CN111617512A - High-purity crystallization method and crystallization device - Google Patents
High-purity crystallization method and crystallization device Download PDFInfo
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- CN111617512A CN111617512A CN202010573810.1A CN202010573810A CN111617512A CN 111617512 A CN111617512 A CN 111617512A CN 202010573810 A CN202010573810 A CN 202010573810A CN 111617512 A CN111617512 A CN 111617512A
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Abstract
The invention discloses a high-purity crystallization method and a crystallization device, and belongs to the technical field of crystallization. And cooling the saturated solution in which a certain solute is dissolved in the saturated solution tank to form a supersaturated solution, stretching the crystal attachment mechanism into the supersaturated solution, crystallizing, separating out crystals, climbing above the liquid level along the crystal attachment mechanism, scraping the crystals attached to the crystal attachment mechanism above the liquid level by using a scraping mechanism, and taking the part of crystals as the obtained crystals. The device comprises a crystal attaching mechanism and a scraping mechanism, wherein the crystal attaching mechanism extends into the saturated solution tank from an opening at the upper end of the saturated solution tank. The method and the device greatly improve the purity of the obtained crystal, and the purity of the obtained crystal can reach at least 99.99 percent.
Description
Technical Field
The invention belongs to the technical field of crystallization, and particularly relates to a high-purity crystallization method and high-purity crystallization equipment.
Background
The hot saturated solution cools to cause supersaturation of the solution due to the decrease in solubility of the solute, whereby the solute precipitates in the form of crystals, a process known as crystallization. Usually, the crystals appear in the solution, and then mother liquor separation is carried out to obtain the crystals, and the method has high impurity content and low purity of the obtained crystals.
There are generally two methods of crystallization: one is the evaporative solvent method, which is suitable for substances whose temperature has little influence on the solubility, and the method of 'solar salt' in coastal areas is utilized. The other method is cooling crystallization, which is suitable for substances with increased temperature and increased solubility, such as salt lake in northern region, with high summer temperature, no crystal on lake surface, and low temperature and lithangine (Na) in winter2CO3·10H2O), mirabilite (Na)2SO4·10H2O) and the likeSeparating out from salt lake. In order to obtain larger, intact crystals in the laboratory, slow temperature reduction, slow crystallization rate methods are often used.
The cooling crystallization method has the advantages of low cost, simple operation and the like, so the cooling crystallization method has wide application in industrial production, and the cooling crystallization method is divided into dividing wall type cooling crystallization and direct contact type cooling crystallization. The research and industrial application of the dividing wall type cooling crystallization are more, and the method generally comprises the following steps: and introducing a coolant into a jacket or an inner coil of the crystallization kettle or naturally cooling, and gradually generating supersaturation in the cooling process so as to separate out crystals.
In the traditional dividing wall type cooling method, precipitated crystals can be attached to the wall of a crystallization kettle, the inside of the crystallization kettle or the surface of a stirrer, the purity of the crystals is low, and secondary purification is needed.
Disclosure of Invention
The invention provides a high-purity crystallization method and a crystallization device.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the crystallization method comprises the following steps: and cooling the saturated solution in which a certain solute is dissolved in the saturated solution tank to form a supersaturated solution, stretching the crystal attachment mechanism into the supersaturated solution, crystallizing, separating out crystals, climbing above the liquid level along the crystal attachment mechanism, scraping the crystals attached to the crystal attachment mechanism above the liquid level by using a scraping mechanism, and taking the part of crystals as the obtained crystals.
The method comprises the steps of forming a supersaturated solution by cooling a saturated solution or an approximately saturated solution, extending a crystal attachment mechanism (such as a stirrer such as a glass rod) into the saturated solution, and climbing crystals along the attachment mechanism, wherein the crystals are only taken above the liquid level, and the crystal purity can reach at least 99.99%; a scraper or the like may be used to scrape off crystals located above the liquid surface on the attachment mechanism.
Separating out crystals by conventional method, such as stirring supersaturated solution with a stirrer, shaking saturated solution tank or rubbing saturated solution tank wall, standing, and standing for crystallization; or solid seed crystals are put in.
The crystal attachment mechanism, such as a glass rod for stirring, has saturated solution adhered to its surface, and the part over the liquid level has crystal formed on its surface due to solvent evaporation, and the crystal attached to the surface of the mechanism forms micro gaps, so that the saturated solution will climb up the gaps under the action of capillary phenomenon and will not crystallize continuously, and the soluble impurity will not reach saturation and will not separate out crystal, and the insoluble impurity will not climb up the gaps, so that the crystal over the liquid level has very high purity, and the purity may reach at least 99.99% in the experiment process.
Capillarity (capillarity) occurs in capillaries where the line is small enough to compare with the radius of curvature of the liquid meniscus. The entire liquid surface in the capillary tube will become curved and the liquid-solid intermolecular interactions may extend through the entire liquid. Common capillary phenomena in daily life, such as water rising in thin glass tubes due to its ability to wet the glass; on the other hand, mercury is reduced in the glass because it does not wet the glass. The reasons for this are all the functions of liquid surface tension and pressure difference between the inside and outside of the curved surface.
The combination of the beaker, the glass rod and the scraper can be used as a simple crystallizing device, saturated solution is put into the beaker, the temperature is reduced to form supersaturated solution, the glass rod is stretched into the position below the liquid level, then the glass rod is kept still, crystals are separated out below the liquid level, meanwhile, the part of the glass rod above the liquid level is also separated out, and the crystals above the liquid level on the glass rod are scraped, so that the purity of the part of the crystals is quite high.
Any apparatus which can utilize the principles of the crystallization method of the present invention can be used as the crystallization apparatus of the present invention.
A high-purity crystallization device comprises a crystal attachment mechanism and a scraping mechanism, wherein the crystal attachment mechanism extends into a saturated solution tank from an opening at the upper end of the saturated solution tank, and the scraping mechanism is used for scraping crystals attached to the surface of the crystal attachment mechanism.
Further, crystallization attachment mechanism includes that one end links firmly a plurality of crystallization attachment plates in the saturated solution groove is stretched into to the other end on the mounting panel, the crystallization attachment plate is close to or contacts the diapire in saturated solution groove, just mutual independence between a plurality of crystallization attachment plates.
Further, the scraping mechanism is a plate-shaped scraper or scraper.
Further, crystallization adheres to the mechanism and includes that one end links firmly diaphragm and the longitudinal plate that a plurality of intercrossing set up that the other end stretched into in the saturated solution groove on the mounting panel, diaphragm and longitudinal plate all are close to or contact the diapire of saturated solution groove, and are adjacent form the crystallization between diaphragm and the longitudinal plate and adhere to the passageway, the crystallization adheres to the passageway and extends the mounting panel.
Further, scrape and insert from the top that the mechanism includes by the mounting panel the crystallization adheres to the bayonet scraping bar of passageway, in bayonet scraping bar is located the crystallization and adheres to the outer one end structure limiting plate of passageway, in it has first handle to construct on the limiting plate.
Further, the crystallization attachment mechanism comprises a plurality of crystallization attachment rods, one end of each crystallization attachment rod is fixedly connected to the mounting plate, the other end of each crystallization attachment rod extends into the saturated solution tank, the plurality of crystallization attachment rods are independent from each other, and the plurality of crystallization attachment rods are close to or contact with the bottom wall of the saturated solution tank.
Furthermore, the crystal attaching rods vertically extend into the saturated solution tank.
Further, scrape from mechanism including locating the mounting panel below and with each crystallization adhere to pole along vertical sliding connection's assembly plate, in assembly plate and each crystallization adhere to pole sliding connection department and construct the crystallization and scrape from the piece, the assembly plate drives through the actuating mechanism who constructs between mounting panel and assembly plate to along vertical reciprocating motion.
Furthermore, actuating mechanism is including installing the positive and negative rotation driving motor on the mounting panel, positive and negative rotation driving motor's output coaxial arrangement has the screw rod with assembly plate threaded connection.
Furthermore, the crystal scraping piece comprises gears which are rotatably installed at the lower end of the assembling plate, the gears which are located in the same row are mutually meshed in sequence and are mutually meshed in the first row, one gear is driven to rotate by a driving wheel meshed with the gear, the driving wheel is coaxially assembled with an output shaft of a power motor installed on the assembling plate, the gears are sleeved on the corresponding crystal attaching rods, a plurality of scraping pieces are formed at the lower ends of the gears along the circumferential direction of the gears, and the scraping pieces are all in contact with the circumferential surface of the crystal attaching rods.
The purity of the crystal obtained by the crystallization method can reach at least 99.99%. Compared with the prior art, the crystallization device of the invention has the technical progress that: preparing a supersaturated solution in a saturated solution tank, extending one end of a crystal attachment mechanism into the saturated solution tank, crystallizing crystals on the crystal attachment mechanism after a period of time, gradually crystallizing upwards along the crystal attachment mechanism to fully cover the crystal attachment mechanism, wherein the purity of the part of the crystals attached to the crystal attachment mechanism above the liquid level can at least reach 99.99%, then lifting the crystal attachment mechanism away from the saturated solution tank, scraping and collecting the part of the crystals attached to the crystal attachment mechanism above the liquid level by using a scraping mechanism, then collecting the crystals below the liquid level, and scraping and collecting the crystals attached to the side wall and the bottom wall of the saturated solution tank in the same way, so that crystals with two different purities can be obtained, stored independently and used in a targeted manner according to different purposes; therefore, the method can extract the high-purity crystal for use in the field with higher purity requirement.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a schematic structural diagram of an embodiment of the present invention;
FIG. 2 is a schematic diagram of a crystal attachment mechanism according to the present invention;
FIG. 3 is a schematic view of the structure of FIG. 2 from another angle;
FIG. 4 is a schematic diagram of another crystal attachment mechanism of the present invention;
FIG. 5 is a schematic view of the structure of FIG. 4 from another angle;
FIG. 6 is a schematic view of another crystal attachment mechanism and scraping mechanism according to the present invention;
FIG. 7 is a schematic view of the structure of FIG. 6 from another angle;
FIG. 8 is a schematic view of the structure of FIG. 6 from another angle;
FIG. 9 is a schematic view of the structure of the crystal attachment bar in connection with the crystal scraping element according to the present invention;
FIG. 10 is a schematic view of a crystallization scraper according to the present invention.
Labeling components: 1-saturated solution tank, 2-mounting plate, 3-telescopic leg, 4-second handle, 501-transverse plate, 502-longitudinal plate, 503-crystal attachment channel, 504-insertion type scraping rod, 505-limiting plate, 506-first handle, 507-crystal attachment plate, 508-crystal attachment rod, 6-assembly plate, 7-power motor, 8-driving wheel, 9-crystal scraping piece, 901-gear, 902-connecting sleeve, 903-bearing, 904-scraping blade, 905-hollow channel, 10-positive and negative rotation driving motor and 11-screw.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the present invention.
The crystallization method comprises the following steps: and cooling the saturated solution in which a certain solute is dissolved in the saturated solution tank to form a supersaturated solution, extending the crystal attachment mechanism into the supersaturated solution to separate out crystals, separating out the crystals, climbing above the liquid level along the crystal attachment mechanism, and scraping the crystals attached to the crystal attachment mechanism above the liquid level by using a scraping mechanism, wherein the part of crystals are the obtained crystals.
Separating out crystals by conventional method, such as stirring supersaturated solution with a stirrer, shaking saturated solution tank or rubbing saturated solution tank wall, standing, and standing for crystallization; or solid seed crystals are put in.
The invention discloses a high-purity crystallization device, which comprises a saturated solution tank 1, a crystal attachment mechanism and a scraping mechanism as shown in figures 1-10, wherein the opening of the saturated solution tank 1 faces upwards, the crystal attachment mechanism extends into the saturated solution tank 1 from the opening at the upper end of the saturated solution tank, and the scraping mechanism is used for scraping off crystals attached to the surface of the crystal attachment mechanism. The principle of the invention is as follows: preparing a supersaturated solution in a saturated solution tank 1, extending one end of a crystal attachment mechanism into the saturated solution tank 1, separating out crystals on the crystal attachment mechanism after a period of time, gradually crystallizing upwards along the crystal attachment mechanism, gradually filling the crystal attachment mechanism, then lifting the crystal attachment mechanism away from the saturated solution tank 1, scraping and collecting the part of the crystals attached to the crystal attachment mechanism above the liquid level by using a scraping mechanism, simultaneously collecting the crystals above the liquid level on a tank wall, and then collecting the crystals in the solution, so that crystals with different purities can be obtained, and the crystals are independently stored and used in a targeted manner according to different purposes; therefore, the method can extract the high-purity crystal for use in the field with higher purity requirement.
The crystal attachment mechanism comprises a mounting plate 2 and a crystal attachment unit, wherein as shown in figures 1-8, the mounting plate 2 is positioned above a saturated solution tank 1, the crystal attachment unit is fixedly connected with the lower surface of the mounting plate 2, the crystal attachment unit extends into the saturated solution tank 1 and is close to or in contact with the bottom wall of the saturated solution tank 1, and crystals mainly grow on the crystal attachment unit and gradually climb upwards. In order to adapt to saturated solution tanks 1 of different models and adjust different gradients of crystal attachment units so as to improve the crystallization speed and purity, a plurality of telescopic legs 3 are arranged on a mounting plate 2, the adjustment of the gradients of the crystal attachment units is realized by adjusting the telescopic legs 3, and different depths of the crystal attachment units extending into the saturated solution tanks 1 can be adjusted. And for the convenience of hoisting or lifting the crystal attachment unit, a second handle 4 is constructed on the mounting plate 2, and an operator or a crane lifts the crystal attachment mechanism off the saturated solution tank 1 through the second handle 4.
As a preferred embodiment of the present invention, as shown in FIGS. 4 and 5, the crystal attachment unit comprises a plurality of crystal attachment plates 507, one end of each crystal attachment plate 507 is fixedly connected to the mounting plate 2, the other end of each crystal attachment plate 507 extends into the saturated solution tank 1, the crystal attachment plates 507 are close to or in contact with the bottom wall of the saturated solution tank 1, and the crystal attachment plates 507 are independent of each other. When the crystal attachment unit is adopted, the selected scraping mechanism is a platy scraper knife or a scraper. The crystal attachment plates 507 of this embodiment are parallel to each other, which facilitates scraping of the crystals.
As a preferred embodiment of the present invention, as shown in FIGS. 1-3, the crystal attachment unit comprises a plurality of transverse plates 501 and longitudinal plates 502 arranged to intersect with each other, one end of each of the transverse plates 501 and the longitudinal plates 502 is fixedly connected to the mounting plate 2, the other end of each of the transverse plates 501 and the longitudinal plates 502 extends into the saturated solution tank 1, each of the transverse plates 501 and the longitudinal plates 502 is close to or in contact with the bottom wall of the saturated solution tank 1, a crystal attachment channel 503 is formed between each of the adjacent transverse plates 501 and the adjacent longitudinal plates 502, and the crystal attachment channel 503 extends out of the mounting plate 2. The scraping mechanism comprises an inserted scraping rod 504 inserted into the crystal attachment channel 503 from above the mounting plate 2, a limiting plate 505 is configured at one end of the inserted scraping rod 504 outside the crystal attachment channel 503, and a first handle 506 is configured on the limiting plate 505. When the solution starts to crystallize and the crystal attachment mechanism is lifted away from the saturated solution tank 1, the operator holds the first handle 506 by hand and inserts the insertion type scraping bar 504 into the crystal attachment passage 503, and inserts the crystal so that the crystal is separated from the surface of the crystal attachment passage 503, and removes the crystal from each crystal attachment passage 503 according to the above operation.
As a preferred embodiment of the present invention, as shown in FIGS. 6 to 8, the crystal attachment unit comprises a plurality of crystal attachment rods 508, one end of each of the crystal attachment rods 508 is fixedly connected to the mounting plate 2, the other end of each of the crystal attachment rods 508 extends into the saturated solution tank 1, the crystal attachment rods 508 are independent from each other, and the crystal attachment rods 508 are close to or contact with the bottom wall of the saturated solution tank 1. The crystal attachment rods 508 in this embodiment all extend vertically into the saturated solution tank 1 to facilitate subsequent crystal removal. Specifically, the scraping mechanism includes a fitting plate 6 disposed below the mounting plate 2 and slidably connected to each of the crystal attaching rods 508 in a vertical direction, a crystal scraping member 9 is configured at a sliding connection portion of the fitting plate 6 and each of the crystal attaching rods 508, and the fitting plate 6 is driven by a driving mechanism configured between the mounting plate 2 and the fitting plate 6 and vertically reciprocates. The working principle of the embodiment is as follows: the driving mechanism drives the assembling plate 6 to reciprocate up and down, so that the crystal scraping piece 9 reciprocates along the corresponding crystal attaching rods 508 until crystals on each crystal attaching rod 508 are all scraped away, the operation is convenient, manual operation is replaced, and the labor intensity is greatly reduced. Wherein, the preferred structure of actuating mechanism is: the driving mechanism comprises a forward and reverse rotation driving motor 10 installed on the installation plate 2, a screw rod 11 in threaded connection with the assembly plate 6 is coaxially installed at the output end of the forward and reverse rotation driving motor 10, the assembly plate 6 is lifted or lowered through forward and reverse rotation of the forward and reverse rotation driving motor 10, and then the crystal scraping and separating piece 9 is used for scraping and separating crystals.
As a preferred embodiment of the present invention, as shown in fig. 7-10, the crystal scraping-off member 9 comprises a gear 901 rotatably mounted on the lower end of the mounting plate 6, the upper end of the gear 901 is configured with a connecting sleeve 902, the connecting sleeve 902 coincides with the axis of the gear 901, and a hollow passage 905 is formed at the axes of the two, the gear 901 is sleeved on the corresponding crystal attaching rod 508 through the hollow passage 905, a plurality of scraping blades 904 are formed on the lower end of the gear 901 along the circumferential direction thereof, each scraping blade 904 contacts the circumferential surface of the crystal attaching rod 508, a bearing 903 is mounted outside the connecting sleeve 902, and the housing of the bearing 903 is fixedly connected with the mounting plate 6. The gears 901 in the same row are mutually meshed in sequence, and the gears 901 in the first row are mutually meshed, wherein one gear 901 is driven by a driving wheel 8 meshed with the gear 901 to rotate, the driving wheel 8 is coaxially assembled with an output shaft of a power motor 7 arranged on an assembly plate 6, and each gear 901 is sleeved on a corresponding crystal attachment rod 508. The working principle of the embodiment is as follows: the power motor 7 drives the driving wheel 8 to rotate, the driving wheel 8 drives the gear 901 meshed with the driving wheel to rotate, other gears 901 rotate through transmission among the gears 901, meanwhile, the forward and reverse rotation driving motor 10 drives the assembling plate 6 to move downwards, and therefore the scraping plates on the gears 901 scrape off crystals on the corresponding crystal attaching rods 508.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (10)
1. A high purity crystallization method characterized by: and cooling the saturated solution in which a certain solute is dissolved in the saturated solution tank to form a supersaturated solution, stretching the crystal attachment mechanism into the supersaturated solution, crystallizing, separating out crystals, climbing above the liquid level along the crystal attachment mechanism, scraping the crystals attached to the crystal attachment mechanism above the liquid level by using a scraping mechanism, and taking the part of crystals as the obtained crystals.
2. The crystallization method according to claim 1, characterized in that: stirring the saturated solution by a stirrer, shaking the saturated solution tank or rubbing the wall of the saturated solution tank, standing, and separating out crystals.
3. A high purity crystallization apparatus, characterized by: comprises a crystal attaching mechanism and a scraping mechanism, wherein the crystal attaching mechanism extends into the saturated solution tank from an opening at the upper end of the saturated solution tank, and the scraping mechanism is used for scraping crystals attached to the surface of the crystal attaching mechanism.
4. A high purity crystallization apparatus according to claim 3, wherein: the crystallization attachment mechanism comprises a plurality of crystallization attachment plates, one end of each crystallization attachment plate is fixedly connected to the mounting plate, the other end of each crystallization attachment plate extends into the saturated solution tank, the crystallization attachment plates are close to or contact with the bottom wall of the saturated solution tank, and the crystallization attachment plates are mutually independent.
5. A high purity crystallization apparatus according to claim 4, wherein: the scraping mechanism is a plate-shaped scraper knife or a scraper.
6. A high purity crystallization apparatus according to claim 3, wherein: the crystallization adheres to the mechanism and includes that one end links firmly diaphragm and the vertical plate that a plurality of intercrossing set up that the other end stretched into in the saturated solution groove on the mounting panel, diaphragm and vertical plate all are close to or contact the diapire of saturated solution groove, and are adjacent form the crystallization between diaphragm and the vertical plate and adhere to the passageway, the crystallization adheres to the passageway and extends the mounting panel.
7. A high purity crystallization apparatus according to claim 6, wherein: scrape and insert from the mechanism and include by the top of mounting panel the crystallization adheres to the bayonet material pole of scraping of passageway, in bayonet material pole of scraping is located the crystallization adheres to the outer one end structure limiting plate of passageway, in it has first handle to construct on the limiting plate.
8. A high purity crystallization apparatus according to claim 3, wherein: the crystallization attachment mechanism comprises a plurality of crystallization attachment rods, one end of each crystallization attachment rod is fixedly connected to the mounting plate, the other end of each crystallization attachment rod extends into the saturated solution tank, the plurality of crystallization attachment rods are independent from each other, and the plurality of crystallization attachment rods are close to or contact with the bottom wall of the saturated solution tank; the crystal attaching rods vertically extend into the saturated solution tank.
9. A high purity crystallization apparatus according to claim 8, wherein: scrape from mechanism including locating the mounting panel below and with each crystallization adhere to pole along vertical sliding connection's assembly plate, in assembly plate and each crystallization adhere to pole sliding connection department and be constructed the crystallization and scrape from the piece, the assembly plate drives through the actuating mechanism who constructs between mounting panel and assembly plate to along vertical reciprocating motion.
10. A high purity crystallization apparatus according to claim 8, wherein: the driving mechanism comprises a forward and reverse rotation driving motor arranged on the mounting plate, and a screw rod in threaded connection with the mounting plate is coaxially arranged at the output end of the forward and reverse rotation driving motor;
the crystal scraping piece comprises gears which are rotatably installed at the lower end of the assembling plate, the gears which are located in the same row are mutually meshed in sequence and are located between the gears in the first row, one gear is driven by a driving wheel meshed with the gear to rotate, the driving wheel is coaxially assembled with an output shaft of a power motor installed on the assembling plate, each gear is sleeved on the corresponding crystal attaching rod, a plurality of scraping pieces are formed at the lower end of the gear along the circumferential direction of the gear, and each scraping piece is in contact with the circumferential surface of the crystal attaching rod.
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| CN202010573810.1A CN111617512B (en) | 2020-06-22 | 2020-06-22 | High-purity crystallization method and crystallization device |
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| CN202010573810.1A CN111617512B (en) | 2020-06-22 | 2020-06-22 | High-purity crystallization method and crystallization device |
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| CN210014855U (en) * | 2019-06-01 | 2020-02-04 | 武汉优斯特传感器科技有限公司 | Surface mounting type thermal resistor protection device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6182325B1 (en) * | 1998-03-10 | 2001-02-06 | Advanced Technology Materials, Inc. | Chamber cleaning mechanism |
| CN103801106A (en) * | 2012-11-02 | 2014-05-21 | 中国石油化工集团公司 | Sleeve type crystallizer |
| CN206701252U (en) * | 2017-03-22 | 2017-12-05 | 深圳市九明药业有限公司 | A kind of reactor of fully recovery crystallization |
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