The main technical difficulty in producing electronic-grade isopropanol is that the water content is required to be less than 100 ppm, and at the same time, the content of impurities such as acetone and isopropyl ether is less than 3 ppm. The water content of ordinary isopropanol is about 3000 ppm, and it also contains about 200 ppm of impurities such as acetone and isopropyl ether. Isopropanol and water are miscible, and an azeotrope will be formed during the rectification separation process, which not only consumes a large amount of energy but also makes it difficult to dehydrate to less than 200 ppm.
[0004] In the prior art, the technologies of rectifying, high-temperature gas-phase adsorption, or molecular sieve membrane for refining isopropanol consume a large amount of energy and require high equipment investment. Summary of the Invention
[0005] In order to make up for the deficiencies of the prior art, make full use of the heat in the extraction process, reduce the energy consumption in the refining process, and at the same time, promote the condensation and liquefaction of water vapor in the auxiliary dehydrator, reduce the partial pressure of water vapor components on the other side of the membrane, promote the removal of water, and improve the removal effect and efficiency, the present invention proposes a process for extracting electronic-grade isopropanol from industrial isopropanol.
[0006] The technical solution adopted by the present invention to solve its technical problems is: The process for extracting electronic-grade isopropanol from industrial isopropanol according to the present invention includes the following steps:
[0007] S1: Perform multi-stage pre-filtration treatment on the raw material isopropanol to remove large-particle impurities carried in the raw material isopropanol. Then, perform light-component rectification and heavy-component rectification on the raw material isopropanol to remove the light components and heavy components contained in the isopropanol raw material, and obtain a secondary raw material;
[0008] S2: Input the secondary raw materials into the dehydration adsorption device for treatment to remove the moisture contained in the materials, obtaining the tertiary raw materials: First, feed the materials into the dehydration tower, and directly send the vaporized materials distilled from the top of the dehydration tower into the auxiliary dehydrator to remove the remaining moisture in the materials through the permeable vaporization membrane; among them, a detector and a temporary storage tank are arranged behind the auxiliary dehydrator: The tertiary raw materials with unqualified moisture content detection are stored in the temporary storage tank, and then the materials in the temporary storage tank are input into the dehydration tower for circulation, and the tertiary raw materials with qualified moisture content detection are directly transported from the temporary storage tank to the subsequent processing equipment;
[0009] S3: Input the tertiary raw materials into the ion tank to remove the metal ions contained therein, obtaining the quaternary raw materials;
[0010] S4: Input the quaternary raw materials into the filtration and separation equipment to remove the impurity particles therein, obtaining the electronic grade isopropyl alcohol product;
[0011] Among them, the components with boiling points lower and higher than isopropyl alcohol in the S1 step are light components and heavy components in sequence; in the S1 step, the raw material isopropyl alcohol is subjected to light component removal and heavy component removal through a multi-stage distillation column; the ion tank and the filtration and separation equipment in the S3 and S4 steps are arranged in series in multiple stages; the ion tank is filled with ion exchange resin;
[0012] Among them, the water absorption and desorption device includes a dehydration tower and an auxiliary dehydrator, and the product outlet on the dehydration tower is communicated with the auxiliary dehydrator;
[0013] An upper isolation plate and a lower isolation plate are installed in the auxiliary dehydrator from top to bottom, and the upper isolation plate and the lower isolation plate divide the space in the auxiliary dehydrator into a separation chamber, a heat exchange chamber, and an exudation chamber from top to bottom. A heat preservation layer is installed outside the auxiliary dehydrator;
[0014] A feed port and a discharge port are installed in the separation chamber, an input port and an output port are installed in the heat exchange chamber, and an exudate port is installed in the exudation chamber;
[0015] A fixing plate is installed in the separation chamber, an exudative vaporization membrane tube is installed between the fixing plate and the lower isolation plate, a heat pipe is installed in the exudative vaporization membrane tube, the upper end of the heat pipe passes through the upper isolation plate and is located in the heat exchange chamber, the heat pipe is fixed by the upper isolation plate, the space between the fixing plate and the upper isolation plate is an air extraction chamber, an air extraction port is installed in the air extraction chamber, the air extraction chamber and the exudation chamber are communicated with each other through the exudative vaporization membrane tube, and a retaining ring is installed on the part of the heat pipe located in the air extraction chamber.
[0016] Preferably, a limiting frame is installed in the exudative vaporization membrane tube to clamp and fix the heat pipe;
[0017] The surfaces of the heat pipe and the limiting frame are provided with a hydrophobic coating.
[0018] Preferably, grooves are provided on the surface of the heat pipe, and protrusions are provided on the limiting frame, and the protrusions and the grooves cooperate with each other;
[0019] A deformation sheet is installed on the limiting frame, and the deformation sheet is a bimetallic sheet.
[0020] Preferably, a vibrating plate is installed in the separation chamber, a connecting rod is installed on the vibrating plate, and both ends of the connecting rod are respectively connected to the fixing plate and the lower partition plate;
[0021] Multiple groups of the vibrating plates are arranged in the separation chamber, and each group of the vibrating plates is composed of multiple units from top to bottom, and the vibrating plates are located at positions close to the pervaporation membrane tubes.
[0022] Preferably, the connecting rod is located at a position close to the middle on the vibrating plate, and the installation positions of the connecting rods on each group of the vibrating plates are different.
[0023] Preferably, an elastic tube sleeve is installed on the connecting rod, and the vibrating plates on the connecting rod are fixed by the elastic tube sleeve, and the vibrating plates are slidably installed on the connecting rod.
[0024] Preferably, uniformly distributed through holes are provided on the vibrating plate.
[0025] Preferably, elastic wires are installed on the side surface of the vibrating plate, and the elastic wires contact the surface of the pervaporation membrane tube.
[0026] The beneficial effects of the present invention are as follows:
[0027] 1. For the process of extracting electronic-grade isopropanol from industrial isopropanol according to the present invention, through the mutual cooperation of the dehydration tower and the auxiliary dehydrator, the heat carried out from the dehydration tower by the material is fully utilized, and the raw material isopropanol is heat-exchanged in the auxiliary dehydrator to increase the temperature of the raw material isopropanol, so as to fully utilize the heat in the extraction process, reduce the energy consumption in the refining process, and improve the effect and efficiency of extracting electronic-grade isopropanol.
[0028] 2. For the process of extracting electronic-grade isopropanol from industrial isopropanol according to the present invention, by providing the pervaporation membrane tubes, heat pipes, heat exchange chambers, and limiting frames, the water entering the pervaporation membrane tubes will condense and liquefy after contacting the surface of the heat pipes, so that the partial pressure of the water component inside the pervaporation membrane tubes is further reduced, thereby promoting the removal of water from the material and improving the efficiency and effect of dehydration.
[0029] 3. In the process of extracting electronic-grade isopropanol from industrial isopropanol according to the present invention, by setting a vibrating plate, a connecting rod, an elastic tube sleeve and through holes, the vibrating plate vibrates to stir and disturb the material, promoting the uniform distribution of the material, avoiding the phenomenon of concentration polarization near the osmotic vaporization membrane tube, preventing the blockage of the permeation membrane, and improving the dehydration effect and efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] The present invention will be further described below with reference to the accompanying drawings.
[0031] Figure 1 is a schematic diagram of the process principle for extracting electronic-grade isopropanol according to the present invention;
[0032] Figure 2 is a process flow block diagram of the present invention;
[0033] Figure 3 is a front view of the auxiliary dehydrator in the present invention;
[0034] Figure 4 is a schematic structural diagram of the auxiliary dehydrator in the present invention;
[0035] Figure 5 is a schematic structural diagram of the vibrating plate and the connecting rod in the auxiliary dehydrator of the present invention;
[0036] Figure 6 is a schematic installation diagram of the osmotic vaporization membrane tube and the heat pipe in the auxiliary dehydrator of the present invention;
[0037] In the figure: light component removal tower 1, heavy component removal tower 2, dehydration tower 3, auxiliary dehydrator 4, separation chamber 41, feed inlet 411, air extraction port 412, discharge port 413, fixing plate 414, osmotic chamber 42, osmotic liquid outlet 421, lower partition plate 422, heat exchange chamber 43, input port 431, output port 432, upper partition plate 433, osmotic vaporization membrane tube 44, vibrating plate 45, connecting rod 451, elastic tube sleeve 452, through hole 453, heat pipe 46, groove 461, limiting frame 462, deformation piece 463, retaining ring 464, ion tank 5, filtration and separation equipment 6. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0038] In order to make the technical means, creative features, achieved purposes and effects of the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.
[0039] As Figures 1 to 6 shown, in the process of extracting electronic-grade isopropanol from industrial isopropanol according to the present invention, the process includes the following steps:
[0040] S1: Perform multi-stage pre-filtration on the raw material isopropanol to remove large particulate impurities contained in the raw material isopropanol. Then, perform light-component removal rectification and heavy-component removal rectification on the raw material isopropanol to remove the light components and heavy components contained in the isopropanol raw material, and obtain a secondary raw material;
[0041] S2: Input the secondary raw material into a dehydration adsorption device for treatment to remove the moisture contained in the material and obtain a tertiary raw material: First, send the material into a dehydration tower 3, and directly send the vaporized material distilled from the top of the dehydration tower 3 into an auxiliary dehydrator 4 to remove the remaining moisture in the material through an exudation vaporization membrane; Among them, a detector and a temporary storage tank are arranged behind the auxiliary dehydrator 4: The tertiary raw material with unqualified moisture content detection is stored in the temporary storage tank, and then the material in the temporary storage tank is input into the dehydration tower 3 for circulation, and the tertiary raw material with qualified moisture content detection is directly transported from the temporary storage tank to subsequent processing equipment;
[0042] S3: Input the tertiary raw material into an ion tank 5 to remove the metal ions contained therein and obtain a quaternary raw material;
[0043] S4: Input the quaternary raw material into a filtration and separation device 6 to remove the impurity particles present therein and obtain an electronic-grade isopropanol product;
[0044] Among them, the components with boiling points lower and higher than isopropanol in the S1 step are light components and heavy components in sequence; In the S1 step, the raw material isopropanol is subjected to light-component removal and heavy-component removal through a multi-stage rectification tower; The ion tank 5 and the filtration and separation device 6 in the S3 and S4 steps are arranged in multiple stages in series; The ion tank 5 is filled with ion exchange resin;
[0045] Among them, the water absorption and desorption device includes a dehydration tower 3 and an auxiliary dehydrator 4, and the product outlet on the dehydration tower 3 is connected to the auxiliary dehydrator 4;
[0046] An upper partition plate 433 and a lower partition plate 422 are installed in the auxiliary dehydrator 4 from top to bottom. The upper partition plate 433 and the lower partition plate 422 divide the space inside the auxiliary dehydrator 4 into a separation chamber 41, a heat exchange chamber 43, and an exudation chamber from top to bottom. A heat preservation layer is installed outside the auxiliary dehydrator 4;
[0047] A feed inlet 411 and a discharge outlet 413 are installed in the separation chamber 41, an input port 431 and an output port 432 are installed in the heat exchange chamber 43, and an exudate port 421 is installed in the exudation chamber 42;
[0048] A fixed plate 414 is installed in the separation chamber 41, and a seepage vaporization membrane tube 44 is installed between the fixed plate 414 and the lower isolation plate 422. A heat pipe 46 is installed in the seepage vaporization membrane tube 44. The upper end of the heat pipe 46 passes through the upper isolation plate 433 and is located in the heat exchange chamber 43. The heat pipe 46 is fixed by the upper isolation plate 433. The space between the fixed plate 414 and the upper isolation plate 433 is an air extraction chamber. An air extraction port 412 is installed in the air extraction chamber. The air extraction chamber and the seepage chamber 42 are connected to each other through the seepage vaporization membrane tube 44. A retaining ring 464 is installed on the portion of the heat pipe 46 located in the air extraction chamber.
[0049] During operation, the raw material isopropyl alcohol is sequentially fed into the light removal tower 1 and the heavy removal tower 2, thereby fully removing the light components and heavy components in the raw material, such as acetone, water, and some metal ions. After that, the material after light and heavy removal is fed into the adsorption dehydration device for dehydration. After dehydration, the material is sequentially fed into the ion tank 5 and the filtration separation equipment 6 to remove the remaining trace metal ions and particulate impurities in the material as much as possible, thereby ensuring that a high-quality electronic-grade isopropyl alcohol product is obtained; wherein, the unspecified parts in this process are implemented using technical methods known in the prior art;
[0050] In the dehydration process, the material transported from the deweight removal tower 2 first enters the dehydration tower 3, where it is dehydrated to remove most of the remaining water in the material. Afterwards, the material distilled from the dehydration tower 3 is input from the feed port 411 into the auxiliary dehydrator 4 for further dehydration to remove as much remaining water as possible. Afterwards, the material discharged from the discharge port 413 subsequently enters the ion tank 5 and the filtration separation device 6.
[0051] At the same time, the pipe between the dehydration tower 3 and the feed inlet 411 is an insulated pipe, and the auxiliary dehydrator 4 is arranged near the dehydration tower 3, ensuring that the length of the insulated pipe between the dehydration tower 3 and the feed inlet 411 is short and the temperature of the material transported in the pipe does not drop too much, so that the material entering the separation chamber 41 of the auxiliary dehydrator 4 is in a vaporized state, fully utilizing the heat and improving the working efficiency of the equipment. As another embodiment, according to actual conditions, an evaporator is provided at the auxiliary dehydrator 4 to further heat the material to ensure that the raw material is in a vaporized state when entering the separation chamber 41;
[0052] At the same time, after the material enters the auxiliary dehydrator 4, the material is located in the separation chamber 41, and the external vacuum pump extracts air from the air extraction port 412, so that the pressure in the air extraction chamber, the inside of the seepage vaporization membrane tube 44, and the seepage chamber 42 is reduced, so that the water in the material seeps and separates into the inside of the seepage vaporization membrane tube 44, and then the water enters the seepage chamber 42 and is discharged from the seepage liquid port 421, completing the removal of water from the material and ensuring that the water content of the material is low after treatment;
[0053] Meanwhile, the relatively low-temperature raw material isopropyl alcohol enters the heat exchange chamber 43 from the input port 431. After heat exchange, the temperature-increased isopropyl alcohol leaves from the output port 432 and is fed into the inlet of the light component removal tower 1, improving the utilization of heat in the production process and reducing energy consumption. At the same time, since the upper end of the heat pipe 46 is located in the heat exchange chamber 43 and the lower end of the heat pipe 46 is located in the pervaporation membrane tube 44, the heat contained in the moisture that enters the pervaporation membrane tube 44 and contacts the surface of the heat pipe 46 will be transferred to the heat exchange chamber 43, thereby promoting the rapid condensation and liquefaction of the moisture in the pervaporation membrane tube 44, reducing the partial pressure of the moisture component in the pervaporation membrane tube 44, and promoting the separation and collection of the moisture contained in the material in the separation chamber 41 through the pervaporation membrane tube 44, improving the efficiency and effect of moisture removal from the material;
[0054] Meanwhile, after the moisture in the pervaporation membrane tube 44 condenses and liquefies on the surface of the heat pipe 46, it will slide downward under the action of gravity and enter the seepage chamber 42, and finally be discharged from the seepage liquid outlet 421 in the seepage chamber 42. During this process, the moisture discharged from the air extraction port 412 is relatively reduced, thereby reducing the moisture content in the gas entering the vacuum pump pipeline system and reducing the possibility of the vacuum pump malfunctioning due to excessive moisture content. At the same time, the retaining ring 464 on the heat pipe 46 is close to the opening of the pervaporation membrane tube 44 in the air extraction chamber, so as to block the tiny liquid droplets driven by the air flow on the surface of the heat pipe 46 through the retaining ring 464, reducing the possibility of the liquid droplets flying away from the surface of the heat pipe 46 driven by the air flow and leaving the air extraction chamber from the air extraction port 412; at the same time, the liquid discharged from the seepage liquid outlet 421 can also be conveniently collected and processed, avoiding the situation that it is difficult to collect and process the moisture after the moisture is pumped into the pipeline system of the vacuum pump along with the air.
[0055] As an embodiment of the present invention, a limiting frame 462 is installed in the pervaporation membrane tube 44, and the limiting frame 462 clamps and fixes the heat pipe 46;
[0056] The surfaces of the heat pipe 46 and the limiting frame 462 are provided with a hydrophobic coating;
[0057] Since the length of the pervaporation membrane tube 44 is relatively long and the diameter of the heat pipe 46 is relatively thin, the heat pipe 46 inside the auxiliary dehydrator 4 is likely to swing and vibrate during operation, resulting in contact or collision between the heat pipe 46 and the inner wall of the pervaporation membrane tube 44, affecting the normal use of the pervaporation membrane tube 44, and the contact between the heat pipe 46 and the pervaporation membrane tube 44 is likely to cause the temperature of the surface of the pervaporation tube to decrease, making the vaporized material in the separation chamber 41 prone to premature cooling and liquefaction, affecting the dehydration and separation effect;
[0058] Meanwhile, a limiting frame 462 is installed inside the pervaporation membrane tube 44. The heat pipe 46 is clamped and fixed by the limiting frame 462 to ensure the stable position of the heat pipe 46 inside the pervaporation membrane tube 44, and to prevent the heat pipe 46 from swinging or vibrating, which may affect the normal use and service life of the heat pipe 46 and the pervaporation membrane tube 44.
[0059] As an embodiment of the present invention, a groove 461 is provided on the surface of the heat pipe 46, and a protrusion is provided on the limiting frame 462. The protrusion and the groove 461 cooperate with each other.
[0060] A deformation sheet 463 is installed on the limiting frame 462, and the deformation sheet 463 is a bimetallic sheet.
[0061] Through the mutual cooperation of the protrusion on the limiting frame 462 and the groove 461 on the heat pipe 46, the position of the heat pipe 46 inside the pervaporation membrane tube 44 is stabilized, and the limiting frame 462 is prevented from skewing or shifting under the influence of external vibration or external force, which may cause the position of the limiting frame 462 to be unstable and affect the normal use of the auxiliary dehydrator 4.
[0062] Meanwhile, since the deformation sheet 463 made of a bimetallic sheet is installed on the limiting frame 462, during the dehydration process, the temperature inside the pervaporation membrane tube 44 rises, causing the deformation sheet 463 on the limiting frame 462 to deform due to heat. As a result, the limiting frame 462 becomes an interference fit between the heat pipe 46 and the inner wall of the pervaporation membrane tube 44, further improving the stability of the limiting frame 462 and ensuring the stable position of the heat pipe 46.
[0063] As an embodiment of the present invention, a vibrating plate 45 is installed in the separation chamber 41. A connecting rod 451 is installed on the vibrating plate 45, and both ends of the connecting rod 451 are respectively connected to the fixed plate 414 and the lower partition plate 422.
[0064] Multiple groups of the vibrating plates 45 are provided in the separation chamber 41. Each group of the vibrating plates 45 is composed of multiple units from top to bottom, and the vibrating plates 45 are located close to the pervaporation membrane tube 44.
[0065] Since multiple groups of vibrating plates 45 are installed in the separation chamber 41 and the vibrating plates 45 are located close to the pervaporation membrane tube 44, when the material enters the separation chamber 41, the material will be blocked and disturbed by the vibrating plates 45, so that the material is evenly distributed in the separation chamber 41 and the residence time of the material in the separation chamber 41 is extended, thereby improving the efficiency and effect of material dehydration.
[0066] Meanwhile, after the material impacts the vibrating plate 45, the vibrating plate 45 will move, causing the material near the vibrating plate 45 to be agitated. Additionally, since the vibrating plate 45 is located near the osmotic vaporization membrane tube 44, after the material is agitated by the vibrating plate 45, it will further evenly distribute the material near the osmotic vaporization membrane tube 44, thereby effectively reducing the possibility of concentration polarization near the osmotic vaporization membrane tube 44, preventing the permeable membrane from being blocked, and ensuring good dehydration effect and efficiency of the auxiliary dehydrator 4.
[0067] As an embodiment of the present invention, the connecting rod 451 is located at a position near the middle on the vibrating plate 45, and the installation positions of the connecting rods 451 on each group of vibrating plates 45 are different;
[0068] Since the installation positions of the connecting rods 451 on each group of vibrating plates 45 are different, the vibration amplitudes and frequencies of each group of vibrating plates 45 when vibrating under impact are different, and further, it will fully disturb the material in the separation chamber 41, promoting the uniform distribution of the material, avoiding the occurrence of concentration polarization phenomenon, and ensuring the water removal effect of the material. At the same time, since the vibration amplitudes and frequencies between each group of vibrating plates 45 are different, it can also avoid resonance between the vibrating plates 45, ensuring the safety of the operation of the auxiliary dehydrator 4.
[0069] As an embodiment of the present invention, an elastic tube sleeve 452 is installed on the connecting rod 451, and the vibrating plates 45 on the connecting rod 451 are fixed through the elastic tube sleeve 452, and the vibrating plate 45 is slidably installed on the connecting rod 451;
[0070] Since the vibrating plate 45 is slidably installed on the connecting rod 451, when the vibrating plate 45 is affected by the impact of the material and external vibration, the vibrating plate 45 will slide up and down on the link rod, thereby expanding the range of the vibrating plate 45 agitating the material, promoting the uniform distribution of the material near the osmotic vaporization membrane tube 44, avoiding the occurrence of concentration polarization phenomenon, and ensuring the smooth progress of material dehydration. At the same time, since the elastic tube sleeve 452 is installed on the connecting rod 451 and the elastic tube sleeve 452 is located between adjacent vibrating plates 45, the vibrating plates 45 will be evenly distributed on the connecting rod 451 under the elastic action of the elastic tube sleeve 452, and there is an interconnection between the vibrating plates 45 on the connecting rod 451. Furthermore, after the vibrating plate 45 slides up and down, it will drive the entire group of vibrating plates 45 installed on the connecting rod 451 to move, fully expanding the agitation effect of the vibrating plate 45 on the material, agitating the material near the osmotic vaporization membrane tube 44, promoting the uniform distribution of the material, and facilitating the removal of water in the material.
[0071] As an embodiment of the present invention, the vibrating plate 45 is provided with uniformly distributed through holes 453;
[0072] Since through holes 453 are formed in the vibrating plate 45, during the up-and-down movement and vibration of the vibrating plate 45, the materials in the separation chamber 41 pass through the through holes 453, causing disordered flow of the materials, thereby increasing the degree of dispersion and uniformity of the materials, avoiding overly orderly flow of the materials, and preventing the occurrence of concentration polarization near the pervaporation membrane tube, which affects the water removal effect of the materials;
[0073] Meanwhile, the through holes 453 reduce the relative acting area between the vibrating plate 45 and the materials during vibration and up-and-down movement, so that the resistance of the interaction between the vibrating plate 45 and the materials during movement is reduced, facilitating the vibration and up-and-down movement of the vibrating plate 45, improving the disturbing effect on the materials near the pervaporation membrane tube 44, making the materials evenly distributed, and promoting the water removal of the materials.
[0074] As an embodiment of the present invention, elastic wires are installed on the side surface of the vibrating plate 45, and the elastic wires contact the surface of the pervaporation membrane tube 44;
[0075] Since the vibrating plate 45 is located near the pervaporation membrane tube 44, when the vibrating plate 45 vibrates and moves up and down, the elastic wires on the vibrating plate 45 will sweep on the surface of the pervaporation membrane tube 44, simply cleaning the surface of the pervaporation membrane tube 44, removing impurities attached to the surface of the pervaporation membrane tube 44 during the material dehydration process, reducing the possibility of blockage of the pervaporation membrane tube, and thus ensuring the normal use of the auxiliary dehydrator 4.
[0076] The specific working process is as follows:
[0077] During operation, the raw material isopropyl alcohol is successively fed into the light component removal tower 1 and the heavy component removal tower 2 to fully remove the light components and heavy components in the raw material. After that, the material after light and heavy component removal is fed into the adsorption dehydration device for dehydration. After dehydration, the material is successively fed into the ion tank 5 and the filtration and separation equipment 6 to remove the remaining trace metal ions and particulate impurities in the material; among them, the parts not specified in this process are implemented by known technical methods in the prior art;
[0078] Among them, during the dehydration process, the material transported by the heavy component removal tower 2 first enters the dehydration tower 3 for dehydration. After that, the material distilled out from the dehydration tower 3 is input into the auxiliary dehydrator 4 from the feed port 411 for further dehydration. After that, the material discharged from the discharge port 413 enters the ion tank 5 and the filtration and separation equipment 6;
[0079] Meanwhile, the pipeline between the dehydration tower 3 and the feed port 411 is a heat-insulating pipeline, and the auxiliary dehydrator 4 is arranged close to the dehydration tower 3, so that the material entering the separation chamber 41 on the auxiliary dehydrator 4 is in a vaporized state; wherein, as another implementation manner, according to the actual situation, an evaporator is arranged at the auxiliary dehydrator 4 to further heat the material;
[0080] Meanwhile, after the material enters the auxiliary dehydrator 4, the material is located in the separation chamber 41, and an external vacuum pump evacuates from the air extraction port 412, reducing the pressure in the air extraction chamber, inside the seepage vaporization membrane tube 44, and inside the seepage chamber 42, so that the water in the material seeps out and is separated into the inside of the seepage vaporization membrane tube 44, and then the water enters the seepage chamber 42 and is discharged from the seepage liquid outlet 421;
[0081] Meanwhile, the relatively low-temperature raw material isopropyl alcohol enters the heat exchange chamber 43 from the input port 431, and the raw material isopropyl alcohol with an increased temperature after heat exchange leaves from the output port 432 and is sent to the inlet of the light component removal tower 1. At the same time, the heat pipe 46 will transfer the heat contained in the water in contact with the surface of the heat pipe 46 inside the seepage vaporization membrane tube 44 to the heat exchange chamber 43, causing the water inside the seepage vaporization membrane tube 44 to quickly condense and liquefy, reducing the component partial pressure of the water inside the seepage vaporization membrane tube 44, and promoting the separation and collection of the water contained in the material in the separation chamber 41 through the seepage vaporization membrane tube 44;
[0082] Meanwhile, after the water inside the seepage vaporization membrane tube 44 condenses and liquefies on the surface of the heat pipe 46, it will slide down under the action of gravity and enter the seepage chamber 42, and finally be discharged from the seepage liquid outlet 421 in the seepage chamber 42. During this process, the water discharged from the air extraction port 412 is relatively reduced, thereby reducing the water content in the gas entering the vacuum pump pipeline system. At the same time, the retaining ring 464 on the heat pipe 46 is close to the opening of the seepage vaporization membrane tube 44 in the air extraction chamber, and the retaining ring 464 blocks the tiny droplets driven by the airflow on the surface of the heat pipe 46, reducing the possibility of the droplets flying away from the surface of the heat pipe 46 driven by the airflow and leaving the air extraction chamber from the air extraction port 412;
[0083] A limiting frame 462 is installed inside the seepage vaporization membrane tube 44, and the limiting frame 462 is used to clamp and fix the heat pipe 46 to ensure the stable position of the heat pipe 46 inside the seepage vaporization membrane tube 44;
[0084] Through the mutual cooperation of the protrusions on the limiting frame 462 and the grooves 461 on the heat pipe 46, the position of the heat pipe 46 inside the seepage vaporization membrane tube 44 is stable, and the limiting frame 462 is prevented from being skewed or displaced under the influence of external vibration or external force;
[0085] Meanwhile, since the deformation piece 463 made of bimetal is installed on the limit frame 462, during the dehydration process, the temperature inside the exudation vaporization film tube 44 rises, causing the deformation piece 463 on the limit frame 462 to deform due to heat, making the limit frame 462 have an interference fit between the heat pipe 46 and the inner wall of the exudation vaporization film tube 44;
[0086] When the material enters the separation chamber 41, the material will be blocked and disturbed by the vibrating vane plate 45, so that the material is evenly distributed in the separation chamber 41 and the residence time of the material in the separation chamber 41 is extended;
[0087] Meanwhile, after the material impacts the vibrating vane plate 45, the vibrating vane plate 45 will move, causing the material near the vibrating vane plate 45 to be agitated. In addition, since the vibrating vane plate 45 is located near the exudation vaporization film tube 44, after the material is agitated by the vibrating vane plate 45, it will further evenly distribute the material near the exudation vaporization film tube 44 and reduce the possibility of concentration polarization near the exudation vaporization film tube 44;
[0088] Since the installation positions of the connecting rods 451 on the vibrating vane plates 45 of each group are different, the vibration amplitudes and frequencies of the vibrating vane plates 45 of each group are different when they are impacted and vibrate, and thus will fully disturb the material in the separation chamber 41, promoting the uniform distribution of the material. At the same time, since the vibration amplitudes and frequencies between the vibrating vane plates 45 of each group are different, the resonance between the vibrating vane plates 45 can also be avoided;
[0089] Since the vibrating vane plate 45 is slidably installed on the connecting rod 451, when the vibrating vane plate 45 is affected by the impact of the material and external vibration, the vibrating vane plate 45 will slide up and down on the connecting rod, expanding the range of the material agitated by the vibrating vane plate 45. At the same time, since the elastic tube sleeve 452 is installed on the connecting rod 451 and the elastic tube sleeve 452 is located between adjacent vibrating vane plates 45, the vibrating vane plates 45 will be evenly distributed on the connecting rod 451 under the elastic action of the elastic tube sleeve 452, and there will be an interconnection between the vibrating vane plates 45 on the connecting rod 451. Therefore, after the vibrating vane plate 45 slides up and down, it will drive the entire group of vibrating vane plates 45 installed on the connecting rod 451 to move, fully expanding the agitation effect of the vibrating vane plate 45 on the material;
[0090] Since through holes 453 are provided on the vibrating vane plate 45, during the up and down movement and vibration of the vibrating vane plate 45, the material in the separation chamber 41 passes through the through holes 453, causing the disordered flow of the material;
[0091] Meanwhile, through the through hole 453 provided, the acting area between the vibrating plate 45 and the material is relatively reduced during vibration and vertical movement, so that the resistance of the interaction between the vibrating plate 45 and the material during movement is reduced, facilitating the vibration and vertical movement of the vibrating plate 45;
[0092] Since the vibrating plate 45 is located near the pervaporation membrane tube 44, when the vibrating plate 45 vibrates and moves vertically, the elastic wires on the vibrating plate 45 will sweep on the surface of the pervaporation membrane tube 44, simply cleaning the surface of the pervaporation membrane tube 44 and removing the impurities adhering to the surface of the pervaporation membrane tube 44 during the material dehydration process.
[0093] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments. The above embodiments and the descriptions in the specification only illustrate the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the scope of the present invention claimed. The scope of the present invention claimed is defined by the appended claims and their equivalents.
Claims
1. A process for extracting electronic-grade isopropanol from industrial isopropanol, characterized in that: The process includes the following steps: S1: Perform multi-stage pre-filtration on the raw material isopropyl alcohol to remove large particle impurities contained in the raw material isopropyl alcohol. Then, perform light component removal distillation and heavy component removal distillation on the raw material isopropyl alcohol to remove the light components and heavy components contained in the isopropyl alcohol raw material, obtaining a secondary raw material; S2: Input the secondary raw material into a dehydration adsorption device for treatment to remove the water contained in the material, obtaining a tertiary raw material: First, feed the material into a dehydration tower (3), and directly feed the vaporized material distilled from the top of the dehydration tower (3) into an auxiliary dehydrator (4) to remove the remaining water in the material through a permeable vaporization membrane; wherein, a detector and a temporary storage tank are arranged behind the auxiliary dehydrator (4): The tertiary raw material with unqualified water content detection is stored in the temporary storage tank, and then the material in the temporary storage tank is input into the dehydration tower (3) for circulation, and the tertiary raw material with qualified water content detection is directly transported from the temporary storage tank to subsequent processing equipment; S3: Input the tertiary raw material into an ion tank (5) to remove the metal ions contained therein, obtaining a quaternary raw material; S4: Input the quaternary raw material into a filtration and separation device (6) to remove the impurity particles present therein, obtaining an electronic grade isopropyl alcohol product; Wherein, the components with boiling points lower and higher than isopropyl alcohol in the S1 step are light components and heavy components in sequence; in the S1 step, the raw material isopropyl alcohol is subjected to light component removal and heavy component removal through a multi-stage distillation column; the ion tank (5) and the filtration and separation device (6) in the S3 and S4 steps are arranged in series in multiple stages; the ion tank (5) is filled with ion exchange resin; Wherein, the dehydration adsorption device includes a dehydration tower (3) and an auxiliary dehydrator (4), and the product outlet on the dehydration tower (3) is communicated with the auxiliary dehydrator (4); An upper partition plate (433) and a lower partition plate (422) are installed in the auxiliary dehydrator (4) from top to bottom. The upper partition plate (433) and the lower partition plate (422) divide the space in the auxiliary dehydrator (4) into a separation chamber (41), a heat exchange chamber (43), and a permeation chamber (42) from top to bottom. A heat preservation layer is installed outside the auxiliary dehydrator (4); A feed inlet (411) and a discharge outlet (413) are installed in the separation chamber (41), an input port (431) and an output port (432) are installed in the heat exchange chamber (43), and a permeate outlet (421) is installed in the permeation chamber (42); A fixing plate (414) is installed in the separation chamber (41). An osmotic evaporation membrane tube (44) is installed between the fixing plate (414) and the lower isolation plate (422). A heat pipe (46) is installed in the osmotic evaporation membrane tube (44). The upper end of the heat pipe (46) passes through the upper isolation plate (433) and is located in the heat exchange chamber (43). The heat pipe (46) is fixed by the upper isolation plate (433). The space between the fixing plate (414) and the upper isolation plate (433) is an air extraction chamber. An air extraction port (412) is installed in the air extraction chamber. The air extraction chamber and the osmotic chamber (42) are interconnected through the osmotic evaporation membrane tube (44). A retaining ring (464) is installed on the part of the heat pipe (46) located in the air extraction chamber).
2. The process for extracting electronic-grade isopropanol from industrial isopropanol according to claim 1, characterized in that: A limiting frame (462) is installed in the osmotic evaporation membrane tube (44), and the limiting frame (462) clamps and fixes the heat pipe (46); Hydrophobic coatings are provided on the surfaces of the heat pipe (46) and the limiting frame (462).
3. The process for extracting electronic-grade isopropanol from industrial isopropanol according to claim 2, characterized in that: A groove (461) is provided on the surface of the heat pipe (46), and a protrusion is provided on the limiting frame (462), and the protrusion and the groove (461) cooperate with each other; A deformation piece (463) is installed on the limiting frame (462), and the deformation piece (463) is a bimetallic piece.
4. The process for extracting electronic-grade isopropanol from industrial isopropanol according to claim 1, wherein: A vibrating plate (45) is installed in the separation chamber (41). A connecting rod (451) is installed on the vibrating plate (45), and the two ends of the connecting rod (451) are respectively connected to the fixing plate (414) and the lower isolation plate (422); Multiple groups of the vibrating plates (45) are arranged in the separation chamber (41). Each group of the vibrating plates (45) is composed of multiple units from top to bottom. The vibrating plate (45) is located close to the osmotic evaporation membrane tube (44).
5. The process for extracting electronic-grade isopropanol from industrial isopropanol according to claim 4, characterized in that: The connecting rod (451) is located at a position close to the middle on the vibrating plate (45), and the installation positions of the connecting rods (451) on each group of the vibrating plates (45) are different.
6. The process for extracting electronic-grade isopropanol from industrial isopropanol according to claim 4, wherein: An elastic tube sleeve (452) is installed on the connecting rod (451). The vibrating plates (45) on the connecting rod (451) are fixed by the elastic tube sleeve (452), and the vibrating plate (45) is slidably installed on the connecting rod (451).
7. The process for extracting electronic-grade isopropanol from industrial isopropanol according to claim 4, wherein: The vibrating plate (45) is provided with uniformly distributed through holes (453).
8. The process for extracting electronic-grade isopropanol from industrial isopropanol according to claim 4, characterized in that: Elastic wires are installed on the side surface of the vibrating plate (45), and the elastic wires contact the surface of the osmotic evaporation membrane tube (44).
Citation Information
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