CN219440736U - Crystallization desolventizing device for liquid compound - Google Patents
Crystallization desolventizing device for liquid compound Download PDFInfo
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- CN219440736U CN219440736U CN202320672649.2U CN202320672649U CN219440736U CN 219440736 U CN219440736 U CN 219440736U CN 202320672649 U CN202320672649 U CN 202320672649U CN 219440736 U CN219440736 U CN 219440736U
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- tank body
- valve
- desolventizing
- liquid compound
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 31
- 238000002425 crystallisation Methods 0.000 title claims abstract description 31
- 230000008025 crystallization Effects 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000004031 devitrification Methods 0.000 claims description 10
- 238000007689 inspection Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 abstract description 18
- 238000002844 melting Methods 0.000 abstract description 7
- 230000008018 melting Effects 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 6
- 239000013557 residual solvent Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 description 16
- 238000001816 cooling Methods 0.000 description 14
- 238000000034 method Methods 0.000 description 10
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 9
- 239000003507 refrigerant Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model discloses a crystallization desolventizing device for a liquid compound, which comprises a first tank body, a condensing device and a second tank body which are sequentially communicated; the upper end and the lower end of the first tank body are respectively provided with a material input pipe and a material output pipe, the material input pipe is provided with a first valve, and the material output pipe is provided with a second valve; a coil is arranged in the first tank body, two ends of the coil extend out of the side wall of the tank body respectively, and two ends of the extending coil are communicated with an external cold and hot medium circulation system respectively; the upper end of the first tank body is provided with a stirring motor, a stirring shaft of the stirring motor extends out of the first tank body, and a stirrer of the stirring shaft is positioned at the inner side of the coil pipe; and the upper part of the second tank body is provided with a three-way valve, and three ports of the three-way valve are respectively communicated with the second tank body, an external negative pressure system and the atmosphere. The utility model combines crystallization, melting and solvent removal of the liquid compound, realizes recovery of residual solvent and avoids pollution of the solvent to the environment.
Description
Technical Field
The utility model relates to the field of chemical industry, in particular to a crystallization desolventizing device for liquid compounds.
Background
The liquid compound is solid at a temperature lower than the melting point of the liquid compound and is liquid at a temperature higher than the melting point of the liquid compound, and the device is used for creating a temperature atmosphere higher than or lower than the melting point of the liquid compound so as to achieve the purpose of quick melting or crystallization of the compound, thereby realizing the purposes of refining the compound containing certain impurities and removing the solvent carried by the compound. For example, CN102471214a discloses an acrylic acid crystallization apparatus and an acrylic acid crystallization method using the same, wherein the apparatus is a crystallization apparatus for separating an acrylic acid-containing solution into a mother solution and a purified acrylic acid solution, the crystallization apparatus having a crystallization device for alternately taking out the mother solution and a purified acrylic acid take-out port; and a supply line for supplying an acrylic acid-containing solution to the devitrification vessel; and a recovery line connected to the take-out port and configured to alternately recover the mother liquor and the purified acrylic acid from the crystallizer, wherein the recovery line is provided with an opening/closing member including a ball valve or a gate valve. By this crystallization apparatus, high-purity acrylic acid can be efficiently obtained.
However, the crystallization device still has the defects that: the reaction temperature cannot be detected in real time, and the temperature value cannot be directly fed back. In addition, the problem of solvent recovery is not well addressed.
Disclosure of Invention
Aiming at the defects in the prior art, the utility model provides a crystallization desolventizing device of a liquid compound, which comprises a first tank body, a condensing device and a second tank body which are sequentially communicated; the upper end and the lower end of the first tank body are respectively provided with a material input pipe and a material output pipe, the material input pipe is provided with a first valve, and the material output pipe is provided with a second valve; a coil is arranged in the first tank body, two ends of the coil extend out of the side wall of the tank body respectively, and two ends of the extending coil are communicated with an external cold and hot medium circulation system respectively; the upper end of the first tank body is provided with a stirring motor, a stirring shaft of the stirring motor extends out of the first tank body, and a stirrer of the stirring shaft is positioned at the inner side of the coil pipe; the upper part of the second tank body is provided with a three-way valve, and three ports of the three-way valve are respectively communicated with the second tank body, an external negative pressure system and the atmosphere; a third valve is arranged between the second tank body and the condensing device.
The utility model has the beneficial effects that: firstly, an external cold and hot medium circulation system is used for introducing a refrigerant into the coil pipe, crystallizing the liquid compound, and opening a second valve after crystallization is finished to release residual solvent. And then the external cold and hot medium circulation system is used for introducing a hot medium into the coil pipe to completely melt the crystallized materials, the tee joint is communicated with the external negative pressure system, the gaseous solvent is liquefied by the condensing device and is discharged into the second tank body until the residual amount of the solvent in the first tank body meets the standard, and the external cold and hot medium circulation system is turned off, so that the external negative pressure system is turned off, the recovery of the residual solvent is realized, the pollution of the solvent to the environment is avoided, and the recovery treatment problem of the solvent is solved.
Preferably, a reflux pipeline communicated with the first tank body is further arranged between the second tank body and the condensing device, and the third valve is positioned between the reflux pipeline and the second tank body. The return pipe is provided with a fourth valve. The fourth valve is switched on and off according to the requirement, and the backflow pipe is reserved for standby. The lower end of the second tank body is provided with a discharge pipe, and the discharge pipe is provided with a fifth valve. The recovered solvent is stored in the second tank body, the fifth valve is opened, the recovered solvent is discharged, and the solvent is convenient to collect.
Preferably, an observation window is arranged at the upper end of the first tank body.
Preferably, a jacket is sleeved outside the first tank body. The jacket is hollow, connecting pipes communicated with the inner cavity of the jacket are respectively arranged at the upper part and the lower part of the jacket, and the two connecting pipes are communicated with an external cold and hot medium circulating system. And two connecting nozzles of the condensing device are respectively communicated with an external cold and hot medium circulating system. The external cooling and heating medium circulation system is provided with more than three groups of interfaces, each group of cooling media or heating media is independently controlled and not affected, and the cooling media and the heating media can be switched, and the cooling media and the heating media can be selected according to requirements.
Preferably, the coil pipe extends from the upper part and the lower part of the first tank body at two ends respectively.
Preferably, a temperature sensor is arranged at the bottom of the first tank body, and the temperature sensor is electrically connected with the temperature inspection instrument. The data collected by the temperature sensor is sent to the temperature inspection instrument, the temperature inspection instrument electrically processes the data and displays the real-time temperature and the temperature curve on the display, so that the crystallization temperature at each moment can be visually seen, and the crystallization process and the desolventizing process can be controlled.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. Like elements or portions are generally identified by like reference numerals throughout the several figures. In the drawings, elements or portions thereof are not necessarily drawn to scale.
Fig. 1 is a schematic structural diagram of a first embodiment.
In the drawing, a first tank 1, a condensing device 2, a second tank 3, a coil 4, a jacket 5, a stirring motor 6, a stirrer 7, an observation window 8, a material input pipe 9, a material output pipe 10, a first valve 11, a second valve 12, a temperature sensor 13, a three-way valve 14, a third valve 15, a fourth valve 16, a discharge pipe 17, a fifth valve 18, a connecting pipe 19, a connecting nozzle 20 and a return pipe 21.
Detailed Description
Embodiments of the technical scheme of the present utility model will be described in detail below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present utility model, and thus are merely examples, and are not intended to limit the scope of the present utility model.
It is noted that unless otherwise indicated, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this utility model pertains.
Embodiment one:
as shown in fig. 1, a first embodiment provides a crystallization desolventizing device for a liquid compound, which includes a first tank 1, a condensing device 2 and a second tank 3 that are sequentially connected, wherein the specific structure of the first tank 1 is as follows:
the inside of the first tank body 1 is provided with a coil pipe 4, and the coil pipe 4 is in a spiral shape and uniformly distributed in the inside of the first tank body 1. Two ends of the coil pipe 4 extend out of the side wall of the tank body respectively, and two ends of the extending coil pipe 4 are communicated with an external cold and hot medium circulation system respectively. Specifically, both ends of the coil pipe 4 protrude from the upper and lower portions of the first tank 1, respectively. The jacket 5 is sleeved outside the first tank body 1. The jacket 5 is hollow, the upper part and the lower part of the jacket 5 are respectively provided with a connecting pipe 19 communicated with the inner cavity of the jacket 5, and the two connecting pipes 19 are both communicated with an external cold and hot medium circulating system. The upper end of the first tank body 1 is provided with a stirring motor 6, a stirring shaft of the stirring motor 6 extends out of the first tank body 1, and a stirrer 7 of the stirring shaft is positioned at the inner side of the coil pipe 4.
In addition, the upper end of the first tank body 1 is provided with an observation window 8, so that the phase change state of the internal materials can be observed conveniently. A material input pipe 9 and a material output pipe 10 are respectively arranged at the upper end and the lower end of the first tank body 1, and the material input pipe 9 is provided with a first valve 11 and the material output pipe 10 is provided with a second valve 12. A temperature sensor 13 is arranged at the bottom of the first tank body 1, and the temperature sensor 13 is electrically connected with a temperature inspection instrument. The data collected by the temperature sensor 13 is sent to a temperature inspection instrument, the temperature inspection instrument electrically processes the data and displays the real-time temperature and the temperature curve on a display thereof, so that the crystallization temperature at each moment can be visually seen, and the crystallization process and the desolventizing process can be controlled.
The specific structure of the second tank 3 and the condensing device 2 in this embodiment is as follows:
the upper part of the second tank body 3 is provided with a three-way valve 14, and three ports of the three-way valve 14 are respectively communicated with the second tank body 3, an external negative pressure system and the atmosphere. A third valve 15 is arranged between the second tank 3 and the condensing device 2. A return pipeline 21 communicated with the first tank 1 is further arranged between the second tank 3 and the condensing device 2, and the third valve 15 is positioned between the return pipeline 21 and the second tank 3. The return line 21 is provided with a fourth valve 16. The fourth valve 16 is opened and closed as required and the return pipe is ready for use. The lower end of the second tank body 3 is provided with a discharge pipe 17, and the discharge pipe 17 is provided with a fifth valve 18. The recovered solvent is stored in the second tank 3, the fifth valve 18 is opened, the recovered solvent is discharged, and the solvent is convenient to collect.
The two connection nozzles 20 of the condensing device 2 in this embodiment are respectively communicated with an external cooling and heating medium circulation system. The external cooling and heating medium circulation system is provided with more than three groups of interfaces, each group of cooling media or heating media is independently controlled and not affected, and the cooling media and the heating media can be switched, and the cooling media and the heating media can be selected according to requirements. In this embodiment, the coil 4, the jacket 5 and the condensing device 2 are respectively connected with three groups of interfaces of an external cooling and heating medium circulation system, and the external cooling and heating medium circulation system provides cooling medium or heating medium, and can also switch cooling and heating medium at any time according to the reaction requirement.
In addition, the first tank 1 and the second tank 3 can be connected with an online cleaning system, and can be cleaned online after use, so that the operation is simple.
Embodiment two:
embodiment two provides a crystallization method, and the crystallization method of embodiment two is based on the crystallization desolventizing device of embodiment one. The method comprises the following steps:
s1, opening a third valve, closing other valves, and vacuumizing the first tank, the condensing device and the second tank, wherein the three-way valve is in a state that the second tank is communicated with an external negative pressure system.
S2, opening a first valve, pumping the mixed solution of the liquid compound and part of solvent into a first tank body through a material input pipe, and switching the three-way valve to a state that the second tank body is communicated with the atmosphere after the material is added.
S3, starting a stirring motor, homogenizing the mixed solution system, and then closing stirring.
S4, respectively introducing refrigerants into the coil pipe and the jacket by the external cold and heat medium circulation system to realize refrigerant circulation.
S5, cooling medium temperature is reduced to be lower than the melting point of the compound, and crystallization of the compound is achieved in the first tank body.
S6, after the crystallization of the materials in the first tank body is finished, opening a second valve, discharging residual solvent, and completing crystallization.
Embodiment III:
embodiment three provides a desolventizing method, and the crystallization method of embodiment three is based on the crystallization method of embodiment two. The method comprises the following steps:
s1, after the steps in the second embodiment are sequentially executed, the external cold and hot medium circulation system introduces a refrigerant into the condensing device to realize refrigerant circulation.
S2, closing the second valve.
S3, respectively introducing heating media into the coil pipe and the jacket by the external cooling and heating medium circulation system, replacing the original cooling media, and realizing heating medium circulation until all solids in the first tank body are melted.
S4, starting the stirring motor.
S5, switching the three-way valve to a state that the second tank body is communicated with an external negative pressure system, and starting to remove the solvent.
S6, after the residual quantity of the material solvent in the first tank body meets the standard, closing the external cold and hot medium circulation system, and switching the three-way valve to a state that the second tank body is communicated with the atmosphere.
S7, opening a second valve, and collecting the desolventized product to finish desolventizing.
The crystallization method of the second embodiment and the desolventizing method of the third embodiment are simple in operation, and industrialization of crystallization, melting and desolventizing operations of the liquid compound can be easily achieved.
The compounds mentioned in the first, second and third embodiments may be acrylic acid, methacrylic acid and other compounds, wherein the impurities are formaldehyde, propionic acid, acetic acid and the like, and the solvent used is selected from dichloromethane, n-hexane, ethyl acetate, methyl tert-butyl ether and the like.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present utility model, and not for limiting the same; although the utility model has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the utility model, and are intended to be included within the scope of the appended claims and description.
Claims (10)
1. A crystallization desolventizing device of liquid compound is characterized in that: comprises a first tank body, a condensing device and a second tank body which are communicated in sequence;
the upper end and the lower end of the first tank body are respectively provided with a material input pipe and a material output pipe, the material input pipe is provided with a first valve, and the material output pipe is provided with a second valve; a coil is arranged in the first tank body, two ends of the coil extend out of the side wall of the tank body respectively, and two ends of the extending coil are communicated with an external cold and hot medium circulation system respectively; the upper end of the first tank body is provided with a stirring motor, a stirring shaft of the stirring motor extends out of the first tank body, and a stirrer of the stirring shaft is positioned at the inner side of the coil pipe;
the upper part of the second tank body is provided with a three-way valve, and three ports of the three-way valve are respectively communicated with the second tank body, an external negative pressure system and the atmosphere; a third valve is arranged between the second tank body and the condensing device.
2. The apparatus for devitrification and desolventizing a liquid compound according to claim 1, wherein: and a reflux pipeline communicated with the first tank body is further arranged between the second tank body and the condensing device, and the third valve is positioned between the reflux pipeline and the second tank body.
3. The apparatus for devitrification and desolventizing a liquid compound according to claim 2, wherein: the reflux pipeline is provided with a fourth valve; the lower end of the second tank body is provided with a discharge pipe, and the discharge pipe is provided with a fifth valve.
4. The apparatus for devitrification and desolventizing a liquid compound according to claim 1, wherein: the upper end of the first tank body is provided with an observation window.
5. The apparatus for devitrification and desolventizing a liquid compound according to claim 1, wherein: the jacket is sleeved outside the first tank body.
6. The apparatus for devitrification and desolventizing a liquid compound according to claim 5, wherein: the jacket is hollow, connecting pipes communicated with the inner cavity of the jacket are respectively arranged at the upper part and the lower part of the jacket, and the two connecting pipes are communicated with an external cold and hot medium circulating system.
7. The apparatus for devitrification and desolventizing a liquid compound according to claim 1, wherein: and two connecting nozzles of the condensing device are respectively communicated with an external cold and hot medium circulating system.
8. The apparatus for devitrification and desolventizing a liquid compound according to claim 1, wherein: the two ends of the coil pipe extend out from the upper part and the lower part of the first tank body respectively.
9. A devitrification and desolventizing device for a liquid compound according to any one of claims 1 to 8, wherein: the bottom of the first tank body is provided with a temperature sensor.
10. The apparatus for devitrification and desolventizing a liquid compound according to claim 9, wherein: the temperature sensor is electrically connected with the temperature inspection instrument.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320672649.2U CN219440736U (en) | 2023-03-30 | 2023-03-30 | Crystallization desolventizing device for liquid compound |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320672649.2U CN219440736U (en) | 2023-03-30 | 2023-03-30 | Crystallization desolventizing device for liquid compound |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN219440736U true CN219440736U (en) | 2023-08-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202320672649.2U Active CN219440736U (en) | 2023-03-30 | 2023-03-30 | Crystallization desolventizing device for liquid compound |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN219440736U (en) |
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- 2023-03-30 CN CN202320672649.2U patent/CN219440736U/en active Active
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| GR01 | Patent grant | ||
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| TR01 | Transfer of patent right |
Effective date of registration: 20231007 Address after: No. 296 Tianfu Road, Wendeng District, Weihai City, Shandong Province, 264499 Patentee after: Weihai Wendeng District Inspection and Testing Center Address before: No. 312, Shichang Avenue, Torch Hi tech Industrial Development Zone, Weihai, Shandong 264200 Patentee before: Han Jiangsheng |