Preparation device of high-purity electronic chemicals

Abstract

The utility model belongs to the technical field of preparation of electronic chemicals, and relates to high-purity electronic chemicals in the fields of semiconductors, display panels, solar energy, power batteries, medicines, chemical engineering and the like. The preparation device of the high-purity electronic chemicals comprises mixing equipment, filtering equipment, anion and cation removal equipment, separation equipment, crystallization equipment and drying equipment, the filtering equipment is selected from at least one of a micro-filter and a nano-filter, and the anion and cation removal equipment is selected from at least one of ion exchange resin and ion exchange fiber; the separation equipment is a dividing wall rectifying tower, the dividing wall rectifying tower is structurally selected from one of a middle dividing wall, an upper dividing wall and a lower dividing wall, and the area ratio of the two sides of the dividing wall rectifying tower ranges from 2: 8 to 8: 2; and the number of the separators is 1-3. The product is a high-purity electronic-grade chemical product with high purity and low impurity content, and can meet the requirements of the highest standard SEMIC12 (G4) of electronic chemicals and above.

Description

Technical Field

[0001] The utility model belongs to the technical field of the preparation of electronic chemicals, and relates to high-purity electronic chemicals in the fields of semiconductors, display panels, solar energy, power batteries, medicine, chemical engineering, etc. Specifically, the utility model relates to a preparation device for high-purity electronic-grade chemicals. Background Art

[0002] As an important type of electronic chemicals, high-purity and ultra-clean electronic chemicals have been widely used in the fields of power batteries, medicine, liquid crystal displays, semiconductor lithography, etc.

[0003] The main preparation processes adopted by domestic enterprises are complex distillation, adsorption distillation, vacuum distillation, and a combination of various coupling technologies. Chinese Patent Application Publication No. CN 109748931 A discloses a production system for high-purity tetraethyl orthosilicate, which includes a high-purity silicon tetrachloride storage tank; a high-purity ethanol storage tank; a reactive distillation column; the high-purity silicon tetrachloride storage tank and the high-purity ethanol storage tank are respectively connected to the reactive distillation column; a decolorization adsorber; an alkaline adsorber; a light component removal distillation column; a boron and phosphorus adsorber; a boron and phosphorus adsorbing resin is arranged in the boron and phosphorus adsorber; a metal ion adsorber; a metal ion adsorbing resin is arranged in the metal ion adsorber; a heavy component removal distillation column, as Figure 6 shown. The process adopted in this application, such as vacuum distillation and sub-boiling distillation, is complex, and the cost is high due to energy consumption and investment. Summary of the Utility Model

[0004] In view of the above problems, the utility model provides a preparation device for high-purity electronic chemicals. The preparation device of the utility model has a short processing flow, low energy consumption, and strong process continuity.

[0005] To achieve the above utility model purpose, the utility model provides the following technical solutions:

[0006] A preparation device for high-purity electronic chemicals, characterized in that it includes a mixing device, a filtering device, a cation and anion removal device, a separation device, a crystallization device, and a drying device. The filtering device is selected from at least one of a microfilter and a nanofiltration membrane. The cation and anion removal device is selected from one of an ion exchange resin and an ion exchange fiber. The separation device is a dividing wall distillation column. The structure of the dividing wall distillation column is selected from one of a middle dividing wall, an upper dividing wall, and a lower dividing wall. The area ratio range on both sides of the dividing wall distillation column is 2:8 to 8:2. The number of the separation devices is 1-3.

[0007] Furthermore, the number of condensers at the top of the dividing wall distillation column is one or more or not provided, and the number of reboilers at the bottom of the dividing wall distillation column is one or more or not provided.

[0008] Further, the preparation device of the high-purity electronic chemical includes a stirring and heating mixer, a microfilter, an anion and cation remover, a nanofiltration filter, a separator, a crystallizer and a dryer connected in series in sequence.

[0009] Further, the microfiltration membrane is selected from one of polytetrafluoroethylene membranes, polyethersulfone membranes, polyvinylidene fluoride membranes (PVDF), polyimide membranes and polyamide membranes with a pore size of 0.1 - 0.5 μm, and the pore size uniformity coefficient is 1.1 - 1.4;

[0010] The particle size of the ion exchange resin and / or ion exchange fiber is 0.3 - 0.6 mm, and it is one or several of sulfonic acid group styrene resins or fibers, carboxyl group styrene resins or fibers, quaternary amine group styrene resins or fibers, perfluorosulfonic acid resins or fibers, sulfonated polyethersulfone resins or fibers, and the pore size uniformity coefficient is 1.1 - 1.3;

[0011] The nanofiltration membrane is selected from one of polytetrafluoroethylene membranes, polyethersulfone membranes, polyvinylidene fluoride membranes (PVDF), polyimide membranes or polyamide membranes with a pore size of 10 - 50 nm, and the pore size uniformity coefficient is 1.1 - 1.4.

[0012] Further, the microfilter uses a polytetrafluoroethylene membrane with a pore size of 0.2 μm and a uniformity coefficient of 1.25; the microfilter uses a polyimide membrane with a pore size of 0.4 μm and a uniformity coefficient of 1.15;

[0013] The ion exchange resin uses a mixed resin of sulfonic acid group styrene and quaternary amine group styrene with a particle size of 0.6 mm and a uniformity coefficient of 1.1; the ion exchange resin uses a mixed resin of perfluorosulfonic acid and quaternary amine group styrene with a particle size of 0.3 mm and a uniformity coefficient of 1.3;

[0014] The nanofiltration filter uses a polytetrafluoroethylene membrane with a pore size of 20 nm and a uniformity coefficient of 1.2; the nanofiltration filter uses a polyimide membrane with a pore size of 10 nm and a uniformity coefficient of 1.25.

[0015] Further, the crystallization device is a falling film crystallizer, and the falling film crystallizer includes a cylinder body, and the upper head and the lower head provided at the upper end and the lower end of the cylinder body are the upper head and the lower head respectively; a material inlet and a tube side vent are provided at the top of the upper head, an upper tube sheet is provided at the upper part of the cylinder body, a lower tube sheet is provided at the lower end of the cylinder body, a shell is surrounded around the cylinder body, an overflow port, a heat transfer oil outlet and a heat transfer oil inlet are sequentially provided on the peripheral wall of the shell from top to bottom; a shell side vent is further provided on the shell, the shell side vent is located below the upper tube sheet, and the overflow port is located above the upper tube sheet.

[0016] Further, in the falling film crystallizer, a plurality of heat exchange tubes are fixedly arranged in the cavity of the cylinder body, and an upcomer is arranged in each of the heat exchange tubes. The upcomer is inserted into the heat exchange tube, and the upper parts of the upcomers in the cylinder body are of a communicating structure; a distributor is plugged at the inlet of the heat exchange tube, and the upper tube sheet is sleeved on the upper end of the heat exchange tube.

[0017] Further, in the falling film crystallizer, a baffle is arranged in the cavity of the cylinder body. The baffle is perpendicular to the heat exchange tube, and the baffle is of a hollow structure and is in a communicating structure with the shell; a crystal outlet is arranged at the bottom wall of the lower head.

[0018] Further, the crystallization device is a plate crystallizer, which includes a cylinder body, a cylinder cover plate arranged at the opening of the cylinder body, a jacket side plate surrounding the side of the cylinder body and a jacket bottom plate at the bottom of the cylinder body. It is characterized in that the cylinder body is divided into upper and lower parts. The upper part of the cylinder body is a liquid storage bin, and an upper end supplement is fixedly arranged in the cavity of the upper part of the cylinder body. The upper end of the upper end supplement is spherical.

[0019] A plurality of crystallization side plates are vertically arranged perpendicular to the bottom of the cylinder body in the cavity of the lower part of the cylinder body. The plurality of crystallization side plates are arranged in parallel and are of a solid structure; the crystallization side plates are communicated with the upper end supplement, and a crystallization cavity is formed between two of the crystallization side plates in the cavity.

[0020] Further, in the plate crystallizer, a feed inlet, a nitrogen inlet, a vent port, a thermometer interface and a pressure gauge interface are respectively arranged at the top of the cylinder body; the feed inlet and the vent port are located at the same opening, and the pressure gauge interface and the nitrogen inlet are located at the same opening.

[0021] A discharge port is arranged on the cylinder bottom plate of the cylinder body through the jacket bottom plate; the jacket side plate and the jacket bottom plate are both of a hollow structure and are communicated with each other; a first heat transfer oil inlet and a first heat transfer oil outlet are respectively arranged at the lower parts of the jacket side plates on the opposite sides; a second heat transfer oil inlet and a second heat transfer oil outlet are arranged on the jacket bottom plate.

[0022] The beneficial effect of the present invention is that the dividing wall distillation column adopted by the present invention can greatly reduce the number of conventional distillation columns. It can be reduced from the original 2 distillation columns to 1, from the original 4 distillation columns to 2, and from 6 conventional distillation columns to 3 dividing wall columns, thus greatly reducing energy consumption and investment and shortening the process. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of Embodiment 1 of the high-purity electronic chemical preparation device of the present invention;

[0024] Figure 2 Schematic diagram of Embodiment 2 of the high-purity electronic chemical preparation device of the present utility model;

[0025] Figure 3 Schematic diagram of Embodiment 3 of the high-purity electronic chemical preparation device of the present utility model;

[0026] Figure 4 Schematic diagram of Embodiment 4 of the high-purity electronic chemical preparation device of the present utility model;

[0027] Figure 5 These are several forms of the dividing wall column, A is the middle dividing wall, B is the upper dividing wall, and C is the lower dividing wall;

[0028] Figure 6 Schematic diagram of the production system of high-purity tetraethyl orthosilicate in the prior art;

[0029] Figure 7 Schematic diagram of a falling film crystallizer of the high-purity electronic chemical preparation device of the present utility model;

[0030] Figure 8 Cross-sectional view of a plate crystallizer of the high-purity electronic chemical preparation device of the present utility model;

[0031] Figure 9 Left view of a plate crystallizer of the high-purity electronic chemical preparation device of the present utility model.

[0032] Explanation of reference numerals:

[0033] 1 Industrial-grade electronic chemicals, 2 Solvent, 3 Stirring and heating mixer, 4 Electronic chemical solution, 5 Microfilter, 6 Microfiltered electronic chemicals, 7 Anion and cation remover, 8 Electronic chemicals after ion removal, 9 Primary separator, 10 Light components, 11 Heavy components, 12 Electronic chemicals after primary separation, 13 Nanofiltration membrane, 14 Electronic chemicals after nanofiltration, 15 Crystallizer, 17 Electronic chemical products after crystallization, 18 Dryer, 19 Electronic-grade electronic chemical products, 20 Secondary separator, 21 Electronic chemicals after secondary separation, 24 Tertiary separator

[0034] Falling film crystallizer cylinder body 30, upper head 31, lower head 32, tube side vent 33, material inlet 34, upper tube sheet 35, lower tube sheet 36, shell 37, overflow port 38, heat transfer oil outlet 39, heat transfer oil inlet 40, shell side vent 41, heat exchange tube 42, distributor 43, riser 44, baffle 45, crystal outlet 46

[0035] Plate crystallizer cylinder body 50, cylinder body cover plate 51, jacket side plate 52, jacket bottom plate 53, feed inlet 54, vent port 55, nitrogen inlet 56, pressure gauge interface 57, thermometer interface 58, crystallization side plate 59, crystallization cavity 60, first heat transfer oil inlet 61, first heat transfer oil outlet 62, cylinder body bottom plate 63, discharge outlet 64, second heat transfer oil inlet 65, second heat transfer oil outlet 66, upper end supplement 67

[0036] Figure 6 : V07 is a crude tetraethyl orthosilicate storage tank, P10 is a feed pump for the tetraethyl orthosilicate light - removal rectification column, S05 is an alkaline adsorber, T05 is a tetraethyl orthosilicate light - removal rectification column, E09 is a reboiler for the tetraethyl orthosilicate light - removal rectification column, E10 is a condenser for the tetraethyl orthosilicate light - removal rectification column, P11 is a discharge pump for the tetraethyl orthosilicate light - removal rectification column, S06 is a boron - phosphorus adsorber, S07 is a metal ion adsorber, T06 is a tetraethyl orthosilicate heavy - removal rectification column, E11 is a reboiler for the tetraethyl orthosilicate heavy - removal rectification column, E12 is a condenser for the tetraethyl orthosilicate heavy - removal rectification column, P12 is a discharge pump for the tetraethyl orthosilicate heavy - removal rectification column, V09 is a high - purity tetraethyl orthosilicate storage tank, V10 is a tetraethyl orthosilicate recovery tank Specific embodiments

[0037] The following embodiments further illustrate the content of the present utility model, but should not be construed as a limitation to the present utility model. Without departing from the spirit and essence of the present utility model, modifications or substitutions made to the methods, steps or conditions of the present utility model all fall within the scope of the present utility model.

[0038] Embodiment 1

[0039] As Figure 1 shown, the preparation device of the high - purity electronic chemical of the present utility model includes a stirring heating mixer 3, a micro - filter 5, an anion - cation remover 7, a nano - filter 13, a dividing - wall distillation column (primary separator 9), a crystallizer 15 and a dryer 18. The primary separator 9 adopts the structure of a dividing - wall distillation column. In this embodiment, the form of the dividing - wall distillation column is an intermediate structure or an upper - dividing - wall structure or a lower - dividing - wall structure. The outlet of the stirring heating mixer 3 is connected to the inlet of the micro - filter 5, the outlet of the micro - filter 5 is connected to the inlet of the anion - cation remover 7, the outlet of the anion - cation remover 7 is connected to the inlet of the nano - filter 13, the outlet of the nano - filter 13 is connected to the inlet of the dividing - wall distillation column, the outlet of the dividing - wall distillation column is connected to the inlet of the crystallizer 15, and the outlet of the crystallizer 15 is connected to the inlet of the dryer 18.

[0040] The industrial-grade electronic chemicals and solvents used in this utility model enter the stirring and heating mixer 3 to obtain an electronic chemical solution, which then enters the microfilter 5. Its function is to remove particles larger than 0.2 μm. The microfilter can use a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane PVDF, a polyimide membrane, a polyamide membrane, or other membranes with the same pore size ranging from 0.1 to 0.5 μm;

[0041] After microfiltration, it enters the anion and cation remover 7. Its function is to remove anions and cations in the electronic chemicals. The anion and cation remover can use ion exchange resins or ion exchange fibers. Among them, the ion exchange resin uses customized functional resins, and the ion exchange fiber uses customized functional fibers, including one or several of sulfonic acid group styrene resins or fibers, carboxyl group styrene resins or fibers, quaternary amine group styrene resins or fibers, perfluorosulfonic acid resins or fibers, and sulfonated polyethersulfone resins or fibers;

[0042] After removing anions and cations, the electronic chemical solution enters the nanofiltration membrane 13. Its function is to filter out particles larger than 10 nm. The membrane of the nanofiltration membrane 13 can be a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane PVDF, a polyimide membrane, a polyamide membrane, or other membranes with the same pore size ranging from 10 to 50 nm;

[0043] The nanofiltrated electronic chemical solution enters the first-stage separator 9. The number of separators can be increased by 0 - 6 according to the requirements of raw materials and product standards. In this embodiment, the area ratio range of the two sides of the dividing-wall distillation column in the first-stage separator 9 is 2:8 to 8:2. Its forms mainly include middle dividing wall, upper dividing wall, and lower dividing wall, but are not limited to the above three; The electronic chemicals obtained from the separator enter the crystallizer 15. After crystallization, the product 17 passes through the dryer 18 to obtain the high-purity electronic chemical product.

[0044] The raw material of the electronic chemicals in this utility model is industrial-grade electronic chemicals. The mass content of the electronic chemicals is above 98%, the water content is above 500 ppm, the metal ions are above 500 ppt, the anions are above 500 ppb, (greater than 0.2 μm (micrometers)), and the particulate matter is greater than 1000 pieces / mL.

[0045] Example 2

[0046] As Figure 2 shown, the preparation device of the high-purity electronic chemicals of this utility model includes a mixer, a microfilter, an anion and cation remover, a nanofiltration membrane, and a dividing-wall distillation column. The form of the dividing-wall distillation column is the upper dividing wall B type, with two condensers and one reboiler. The outlet of the mixer is connected to the inlet of the microfilter, the outlet of the microfilter is connected to the inlet of the anion and cation remover, the outlet of the anion and cation remover is connected to the inlet of the nanofiltration membrane, and the outlet of the nanofiltration membrane is connected to the inlet of the dividing-wall distillation column.

[0047] The solvent water and the electronic chemical enter the stirring mixer 3 and then enter the microfilter. The microfilter uses a polyvinylidene fluoride (PVDF) membrane with a pore size of 0.5 μm and a uniformity coefficient of 1.1; the ion exchange resin uses a mixed resin of carboxystyrene and primary amine styrene with a particle size of 0.4 mm and a uniformity coefficient of 1.25; the nanofiltration membrane uses a polytetrafluoroethylene membrane with a pore size of 10 nm and a uniformity coefficient of 1.4; the separator 9 adopts the form of a dividing wall column type B, with a side area ratio of 5:5 and 30 theoretical plates.

[0048] Example 3

[0049] As Figure 3 shown, the preparation device of the high-purity electronic chemical of the present utility model includes a mixer, a microfilter, an anion and cation remover, a nanofiltration membrane, a dividing wall rectification column, a crystallizer and a dryer. The form of the dividing wall rectification column is the intermediate dividing wall type A, with one condenser and one reboiler. The outlet of the mixer is connected to the inlet of the microfilter, the outlet of the microfilter is connected to the inlet of the anion and cation remover, the outlet of the anion and cation remover is connected to the inlet of the nanofiltration membrane, the outlet of the nanofiltration membrane is connected to the inlet of the dividing wall rectification column, the outlet of the dividing wall rectification column is connected to the inlet of the crystallizer, and the outlet of the crystallizer is connected to the inlet of the dryer.

[0050] The solvent ethyl acetate and the electronic chemical enter the stirring mixer 3 and then enter the microfilter. The microfilter uses a polyamide membrane with a pore size of 0.2 μm and a uniformity coefficient of 1.35; the ion exchange resin uses a mixed resin of sulfonic acid styrene resin and quaternary amine styrene with a particle size of 0.5 mm and a uniformity coefficient of 1.12, and the volume ratio of sulfonic acid styrene resin to quaternary amine styrene is 3:1; the nanofiltration membrane 13 uses a polyvinylidene fluoride (PVDF) membrane with a pore size of 30 nm and a uniformity coefficient of 1.1; the separator 9 adopts the form of a dividing wall column type A, with a side area ratio of 6:4 and 18 theoretical plates; the crystallizer 15 uses a 1-stage falling film crystallizer.

[0051] Example 4

[0052] As Figure 4As shown in the figure, the preparation device for high-purity electronic chemicals of the present utility model includes a mixer, a microfilter, an anion-cation remover, a nanofiltration membrane, and a separator. Three dividing-wall distillation columns are used. The first dividing-wall distillation column adopts a C-type lower dividing wall, one condenser, two reboilers, one condenser, and one reboiler. The second dividing-wall distillation column adopts an A-type middle dividing wall, and the third dividing-wall column adopts a B-type upper dividing wall, with two condensers and one reboiler. The outlet of the mixer is connected to the inlet of the microfilter, the outlet of the microfilter is connected to the inlet of the anion-cation remover, the outlet of the anion-cation remover is connected to the inlet of the nanofiltration membrane, the outlet of the nanofiltration membrane is connected to the inlet of the first dividing-wall distillation column, the outlet of the first dividing-wall distillation column is connected to the inlet of the second dividing-wall distillation column, and the outlet of the second dividing-wall distillation column is connected to the inlet of the third dividing-wall distillation column.

[0053] Solvent water and electronic chemicals enter the stirring mixer 3 and then enter the microfilter. The microfilter uses a polyvinylidene fluoride (PVDF) membrane with a pore size of 0.5 μm and a uniformity coefficient of 1.1; the ion exchange resin has a particle size of 0.4 mm, a uniformity coefficient of 1.25, and is a mixed resin of carboxystyrene and primary amino styrene; the nanofiltration membrane uses a polytetrafluoroethylene membrane with a pore size of 10 nm and a uniformity coefficient of 1.4; the separator 9 adopts a C-type dividing-wall column, with a side area ratio of 4:6 and 18 theoretical plates; the separator 20 adopts an A-type dividing-wall column, with a side area ratio of 5:5 and 12 theoretical plates; the separator 24 adopts a B-type dividing-wall column, with a side area ratio of 6:4 and 10 theoretical plates.

[0054] In the preparation device, the crystallization device is a falling-film crystallizer. The falling-film crystallizer includes a cylinder body 30, and the upper and lower end heads provided at the upper and lower ends of the cylinder body 30 are an upper end head 31 and a lower end head 32 respectively; a material inlet 34 and a tube-side vent are provided at the top of the upper end head 31, an upper tube sheet 35 is provided at the upper part of the cylinder body 30, a lower tube sheet 36 is provided at the lower end of the cylinder body, a shell 37 is provided around the cylinder body 30, and an overflow port 38, a heat transfer oil outlet 39, and a heat transfer oil inlet 40 are sequentially provided on the peripheral wall of the shell 37 from top to bottom; a shell-side vent 41 is further provided on the shell 30, the shell-side vent 41 is located below the upper tube sheet 35, and the overflow port 38 is located above the upper tube sheet 35.

[0055] In the falling-film crystallizer, a plurality of heat exchange tubes 42 are fixedly provided in the cavity of the cylinder body 30, and an upcomer 44 is provided in each of the heat exchange tubes 42. The upcomer 44 is inserted into the heat exchange tube 42, and the upper parts of the upcomers 44 in the cylinder body 30 are in a communicating structure; a distributor 43 is plugged at the inlet of the heat exchange tube 42, and the upper tube sheet 35 is sleeved on the upper end of the heat exchange tube 42.

[0056] In the falling film crystallizer, a baffle plate 45 is arranged in the cavity of the cylinder body 30. The baffle plate 45 is vertically arranged with respect to the heat exchange tube 42. The baffle plate 45 is of a hollow structure and is a communicating structure with the shell 37. A crystal outlet 46 is arranged on the bottom wall part of the lower head.

[0057] In the preparation device, in combination Figures 7 to 9 As shown, the crystallization device is a plate - type crystallizer. The plate - type crystallizer includes a cylinder body 50, a cylinder body cover plate 51 arranged at the opening of the cylinder body 50, a jacket side plate 52 surrounding the side part of the cylinder body and a jacket bottom plate 53 at the bottom of the cylinder body. The cylinder body 50 is divided into upper and lower parts. The upper part of the cylinder body 50 is a liquid storage bin. An upper end supplement 67 is fixedly arranged in the upper cavity of the cylinder body 50. The upper end part of the upper end supplement 67 is spherical.

[0058] In the lower cavity of the cylinder body 50, a plurality of crystallization side plates 59 are vertically arranged with respect to the bottom of the cylinder body 50. The plurality of crystallization side plates 59 are arranged in parallel and are of solid structures. The crystallization side plates 59 are communicated with the upper end supplement 67. A crystallization cavity 60 is formed between two of the crystallization side plates 59 located in the cavity.

[0059] In the plate - type crystallizer, a feed inlet 54, a nitrogen inlet 56, a vent outlet 55, a thermometer interface 58 and a pressure gauge interface 57 are respectively arranged at the top of the cylinder body 50. The feed inlet 54 and the vent outlet 55 are located at the same opening. The pressure gauge interface 57 and the nitrogen inlet 56 are located at the same opening.

[0060] An outlet 64 is arranged on the cylinder body bottom plate 63 of the cylinder body 50 and passes through the jacket bottom plate 53. The jacket side plate 52 and the jacket bottom plate 53 are both of hollow structures and are communicated with each other. A first heat - conducting oil inlet 61 and a first heat - conducting oil outlet 62 are respectively arranged at the lower parts of the jacket side plates 52 on the opposite sides. The jacket bottom plate is provided with a second heat - conducting oil inlet 65 and a second heat - conducting oil outlet 66.

[0061] In summary, the preparation equipment of the present utility model can be used for the purification of high - purity electronic chemicals such as catechol, resorcinol and hydroquinone. The dividing - wall distillation column adopted by the present utility model can greatly reduce the number of conventional distillation columns. It can be reduced from the original 2 distillation columns to 1, from the original 4 distillation columns to 2, and from 6 conventional distillation columns to 3 dividing - wall columns, thus greatly reducing energy consumption and investment and shortening the process.

[0062] Although the present utility model has been described in detail above with general descriptions, specific embodiments and experiments, some modifications or improvements can be made to it based on the present utility model, which are obvious to those skilled in the art. Therefore, these modifications or improvements made without departing from the spirit of the present utility model all fall within the scope of protection required by the present utility model.

Claims

1. A preparation device for high-purity electronic chemicals, characterized in that, it includes a mixing device, a filtering device, an anion and cation removal device, a separation device, a crystallization device and a drying device. The filtering device is selected from at least one of a microfilter and a nanofiltration membrane. The anion and cation removal device is selected from one of ion exchange resins and ion exchange fibers. The separation device is a dividing-wall distillation column. The structure of the dividing-wall distillation column is selected from one of a middle dividing wall, an upper dividing wall and a lower dividing wall. The area ratio range on both sides of the dividing-wall distillation column is 2:8 to 8:

2. The number of the separation devices is 1-3. The crystallization device is a falling-film crystallizer. The falling-film crystallizer includes a cylinder body, and the upper end head and the lower end head arranged at the upper end and the lower end of the cylinder body are respectively an upper end head and a lower end head. A material inlet and a tube-side vent are arranged at the top of the upper end head. An upper tube sheet is arranged at the upper part of the cylinder body. A lower tube sheet is arranged at the lower end of the cylinder body. A shell is surrounded around the cylinder body. An overflow port, a heat transfer oil outlet and a heat transfer oil inlet are sequentially arranged on the peripheral wall of the shell from top to bottom. The shell is also provided with a shell-side vent, and the shell-side vent is located below the upper tube sheet, and the overflow port is located above the upper tube sheet.

2. The preparation device according to claim 1, characterized in that, a plurality of heat exchange tubes are fixedly arranged in the cavity of the cylinder body, and an upcomer is arranged in each of the heat exchange tubes. The upcomer is inserted into the heat exchange tube, and the upper parts of the upcomers in the cylinder body are in a communicating structure. A distributor is plugged at the inlet of the heat exchange tube, and the upper tube sheet is sleeved on the upper end of the heat exchange tube.

3. The preparation device according to claim 2, characterized in that, a baffle plate is arranged in the cavity of the cylinder body. The baffle plate is perpendicular to the heat exchange tubes. The baffle plate is of a hollow structure and is in a communicating structure with the shell. A crystal outlet is arranged on the bottom wall of the lower end head.

4. The preparation device according to claim 1, characterized in that, the crystallization device is a plate crystallizer. The plate crystallizer includes a cylinder body, a cylinder cover arranged at the opening of the cylinder body, a jacket side plate surrounded on the side of the cylinder body and a jacket bottom plate at the bottom of the cylinder body. The cylinder body is divided into upper and lower parts. The upper part of the cylinder body is a liquid storage bin. An upper end supplement is fixedly arranged in the cavity of the upper part of the cylinder body, and the upper end of the upper end supplement is spherical. A plurality of crystallization side plates are vertically arranged perpendicular to the bottom of the cylinder body in the cavity of the lower part of the cylinder body. The plurality of crystallization side plates are arranged in parallel and are of a solid structure. The crystallization side plates are communicated with the upper end supplement, and a crystallization cavity is formed between two of the crystallization side plates in the cavity.

5. The preparation device according to claim 4, characterized in that, a feed inlet, a nitrogen inlet, a vent, a thermometer interface and a pressure gauge interface are respectively arranged at the top of the cylinder body. The feed inlet and the vent are located at the same opening. The pressure gauge interface and the nitrogen inlet are located at the same opening. An outlet is provided on the bottom plate of the cylinder body and passes through the bottom plate of the jacket; both the side plates and the bottom plate of the jacket are hollow structures and are interconnected; a first heat transfer oil inlet and a first heat transfer oil outlet are respectively provided at the lower parts of the jacket side plates on the opposite sides; a second heat transfer oil inlet and a second heat transfer oil outlet are provided on the bottom plate of the jacket.

6. The preparation device according to claim 1, characterized in that the number of condensers at the top of the dividing wall distillation column is one or more or not provided, and the number of reboilers at the bottom of the dividing wall distillation column is one or more or not provided.

7. The preparation device according to claim 2, characterized in that the preparation device for high-purity electronic chemicals includes a stirring and heating mixer, a microfilter, an anion and cation remover, a nanofiltration membrane, a separator, a crystallizer and a dryer connected in series in sequence.

8. The preparation device according to claim 1, characterized in that the microfilter is selected from one of a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane (PVDF), a polyimide membrane and a polyamide membrane with a pore size of 0.1-0.5 μm, and the pore size uniformity coefficient is 1.1-1.4; the particle size of the ion exchange resin and / or ion exchange fiber is 0.3-0.6 mm, and it is one of a sulfonic acid group styrene resin or fiber, a carboxyl group styrene resin or fiber, a quaternary amine group styrene resin or fiber, a perfluorosulfonic acid resin or fiber, a sulfonated polyethersulfone resin or fiber, and the pore size uniformity coefficient is 1.1-1.3; the nanofiltration membrane is selected from one of a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane (PVDF), a polyimide membrane or a polyamide membrane with a pore size of 10-50 nm, and the pore size uniformity coefficient is 1.1-1.

4.

9. The preparation device according to claim 4, characterized in that the microfilter uses a polytetrafluoroethylene membrane with a pore size of 0.2 μm and a uniformity coefficient of 1.25; the microfilter uses a polyimide membrane with a pore size of 0.4 μm and a uniformity coefficient of 1.15; the ion exchange resin uses a mixed resin of sulfonic acid group styrene and quaternary amine group styrene with a particle size of 0.6 mm and a uniformity coefficient of 1.1; the ion exchange resin uses a mixed resin of perfluorosulfonic acid and quaternary amine group styrene with a particle size of 0.3 mm and a uniformity coefficient of 1.3; the nanofiltration membrane uses a polytetrafluoroethylene membrane with a pore size of 20 nm and a uniformity coefficient of 1.2; the nanofiltration membrane uses a polyimide membrane with a pore size of 10 nm and a uniformity coefficient of 1.25.

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