Fin-type plate-type static melt crystallizer
By designing a finned plate static melt crystallizer, the crystallization plates are inclined and have guide grooves and concave bubbling on the plate surface, which solves the problems of crystal shedding and mother liquor residue, and improves product purity and yield.
Patent Information
- Application Number
- CN202422566299.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-23
- Publication Date
- 2026-01-27
- Estimated Expiration
- 2034-10-23
AI Technical Summary
In existing plate crystallizers, crystals easily detach from the crystallization plate, hindering the discharge of mother liquor and affecting product purity.
A finned plate static melt crystallizer is adopted, with the crystallization plates distributed at an angle and the plates having guide grooves and concave bubbling on the surface to improve crystal adhesion and mother liquor discharge efficiency.
It effectively alleviates the problem of crystal shedding, improves the efficiency of mother liquor discharge, and enhances product purity.
Smart Images
Figure CN223831826U_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of crystal melting and crystallization equipment technology, and in particular to a finned plate static melting and crystallization apparatus. Background Technology
[0002] Crystallization is a fundamental unit operation in chemical engineering, with applications in many technological fields, such as organic purification and pharmaceutical preparation. Depending on the specific crystallization process, it can be divided into solution crystallization and melt crystallization. Melt crystallization, in particular, requires no additional solvent, has low energy consumption, and uses simple equipment, making it highly advantageous for separating easily polymerized systems. With the development of crystallization technology, melt crystallization has demonstrated significant superiority in separating and extracting organic compounds, and plate crystallizers are a typical device for realizing static melt crystallization technology.
[0003] In existing plate crystallizers, the crystallization plates are vertically distributed in the internal structure and the surface of the crystallization plates is smooth. During crystallization, due to the influence of gravity, a large number of crystals will fall off the crystallization plates, which will seriously affect the effect. At the same time, the mother liquor cannot be discharged smoothly during the crystallization "sweating" process, which will affect the purity of the final product. Summary of the Invention
[0004] To address the shortcomings of the existing technology, this invention provides a finned plate static melt crystallizer, comprising:
[0005] A multi-layered crystallizing glass reactor shell is provided with a reactor lid on top, and the reactor lid is provided with an inlet and outlet for an internal circulating medium.
[0006] The crystallization plate assembly is integrated with the vessel lid through the internal circulation medium inlet and outlet, and the crystallization plate assembly is distributed at a certain angle inside the multi-layer crystallization glass vessel shell;
[0007] The crystallization plate assembly includes multiple crystallization plates, and the surface of each crystallization plate is provided with a flow guide groove and a bubble.
[0008] In some embodiments, the crystallization plate group includes multiple crystallization plates, the crystallization plates are hollow inside, and their distribution is either cross or parallel. The crystallization plates are inclined at an angle of 0-90° inside the multilayer crystallization glass reactor shell.
[0009] In some embodiments, the guide channels are alternately distributed between the bubbles; the crystallization plate group is at a certain distance from the multilayer crystallization glass reactor shell and is uniform.
[0010] In some embodiments, the guide channels are obliquely distributed on the crystallizing plate, with both ends of the guide channels connected to the outer ends of the crystallizing plate, and the guide channels are arranged in parallel with equal spacing, and the distribution of the guide channels is either cross-distribution or parallel distribution.
[0011] In some embodiments, the guide groove is cylindrical, conical, or rectangular in shape.
[0012] In some embodiments, the bubbles are formed by concave bubbling on the surface of the crystallizing plate, and the bubbles are arranged in triangular, square, and circular patterns, with equal spacing and parallel distribution on the crystallizing plate.
[0013] In some embodiments, the bubble is circular, square, or triangular.
[0014] In some embodiments, the multilayer crystallizing glass reactor shell includes three layers: an inner layer, a middle layer, and an outer layer. The reactor lid is also provided with a thermocouple temperature sensor inlet and a raw material inlet. A discharge port is provided at the bottom of the crystallizing glass reactor shell, and the discharge port can be opened and closed by a screw button.
[0015] In some embodiments, the multilayer crystallizing glass reactor shell is provided with an external circulation medium outlet and an external circulation medium inlet on both sides, respectively, for the intermediate layer.
[0016] In some embodiments, the vessel lid and the multilayer crystallized glass vessel shell are fixed together by metal clamps and sealing rings.
[0017] The finned plate static melt crystallizer provided by this invention optimizes existing traditional plate crystallizers. It optimizes the traditional vertical clean plate to alleviate the problem of crystals falling off the crystallization plate and not easily adhering. By setting guide grooves on the plate surface, the efficiency of mother liquor discharge is improved, overcoming the problem of mother liquor residue affecting the purity of the final product. By performing concave bubbling treatment on the plate surface, the ability of crystals to adhere to the plate surface is improved. Attached Figure Description
[0018] Figure 1 This is a schematic diagram of the structure of the finned plate static melting crystallizer shown in the embodiment of this utility model. Figure 1 ;
[0019] Figure 2 This is a schematic diagram of the structure of the finned plate static melting crystallizer shown in the embodiment of this utility model. Figure 2 ;
[0020] Figure 3 This is a schematic diagram of the crystallization plate structure shown in an embodiment of the present invention;
[0021] In the attached figures, the following labels are used:
[0022] 1-Thermocouple temperature sensor inlet;
[0023] 2-Internal circulation medium inlet and outlet;
[0024] 3. Imported raw materials;
[0025] 4-External circulating medium outlet;
[0026] 5-Multi-layer crystallization glass reactor shell;
[0027] 6-External circulation medium inlet;
[0028] 7-Discharge port;
[0029] 8-Spiral button;
[0030] 9-Vertical angle of the crystallizing plate;
[0031] 10-Crystallization plate;
[0032] 11-Guide channel;
[0033] 12-Bubbling. Detailed Implementation
[0034] The technical solution of the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments to further understand the purpose, solution and effect of the present invention, but it is not intended to limit the scope of protection of the appended claims.
[0035] Certain terms are used in this specification and the following claims to refer to specific components or parts. Those skilled in the art will understand that users or manufacturers may use different names or terms to refer to the same component or part. This specification and the following claims do not distinguish components or parts by differences in name, but rather by differences in function. The terms "comprising" and "including" used throughout this specification and the following claims are open-ended and should be interpreted as "including but not limited to". Furthermore, the term "connection" here includes any direct and indirect electrical connection means. Indirect electrical connection means include connections made through other means.
[0036] It should be noted that in the description of this invention, the terms "lateral", "longitudinal", "up", "down", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and "about", or "approximately", "substantially", "left and right", etc., indicating the orientation or positional relationship or parameters, are all based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, a specific size, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.
[0037] See Figure 1-3 This utility model provides a finned plate static melting crystallizer, characterized by: a multi-layer crystallizing glass vessel shell 5, with a vessel lid installed on top, the vessel lid having an internal circulation medium inlet / outlet 2 for introducing the device's refrigerant / heat medium; a crystallizing plate assembly, the crystallizing plate assembly being integrally formed with the vessel lid via the internal circulation medium inlet / outlet 2, for example, it can be connected by a manifold, the crystallizing plate assembly being inclined at a certain angle inside the multi-layer crystallizing glass vessel shell 5; wherein, the crystallizing plate assembly includes multiple crystallizing plates 10, the surface of the crystallizing plates 10 having a guide groove 11 and bubbling.
[0038] In this embodiment, the crystallization plate group includes multiple crystallization plates 10, preferably 2-4 groups. The crystallization plates 10 are hollow inside and are distributed in a cross or parallel manner, preferably symmetrically cross-distributed at equal intervals. The crystallization plates 10 are inclined at an angle of 0-90° inside the multilayer crystallization glass reactor shell 5, preferably 30-60°.
[0039] In this embodiment, the guide channels 11 are alternately distributed between the bubbles; the crystallization plate group is at a certain distance from the multilayer crystallization glass reactor shell 5 and is uniform.
[0040] The guide grooves 11 are inclinedly distributed on the crystallizing plate 10, and the two ends of the guide grooves 11 are respectively connected to the outer end of the crystallizing plate 10. The guide grooves 11 are arranged in parallel with equal spacing, and the distribution mode of the guide grooves 11 is either cross-distribution or parallel distribution, preferably parallel distribution. The shape of the guide grooves 11 is cylindrical, conical and rectangular, preferably cylindrical.
[0041] In this embodiment, the bubbling is achieved by performing a concave bubbling process on the surface of the crystallizing plate 10. The bubbles are arranged in a triangular, square, or circular pattern, preferably in a square pattern. The bubbles are evenly spaced and parallel on the crystallizing plate 10. The bubbles are circular, square, or triangular, preferably circular. The number of bubbles is 4-12, preferably 6-8.
[0042] In this embodiment, the multilayer crystallizing glass reactor shell 5 comprises three layers: an inner layer, a middle layer, and an outer layer. The innermost layer contains the raw material, the middle layer can be circulated with different hot and cold media for cooling or heating, and the outermost layer is filled with air for insulation. The reactor lid is also equipped with a thermocouple temperature sensor inlet 1 and a raw material inlet 3. The bottom of the crystallizing glass reactor shell is provided with a discharge port 7, which can be opened and closed by a screw button 8 to control the flow rate of the mother liquor. The multilayer crystallizing glass reactor shell 5 is provided with an external circulation medium outlet 4 and an external circulation medium inlet 6 on both sides, respectively, for the middle layer. In this embodiment, each inlet and outlet can be sealed with a glass plug.
[0043] The vessel lid and the multi-layer crystallized glass vessel shell 5 are fixed together by a metal clamp and a sealing ring. The metal clamp is fixed by a screw clamp and can be flexibly disassembled.
[0044] In summary, the finned plate static melting crystallizer provided in this embodiment uses a three-layer glass crystallizer, a lid, a crystallization plate 10, raw material inlet / outlet, and a circulating medium inlet / outlet, all made of transparent glass. The crystallization plate 10 undergoes concave bubbling treatment, and guide grooves 11 are provided on the crystallization plate 10, which are alternately distributed between the bubbles. The crystallization plate 10 is distributed in the three-layer crystallizer with a vertical angle 9 of 0-90°, integrated with the lid, and is evenly spaced from the four walls of the crystallizer. The lid and the three-layer crystallizer are fixed by metal clamps and sealing rings. A dual circulation system is adopted, with the internal circulation connected to the crystallization plate 10 through the circulating medium inlet / outlet on the lid, and the external circulation located in the middle layer of the three-layer glass crystallizer. The raw material liquid enters the vessel from the inlet on the lid and is discharged through the outlet 7 at the bottom of the three-layer glass crystallizer using a spiral button 8. When the three-layer glass crystallizer is undergoing cooling or heating circulation, an insulation sleeve, such as insulation cotton, is used to wrap it to avoid the influence of external temperature.
[0045] The crystallizing plates are distributed at an angle inside the crystallizer, which can effectively alleviate the problem of a large number of crystals falling off the plates due to gravity. The plates are provided with guide grooves, which can effectively alleviate the problem of mother liquor remaining on the plates due to the plate tilt, and enhance the mother liquor discharge efficiency. The plates are treated with concave bubbling, and different arrangement methods can effectively improve the ability of crystals to adhere to the plates.
[0046] The purpose of this invention is to optimize existing traditional plate crystallizers and provide a finned plate static melt crystallizer. This invention optimizes the traditional vertical crystallization plate to alleviate the problem of crystals falling off the crystallization plate. By setting guide grooves on the plate surface, the efficiency of mother liquor discharge is improved. By performing concave bubbling treatment on the plate surface, the ability of crystals to adhere to the plate surface is improved.
[0047] Furthermore, as can be seen from the following detailed embodiments, the finned plate static melt crystallizer provided by this utility model has even more superior technical effects.
[0048] Example 1
[0049] This embodiment uses, as follows: Figures 1 to 3 The finned plate static melting crystallizer design shown has an inner diameter of 252mm and a height of 334mm. The crystallization plate has a vertical angle of 45°, a length of 160mm, a width of 84mm, and a thickness of 12mm. The distance between the crystallization plate and the outer wall of the three-layer glass crystallizer is 34mm. The distance between two sets of crystallization plates is 8mm. The distance between the bottom of the crystallization plate and the sand core of the crystallizer is 20mm. The distance between the top of the crystallization plate and the top port of the three-layer glass crystallizer is 62mm. The width of the guide groove on the crystallization plate is 4mm, and the distance between the guide grooves is 40mm. The diameter of the bubble 12 is 12mm, and the distance between the bubble 12 is 45mm. The entire crystallizer, including the crystallization vessel, crystallization plate, and crystallization vessel cover, is made of high borosilicate material.
[0050] The experimental system used in this embodiment was a mixture of mesitylene, wherein the purity of mesitylene was 76.08%, the purity of pseudotetramethylbenzene was 8.231%, and the purity of methyltetramethylbenzene was 3.985%. The system pressure was atmospheric pressure, the starting temperature of cooling was 80°C, the cooling rate was 0.05°C / min, the final crystallization temperature was 75°C, the heating rate was 0.05°C / min, and the final sweating temperature was 78.5°C. Under the operating conditions of this embodiment, the final product had a mesitylene yield of 72.38% and a purity of 96.24%.
[0051] Example 2
[0052] This embodiment uses a crystallizer design with the same dimensions as Embodiment 1, but the vertical angle of the crystallization plate is 30°, that is, the inner diameter of the crystallization vessel shell is 252mm, the height is 334mm, the length of the crystallization plate is 160mm, the width is 84mm, the thickness is 12mm, the distance between the crystallization plate and the outer wall of the three-layer glass crystallization vessel is 34mm, the distance between the two sets of crystallization plates is 8mm, the distance between the bottom end of the crystallization plate and the sand core of the crystallization vessel is 20mm, the distance between the top end of the crystallization plate and the top port of the three-layer glass crystallization vessel is 62mm, the width of the guide groove on the crystallization plate is 4mm, the diameter of the bubble 12 is 12mm, and the entire crystallizer, including the crystallization vessel, crystallization plate, and crystallization vessel cover, is made of high borosilicate material.
[0053] The experimental system used in this embodiment was the same mesitylene mixture and operating parameters as in Example 1, namely, mesitylene purity of 76.08%, metatetramethylbenzene purity of 8.231%, and methyltetramethylbenzene purity of 3.985%. The system pressure was atmospheric pressure, the starting temperature for cooling was 80°C, the cooling rate was 0.05°C / min, the final crystallization temperature was 75°C, the heating rate was 0.05°C / min, and the final sweating temperature was 78.5°C. Under the operating conditions of this embodiment, the final product had a mesitylene yield of 68.38% and a purity of 99.07%.
[0054] Example 3
[0055] This embodiment uses a crystallizer design with the same dimensions as Embodiment 1, but the vertical angle of the crystallizing plate is 60°, that is, the inner diameter of the crystallizing vessel shell is 252mm, the height is 334mm, the length of the crystallizing plate is 160mm, the width is 84mm, the thickness is 12mm, the distance between the crystallizing plate and the outer wall of the three-layer glass crystallizing vessel is 34mm, the distance between the two sets of crystallizing plates is 8mm, the distance between the bottom of the crystallizing plate and the sand core of the crystallizing vessel is 20mm, the distance between the top of the crystallizing plate and the top port of the three-layer glass crystallizing vessel is 62mm, the width of the guide groove on the crystallizing plate is 4mm, the diameter of the bubble 12 is 12mm, and the entire crystallizer, including the crystallizing vessel, crystallizing plate, and crystallizing vessel cover, is made of high borosilicate material.
[0056] The experimental system used in this embodiment was the same mesitylene mixture and operating parameters as in Example 1, namely, mesitylene purity of 76.08%, metatetramethylbenzene purity of 8.231%, and methyltetramethylbenzene purity of 3.985%. The system pressure was atmospheric pressure, the starting temperature for cooling was 80°C, the cooling rate was 0.05°C / min, the final crystallization temperature was 75°C, the heating rate was 0.05°C / min, and the final sweating temperature was 78.5°C. Under the operating conditions of this embodiment, the final product had a mesitylene yield of 77.09% and a purity of 92.86%.
[0057] Comparative Example 1
[0058] This embodiment uses the same crystallizer design as Embodiment 1, but the crystallizer plate does not have an inward bubbling treatment. That is, the inner diameter of the crystallizer shell is 252mm, the height is 334mm, the vertical angle of the crystallizer plate is 45°, the length is 160mm, the width is 84mm, the thickness is 12mm, the distance between the crystallizer plate and the outer wall of the three-layer glass crystallizer is 34mm, the distance between the two sets of crystallizer plates is 8mm, the distance between the bottom of the crystallizer plate and the sand core of the crystallizer is 20mm, the distance between the top of the crystallizer plate and the top port of the three-layer glass crystallizer is 62mm, the width of the guide groove on the crystallizer plate is 4mm, and the diameter of the bubbling is 12mm. The entire crystallizer, including the crystallizer, crystallizer plate, and crystallizer lid, is made of high borosilicate material.
[0059] The experimental system used in this embodiment was the same mesitylene mixture and operating parameters as in Example 1, namely, mesitylene purity of 76.08%, metatetramethylbenzene purity of 8.231%, and methyltetramethylbenzene purity of 3.985%. The system pressure was atmospheric pressure, the starting temperature for cooling was 80°C, the cooling rate was 0.05°C / min, the final crystallization temperature was 75°C, the heating rate was 0.05°C / min, and the final sweating temperature was 78.5°C. Under the operating conditions of this embodiment, the final product had a mesitylene yield of 65.77% and a purity of 95.16%.
[0060] Comparative Example 2
[0061] This embodiment uses the same crystallizer design as Embodiment 1, but the crystallization plate is not treated with a guide groove. That is, the inner diameter of the crystallization vessel shell is 252mm, the height is 334mm, the vertical angle of the crystallization plate is 45°, the length is 160mm, the width is 84mm, the thickness is 12mm, the distance between the crystallization plate and the outer wall of the three-layer glass crystallization vessel is 34mm, the distance between the two sets of crystallization plates is 8mm, the distance between the bottom end of the crystallization plate and the sand core of the crystallization vessel is 20mm, the distance between the top end of the crystallization plate and the top port of the three-layer glass crystallization vessel is 62mm, the width of the guide groove on the crystallization plate is 4mm, and the diameter of the bubble is 12mm. The entire crystallizer, including the crystallization vessel, the crystallization plate, and the crystallization vessel cover, is made of high borosilicate material.
[0062] The experimental system used in this embodiment was the same mesitylene mixture and operating parameters as in Example 1, namely, mesitylene purity of 76.08%, metatetramethylbenzene purity of 8.231%, and methyltetramethylbenzene purity of 3.985%. The system pressure was atmospheric pressure, the starting temperature for cooling was 80°C, the cooling rate was 0.05°C / min, the final crystallization temperature was 75°C, the heating rate was 0.05°C / min, and the final sweating temperature was 78.5°C. Under the operating conditions of this embodiment, the final product had a mesitylene yield of 74.03% and a purity of 91.04%.
[0063] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any other way. Any person skilled in the art may make changes or modifications to the above-disclosed technical content to create equivalent embodiments for application in other fields. However, any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the protection scope of the present invention.
Claims
1. A finned plate static melting crystallizer, characterized in that: include: A multi-layered crystallizing glass reactor shell is provided with a reactor lid on top, and the reactor lid is provided with an inlet and outlet for an internal circulating medium. The crystallization plate assembly is integrated with the vessel lid through the internal circulation medium inlet and outlet, and the crystallization plate assembly is distributed at a certain angle inside the multi-layer crystallization glass vessel shell; The crystallization plate assembly includes multiple crystallization plates, and the surface of each crystallization plate is provided with a flow guide groove and a bubble.
2. The finned plate static melting crystallizer according to claim 1, characterized in that: The crystallization plate group includes multiple crystallization plates, which are hollow inside and are distributed in a crisscross or parallel manner. The crystallization plates are inclined at an angle of 0-90° inside the multi-layer crystallization glass reactor shell.
3. The finned plate static melting crystallizer according to claim 1, characterized in that: The guide channels are alternately distributed between the bubbles; the crystallization plate group is at a certain distance from the multilayer crystallization glass reactor shell and is uniform.
4. The finned plate static melting crystallizer according to claim 3, characterized in that: The guide channels are inclinedly distributed on the crystallizing plate, and the two ends of the guide channels are respectively connected to the outer end of the crystallizing plate. The guide channels are arranged in parallel with each other at equal intervals, and the distribution mode of the guide channels is either cross distribution or parallel distribution.
5. The finned plate static melting crystallizer according to claim 4, characterized in that: The guide channel can be cylindrical, conical, or rectangular.
6. The finned plate static melting crystallizer according to claim 3, characterized in that: The bubbles are formed by a concave bubbling process on the surface of the crystallizing plate. The bubbles are arranged in triangular, square, and circular patterns and are distributed equally and parallelly on the crystallizing plate.
7. The finned plate static melting crystallizer according to claim 6, characterized in that: The bubbles can be round, square, or triangular.
8. The finned plate static melting crystallizer according to claim 1, characterized in that: The multi-layered crystallizing glass reactor shell comprises three layers: an inner layer, a middle layer, and an outer layer. The reactor lid is also equipped with a thermocouple temperature sensor inlet and a raw material inlet. A discharge port is located at the bottom of the crystallizing glass reactor shell, and the discharge port can be opened and closed by a screw button.
9. The finned plate static melting crystallizer according to claim 8, characterized in that: The multi-layered crystallizing glass reactor shell is provided with an external circulation medium outlet and an external circulation medium inlet on both sides, respectively, for the intermediate layer.
10. The finned plate static melting crystallizer according to claim 1, characterized in that: The vessel lid and the multilayer crystallized glass vessel shell are fixed together by metal clamps and sealing rings.