CN113476882A - Sublimation crystallization device with magnetic stirring and method - Google Patents
Sublimation crystallization device with magnetic stirring and method Download PDFInfo
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- CN113476882A CN113476882A CN202110956637.8A CN202110956637A CN113476882A CN 113476882 A CN113476882 A CN 113476882A CN 202110956637 A CN202110956637 A CN 202110956637A CN 113476882 A CN113476882 A CN 113476882A
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- main reaction
- reaction tube
- sublimation
- crystallization
- tube
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- 238000000859 sublimation Methods 0.000 title claims abstract description 52
- 230000008022 sublimation Effects 0.000 title claims abstract description 52
- 238000002425 crystallisation Methods 0.000 title claims abstract description 51
- 230000008025 crystallization Effects 0.000 title claims abstract description 46
- 238000003760 magnetic stirring Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 64
- 239000011521 glass Substances 0.000 claims abstract description 34
- 230000000903 blocking effect Effects 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000741 silica gel Substances 0.000 claims abstract description 19
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 19
- 239000011324 bead Substances 0.000 claims abstract description 17
- 239000002826 coolant Substances 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 description 8
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 description 5
- 229960001680 ibuprofen Drugs 0.000 description 5
- 239000011049 pearl Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- 238000005092 sublimation method Methods 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002061 vacuum sublimation Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
- B01D7/02—Crystallisation directly from the vapour phase
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Silicon Compounds (AREA)
Abstract
A sublimation crystallization device with magnetic stirring and a method thereof are provided, wherein a sublimation crystallization mechanism is arranged on a magnetic stirrer, the sublimation crystallization mechanism is a heating jacket arranged at the lower end of a main reaction tube, a cooling jacket is arranged at the upper end of the main reaction tube, the area corresponding to the heating jacket in a cavity of the main reaction tube is a sublimation area, the area corresponding to the cooling jacket is a crystallization area, a flow blocking cone is arranged in the crystallization area in the main reaction tube, the central line of the flow blocking cone is superposed with the central line of the main reaction tube, the diameter of the upper port of the flow blocking cone is larger than that of the lower port, a silica gel plug with a glass tube is arranged on the orifice of the main reaction tube, and magnetons and at least 2 glass beads with different sizes are arranged at the bottom in the main reaction tube; the sublimation crystallization method comprises the following steps: weighing raw material powder and putting the raw material powder into a main reaction tube; vacuumizing the main reaction tube; inputting a heat medium and a cooling medium; starting a magnetic stirrer for sublimation; the crystals were collected. The invention has the advantages of simple structure, cost saving, convenient operation and high efficiency.
Description
Technical Field
The invention belongs to the technical field of chemical experimental instruments, and particularly relates to a sublimation crystallization device with magnetic stirring and a sublimation crystallization method.
Background
Sublimation crystallization is the crystallization process from a gaseous state to a solid state crystal. Sublimation crystallization tends to achieve a unique crystal structure and morphology that is different from other crystallization modes, due to less interference from other molecules. In addition, sublimation crystallization is also commonly used as a separation method to purify the target product.
The sublimation crystallization mode in the present experiment is mainly divided into vacuum sublimation crystallization and carrier gas conveying sublimation crystallization. The sublimation raw material is statically placed in the heating area in the vacuum sublimation process, and the gasified molecules are desublimated and crystallized in the low-temperature crystallization area. In the sublimation process, the raw material particles are often agglomerated along with the sublimation, the particles are bonded, the particle hardening greatly hinders the outward diffusion of the gasified molecules in the particles, and the sublimation rate is reduced.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the existing sublimation crystallization device and provide the sublimation crystallization device with magnetic stirring, which has reasonable design, simple operation and high efficiency.
The technical scheme for solving the technical problems is as follows: the utility model provides a take magnetic stirring's sublimation crystallization device, be provided with sublimation crystallization mechanism on the magnetic stirrers, sublimation crystallization mechanism is provided with the heating jacket for the lower extreme of main reaction tube, the upper end is provided with the cooling jacket, the region that the heating jacket corresponds is sublimation district in the cavity of main reaction tube, the region that the cooling jacket corresponds is crystallization district, install the silica gel stopper of taking the glass pipe on the mouth of pipe of main reaction tube, the intraductal crystallization district of main reaction is installed and is kept off the stream awl, it is fixed continuous with the silica gel stopper through the connecting rod to keep off the upper end of stream awl, the central line that keeps off the stream awl coincides with the central line of main reaction tube, the last port diameter that keeps off the stream awl is greater than the port diameter down, the intraductal bottom of main reaction is provided with magnet and 2 at least glass pearls that the size is unequal.
As a preferred technical scheme, the main reaction tube has a structure that a cylindrical tube is arranged on the spherical bottom, the spherical bottom and the cylindrical tube are connected into a whole, the wall thickness of the bottom is equal to that of the bottom, and the maximum inner diameter of the spherical bottom is equal to that of the cylindrical tube.
As a preferred technical scheme, the inner diameter of the cylindrical tube of the main reaction tube is 5-10 cm, and the height of the cylindrical tube is 20-30 cm.
As a preferred technical scheme, the taper of the flow blocking cone is 0.1-0.2, the height of the flow blocking cone is equal to the height of the cooling jacket, and the diameter of the large port is 0.6-0.8 times of the inner diameter of the main reaction pipe.
As a preferable technical scheme, the heating jacket and the cooling jacket are both of a hollow structure, the lower end of the heating jacket is provided with a heat medium inlet pipe, the upper end of the heating jacket is provided with a heat medium outlet pipe, the lower end of the cooling jacket is provided with a cooling medium inlet pipe, and the upper end of the cooling jacket is provided with a cooling medium outlet pipe.
As a preferred technical scheme, the diameter of the glass bead is 2-10 mm.
The invention also provides a sublimation crystallization method of the sublimation crystallization device with magnetic stirring, which comprises the following steps:
s1, weighing raw material powder to be sublimated, wherein the mass of the raw material powder is m grams, putting the raw material powder into a main reaction tube, and then putting magnetons, glass beads and a flow blocking cone into the main reaction tube;
s2, connecting a vacuum system on a glass tube of the silica gel plug, vacuumizing the main reaction tube at a low vacuumizing speed and then at a high vacuumizing speed, and finally keeping the vacuum pressure at p;
s3, inputting a heat medium into the heating jacket and inputting a cooling medium into the cooling jacket, wherein the temperature of the heat medium is T1The temperature of the cooling medium is T2，T1>T2；
S4, starting the magnetic stirrer, setting the rotating speed to be R, stopping inputting the heat medium and the cooling medium after sublimating for a period of time, and closing the magnetic stirrer;
s5, when the temperature of the main reaction tube is stabilized to be room temperature, slowly discharging the vacuum, opening a silica gel plug, and collecting crystals.
The invention has the following beneficial effects:
1. according to the invention, the stirring magnetons and the glass beads are arranged in the sublimation area, so that particle hardening in the sublimation process can be damaged, and transfer of sublimation gas is facilitated;
2. the grinding effect of stirring of the magnetons and the glass beads on the particles can cause the damage of the crystal structure, thereby reducing the energy barrier of crystal gasification and improving the sublimation rate;
3. the particles are crushed by stirring the magnetons and the glass beads, the specific surface area of the particles is increased, and the total sublimation area is increased;
4. the flow blocking cone guides the sublimation airflow to flow along the inner wall surface of the cavity of the crystallization area of the main reaction tube, so that the sublimation airflow can be rapidly and fully cooled and crystallized, and the airflow loss is reduced.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Figure 2 is a diagram of the crystalline ibuprofen product obtained in example 1.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and examples, but the present invention is not limited to the embodiments described below.
In fig. 1, the sublimation crystallization device with magnetic stirring of the embodiment is formed by connecting a cooling jacket 1, a main reaction tube 2, a silica plug 3, a flow blocking cone 4, a heating jacket 5, a magneton 6, glass beads 7 and a magnetic stirrer 8, wherein the magnetic stirrer 8 is provided with a sublimation crystallization mechanism, the sublimation crystallization mechanism is formed by installing the heating jacket 5 at the lower end of the main reaction tube 2 and installing the cooling jacket 1 at the upper end, the area corresponding to the heating jacket 5 in the cavity of the main reaction tube 2 is a sublimation area, the area corresponding to the cooling jacket 1 is a crystallization area, the main reaction tube 2 is a cylindrical tube processed on a spherical bottom, the spherical bottom and the cylindrical tube are connected into a whole and have the same wall thickness, the maximum inner diameter of the spherical bottom is equal to the inner diameter of the cylindrical tube, the height of the main reaction tube 2 is 25cm and the inner diameter is 8cm, the heating jacket 5 and the cooling jacket 1 are both hollow structures, a hot medium inlet pipe is processed at the lower end of a heating jacket 5, a hot medium outlet pipe is processed at the upper end of the heating jacket, a cooling medium inlet pipe is processed at the lower end of a cooling jacket 1, a cooling medium outlet pipe is processed at the upper end of the cooling jacket, a silica gel plug 3 with a glass tube is installed on a pipe orifice of a main reaction tube 2, a flow blocking cone 4 is installed in a crystallization area in the main reaction tube 2, the upper end of the flow blocking cone 4 is fixedly connected with the silica gel plug 3 through a connecting rod, the central line of the flow blocking cone 4 is superposed with the central line of the main reaction tube 2, the diameter of the upper port of the flow blocking cone 4 is larger than that of the lower port, the taper of the flow blocking cone 4 is 0.15, the height is equal to that of the cooling jacket 1, the diameter of the large port is 0.7 times of the inner diameter of the main reaction tube 2, the flow blocking cone 4 is used for guiding sublimation airflow to flow along the inner wall surface of a cavity of the crystallization area of the main reaction tube, thereby being beneficial to rapid and full cooling crystallization of sublimation gas and reducing airflow loss, glass beads 7 with different sizes in the magnet 6 and 4 are placed at the bottom of the main reaction tube 2, the diameter of biggest glass pearl 7 is 10mm, the diameter of minimum glass pearl is 2mm, help destroying the granule among the sublimation process and harden, be favorable to sublimating gaseous transfer, the stirring of magnet 6 and glass pearl 7 will arouse the destruction of crystal structure to the grinding effect that the granule produced to reduce the energy barrier of crystal gasification, improve sublimation rate, the stirring of magnet 6 and glass pearl 7 causes the breakage to the granule, the specific surface area of granule has been increased, total sublimation area has been improved.
The sublimation crystallization method of ibuprofen by adopting the device comprises the following steps:
s1, weighing 1 g of ibuprofen crystal powder to be sublimated, putting the ibuprofen crystal powder into a main reaction tube 2, and then putting a magneton 6, glass beads 7 and a flow blocking cone 4 into the reaction tube;
s2, connecting a vacuum system on the glass tube of the silica gel plug 3, starting to vacuumize, wherein the vacuumization speed is firstly low and then high, and finally keeping the vacuum pressure at 30 Pa;
s3, inputting a heat medium into the heating jacket 5 and inputting a cooling medium into the cooling jacket 1, wherein the temperature of the heat medium is T160 ℃, the temperature of the cooling medium is T2＝10℃；
S4, starting the magnetic stirrer 8, setting the rotating speed to be 20R/min, after sublimation is carried out for 6 hours, stopping inputting of the heat medium and the cooling medium, and closing the magnetic stirrer 8;
s5, when the temperature of the main reaction tube 2 is stabilized to be room temperature, slowly discharging vacuum, enabling ibuprofen crystals as shown in the figure 2 to appear in a crystallization area, opening a silica gel plug 3, and collecting the crystals.
Example 2
In this embodiment, the height of the main reaction tube 2 is 20cm, the inner diameter is 5cm, the silica gel plug 3 with a glass tube is installed on the tube opening of the main reaction tube 2, the flow blocking cone 4 is installed in the crystallization area in the main reaction tube 2, the upper end of the flow blocking cone 4 is fixedly connected with the silica gel plug 3 through a connecting rod, the central line of the flow blocking cone 4 coincides with the central line of the main reaction tube 2, the diameter of the upper port of the flow blocking cone 4 is larger than that of the lower port, the taper of the flow blocking cone 4 is 0.1, the height of the flow blocking cone is equal to that of the cooling jacket 1, the diameter of the large port is 0.6 times of the inner diameter of the main reaction tube 2, the silica gel plug 3 with a glass tube is installed on the tube opening of the main reaction tube 2, 6 and 5 glass beads 7 with different sizes are placed on the bottom in the main reaction tube 2, the diameter of the largest glass bead 7 is 8mm, and the diameter of the smallest glass bead is 3 mm. The other components and the connection relationship of the components are the same as those in embodiment 1.
Example 3
In this embodiment, the height of the main reaction tube 2 is 30cm, the inner diameter is 10cm, the silica gel plug 3 with a glass tube is installed on the tube opening of the main reaction tube 2, the flow blocking cone 4 is installed in the crystallization area in the main reaction tube 2, the upper end of the flow blocking cone 4 is fixedly connected with the silica gel plug 3 through a connecting rod, the central line of the flow blocking cone 4 coincides with the central line of the main reaction tube 2, the diameter of the upper port of the flow blocking cone 4 is larger than that of the lower port, the taper of the flow blocking cone 4 is 0.1, the height of the flow blocking cone is equal to that of the cooling jacket 1, the diameter of the large port is 0.8 times of the inner diameter of the main reaction tube 2, the silica gel plug 3 with a glass tube is installed on the tube opening of the main reaction tube 2, the bottom in the main reaction tube 2 is provided with 6 glass beads 7 with different sizes, the diameter of the largest glass bead 7 is 9mm, and the diameter of the smallest glass bead is 2 mm. The other components and the connection relationship of the components are the same as those in embodiment 1.
Claims (7)
1. The utility model provides a take magnetic stirring's sublimation crystallization device which characterized in that: the magnetic stirrer (8) is provided with a sublimation crystallization mechanism, the sublimation crystallization mechanism is characterized in that the lower end of the main reaction tube (2) is provided with a heating jacket (5), the upper end of the main reaction tube is provided with a cooling jacket (1), the area corresponding to the heating jacket (5) in the cavity of the main reaction tube (2) is a sublimation area, the region that cooling jacket (1) corresponds is the crystallization zone, install silica gel stopper (3) of taking the glass pipe on the mouth of pipe of main reaction tube (2), crystallization zone installs in main reaction tube (2) and keeps off stream awl (4), the upper end that keeps off stream awl (4) is passed through the connecting rod and is fixed continuous with silica gel stopper (3), the central line that keeps off stream awl (4) coincides with the central line of main reaction tube (2), the last port diameter that keeps off stream awl (4) is greater than the port diameter down, the bottom is provided with magneton (6) and 2 at least glass pearl (7) that the size is unequal in main reaction tube (2).
2. A sublimation crystallization apparatus with magnetic stirring according to claim 1, characterized in that: the main reaction tube (2) is structurally characterized in that a cylindrical tube is arranged on the spherical-crown-shaped bottom, the spherical-crown-shaped bottom and the cylindrical tube are connected into a whole, the wall thickness of the cylindrical tube is equal, and the maximum inner diameter of the spherical-crown-shaped bottom is equal to the inner diameter of the cylindrical tube.
3. A sublimation crystallization apparatus with magnetic stirring according to claim 2, characterized in that: the inner diameter of the cylindrical tube of the main reaction tube (2) is 5-10 cm, and the height of the cylindrical tube is 20-30 cm.
4. A sublimation crystallization apparatus with magnetic stirring according to claim 1, characterized in that: the taper of the flow blocking cone (4) is 0.1-0.2, the height of the flow blocking cone is equal to that of the cooling jacket (1), and the diameter of the large port is 0.6-0.8 times of the inner diameter of the main reaction tube (2).
5. A sublimation crystallization apparatus with magnetic stirring according to claim 1, characterized in that: the heating jacket (5) and the cooling jacket (1) are both of a hollow structure, a heat medium inlet pipe is arranged at the lower end of the heating jacket (5), a heat medium outlet pipe is arranged at the upper end of the heating jacket, a cooling medium inlet pipe is arranged at the lower end of the cooling jacket (1), and a cooling medium outlet pipe is arranged at the upper end of the cooling jacket.
6. A sublimation crystallization apparatus with magnetic stirring according to claim 1, characterized in that: the diameter of the glass beads (7) is 2-10 mm.
7. The sublimation crystallization method of claim 1, comprising the steps of:
s1, weighing raw material powder to be sublimated, wherein the mass of the raw material powder is m grams, putting the raw material powder into a main reaction tube (2), and then putting a magneton (6), glass beads (7) and a flow blocking cone (4);
s2, connecting a vacuum system on a glass tube of the silica gel plug (3), vacuumizing the main reaction tube (2), wherein the vacuumizing speed is low firstly and then high, and finally, keeping the vacuum pressure as p;
s3, inputting a heat medium into the heating jacket (5) and inputting a cooling medium into the cooling jacket (1), wherein the temperature of the heat medium is T1The temperature of the cooling medium is T2，T1>T2；
S4, starting the magnetic stirrer (8), setting the rotating speed to be R, stopping inputting the heat medium and the cooling medium after sublimating for a period of time, and closing the magnetic stirrer (8);
s5, when the temperature of the main reaction tube (2) is stabilized to be room temperature, slowly discharging the vacuum, opening the silica gel plug (3), and collecting crystals.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110956637.8A CN113476882A (en) | 2021-08-19 | 2021-08-19 | Sublimation crystallization device with magnetic stirring and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110956637.8A CN113476882A (en) | 2021-08-19 | 2021-08-19 | Sublimation crystallization device with magnetic stirring and method |
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| CN202110956637.8A Pending CN113476882A (en) | 2021-08-19 | 2021-08-19 | Sublimation crystallization device with magnetic stirring and method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11171801A (en) * | 1997-12-11 | 1999-06-29 | Idemitsu Kosan Co Ltd | Sublimation purification |
| CN205613076U (en) * | 2016-04-22 | 2016-10-05 | 马骋 | Honeycomb formula sublimator |
| CN208805975U (en) * | 2017-11-10 | 2019-04-30 | 范唯凌 | A kind of experiment solid sublimation device |
| CN212806605U (en) * | 2020-08-21 | 2021-03-26 | 圣奥化学科技有限公司 | Condenser |
-
2021
- 2021-08-19 CN CN202110956637.8A patent/CN113476882A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11171801A (en) * | 1997-12-11 | 1999-06-29 | Idemitsu Kosan Co Ltd | Sublimation purification |
| CN205613076U (en) * | 2016-04-22 | 2016-10-05 | 马骋 | Honeycomb formula sublimator |
| CN208805975U (en) * | 2017-11-10 | 2019-04-30 | 范唯凌 | A kind of experiment solid sublimation device |
| CN212806605U (en) * | 2020-08-21 | 2021-03-26 | 圣奥化学科技有限公司 | Condenser |
Non-Patent Citations (1)
| Title |
|---|
| 余绍火等, 西安地图出版社 * |
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Application publication date: 20211008 |