CN111139517A - Preparation method and device of array type liquid drop crystal - Google Patents
Preparation method and device of array type liquid drop crystal Download PDFInfo
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- CN111139517A CN111139517A CN202010005665.7A CN202010005665A CN111139517A CN 111139517 A CN111139517 A CN 111139517A CN 202010005665 A CN202010005665 A CN 202010005665A CN 111139517 A CN111139517 A CN 111139517A
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- 239000013078 crystal Substances 0.000 title claims abstract description 128
- 239000007788 liquid Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 63
- 239000000758 substrate Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 12
- 230000002209 hydrophobic effect Effects 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 6
- 238000005192 partition Methods 0.000 claims description 4
- 239000002250 absorbent Substances 0.000 claims description 3
- 230000002745 absorbent Effects 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000003814 drug Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000003570 air Substances 0.000 description 16
- 230000033001 locomotion Effects 0.000 description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
Abstract
The invention discloses a method and a device for preparing an array crystal. The array type crystal preparation device comprises an operation box, an array liquid drop preparation module and a crystal growth substrate module; the method can accurately obtain the quality of the crystal crystals by adjusting the volume of the array liquid drops, and accurately regulate and control the temperature and humidity to obtain the target crystal form or crystal habit, and has the advantages of quick and simple operation, economic and cheap production process, and environmental protection. The whole set of device can be widely used for the growth and preparation of various crystals (nano, atomic and molecular), in particular to the production process of medicine preparation.
Description
Technical Field
The invention relates to a preparation method for efficiently and economically growing various crystals and a related device thereof.
Background
The preparation method of the crystal at the present stage mainly comprises a melt growth method (a pulling method, a Bridgman-Stockbarge method, a zone melting method and a flame melting method), a solution growth method (a water solution method, a hydrothermal method and a fluxing agent method), a vapor deposition method, a solid phase reaction method and the like. The solution growth method takes a hydrothermal method as an example, the method has extremely high requirements on equipment, needs high-quality crystal seeds and has a long growth rate and a long period; the vapor deposition method has the disadvantages that the formed crystal is not wide enough in category, the product quality is difficult to control, and the operation and the working device are complicated; solid phase reaction methods are slow and generally require high temperatures (harsh reaction conditions).
The solvent volatilization method is adopted for the crystal growth in a very small number, the spray drying method is usually adopted in a factory, the spray drying method is usually to form spray from the raw material liquid by adopting ultrahigh temperature, and the energy consumption is large. In addition, in the production and preparation of part of pharmaceutical enterprises, the existing preparation method is to form a spray evaporation solution from a raw material liquid so as to form target crystals, and then mix the obtained target crystals with auxiliary materials to prepare the medicine.
Disclosure of Invention
In order to overcome the defects of complex operation, uncontrollable product quality and slow reaction speed and long growth period of the existing crystal preparation method and device, the invention provides the array type liquid drop crystal preparation method and device.
The technical scheme of the invention is as follows:
the array type liquid drop crystal preparation device comprises an operation box, an array liquid drop preparation module, a crystal growth substrate module and a solvent absorption device;
the operation box is a closable cavity, a temperature and humidity regulation module is arranged in the operation box, and the solvent absorption device is arranged on the operation box; the operation box is internally provided with a plurality of layers of crystal growth areas which are separated by partition plates, and the gas between the crystal growth areas is communicated;
the upper surface of the crystal growth substrate module is a smooth plane, and the surface is subjected to hydrophobic treatment; the crystal growth substrate module may be horizontally placed within the crystal growth region and may be removed from the crystal growth region.
The array liquid drop preparation module comprises a plurality of liquid drop tubes which have the same structure and are arranged in an array, and the array liquid drop preparation module is used for dropping liquid to the crystal growth substrate plate; when dropping liquid, the array liquid drop preparation module is positioned right above the crystal growth substrate module. The number and arrangement of the drip tubes can be changed as required.
As a preferable scheme of the invention, a base access door is arranged on the side edge of the operation box, and a sealing strip is arranged between the base access door and the box body of the operation box.
As a preferable scheme of the invention, the solvent absorption module comprises a cylinder and an air suction pump connected with the cylinder, wherein a solid absorbent (such as activated carbon) is filled in the cylinder, and the cylinder is communicated with a cavity in the operation box.
As a preferred scheme of the present invention, the temperature and humidity control module includes a controller, a heater, an air cooler, a humidifier, and a temperature and humidity sensor, the temperature and humidity sensor is connected to the controller for transmitting temperature and humidity detection data, and the controller is electrically connected to the heater, the air cooler, and the humidifier.
As a preferable scheme of the invention, the hydrophobic layer of the crystal growth substrate module is obtained by performing hydrophobic treatment by adopting a plasma technology.
As the preferable scheme of the invention, a piston is arranged in the dropping liquid pipe, and a dropping liquid port is arranged at the bottom of the dropping liquid pipe; the array liquid drop preparation module also comprises at least one stepping motor, and a piston of the liquid drop tube is connected with the stepping motor through a connecting piece; the pistons in the array droplet preparation module move synchronously.
The invention also discloses a preparation method of the array type liquid drop crystal, which comprises the following steps:
1) preparing a crystal growth solution;
2) the array type liquid drop preparation module absorbs the crystal growth solution and moves the array type liquid drop preparation module to be right above the crystal growth substrate module; adjusting the distance between the array type liquid drop preparation module and the crystal growth substrate module to a set value;
3) the array type liquid drop preparation module quantitatively and accurately drops liquid drops on the crystal growth substrate module;
4) setting temperature and humidity set values in the operation box, horizontally conveying the crystal growth substrate module to a crystal growth area in the operation box, and then sealing the operation box; the temperature and humidity control module works to maintain the temperature and humidity in the operation box at a set value; starting a solvent absorption device to absorb the solvent volatilized in the operation box;
5) and starting the crystal growth process, taking out the crystal growth substrate module after the growth is finished, and separating the crystal from the crystal growth substrate module.
As a preferred scheme of the invention, the movement of the crystal growth substrate module is completed by a three-dimensional operation platform, and the three-dimensional operation platform comprises an X-axis motion assembly, a Y-axis motion assembly and a Z-axis motion assembly; as an optional scheme, the X-axis motion assembly is arranged on the base, the Y-axis motion assembly is arranged on the X-axis motion assembly, and the whole Y-axis motion assembly can translate along the X-axis direction; the Z-axis motion assembly is arranged on the Y-axis motion assembly, and the whole Z-axis motion assembly can translate along the Y-axis direction; a carrying component is arranged on the Z-axis motion component and can move up and down along the Z-axis direction; the three-dimensional operation platform can integrally realize the movement of the carrying component in the X direction, the Y direction and the Z direction, the movement operation is realized by the driving of a motor, and the carrying component can hold or clamp the crystal growth substrate module to move.
The invention can effectively control the content of each piece, and saves one step of sorting qualified products. The invention can effectively regulate and control crystal form and crystal habit by controlling temperature and humidity, ensures the effectiveness, safety and quality controllability of the medicine and meets the requirement of industrial 4.0 development trend.
The preparation method of the array type liquid drop crystal disclosed by the invention has the advantages of prominent product controllability (controllable product quality and crystal form and crystal habit), can accurately obtain the crystal quality and control the crystal form and crystal habit, and is simple to operate, short in growth period, economic and low in price. The method and the device can be widely used for the growth and preparation of various crystals (including nano, atomic and molecular crystals), and particularly can be applied to the production and preparation of medicines. And the preparation method has relatively low temperature and saves more energy.
The invention adopts the array type dropping liquid tubes, and the product quality contained in the formed liquid drops can be controlled by different dropping volumes. And can the productivity high, once can carry out the multiunit simultaneously, production efficiency has also promoted greatly.
The invention controls the temperature and the humidity to achieve the effect of controlling the crystal form and crystal habit, the temperature and the humidity are controlled remotely by the central controller, and the automatic production is realized in the whole process.
The solvent absorption device is arranged in the device, so that the pressure balance in the closed reactor can be maintained, industrial waste gas which is toxic and harmful to the environment can be absorbed, and the effect of environmental protection is achieved.
The crystal growth substrate module provided by the invention has a hydrophobic growth plane, so that the subsequent operation process of separating the crystal from the plate is more convenient.
The invention can further adopt a three-dimensional operating platform to control the sampling and dripping processes of the liquid dropper, and the subsequent operation of putting the base plate into different interlayers of the main reactor, and can realize full automation under the control of a computer.
The main operation box adopts a multi-interlayer design, and can synchronously carry out the growth process of a plurality of groups of crystals under the same temperature and humidity condition. The production efficiency is greatly improved, uncertain factors in production are reduced, and the qualification rate of products is improved.
The present invention can prepare a plurality of crystals with the same apparatus for the initial solution obtained by different means. For example, high purity molecular crystals are produced from supersaturated solutions passing through a device.
Drawings
FIG. 1 is a schematic diagram of an array type droplet crystal manufacturing apparatus.
FIG. 2 is a schematic flow chart of a method for preparing an array of droplet crystals;
FIG. 3 is a schematic view of the structure of the operation box of the present invention;
FIG. 4 is a schematic diagram of the structure of an array droplet preparation module, wherein a is a batch view and b is a top view;
fig. 5 is a schematic view of a crystal growth substrate module.
Detailed Description
The invention is further described with reference to the accompanying drawings.
As shown in figure 1, the array type liquid drop crystal preparation device comprises an operation box 1 and a solvent absorption device 4, wherein the solvent absorption device comprises a cylinder 42 and an air suction pump 41 connected with the cylinder, a solid absorbent (such as activated carbon) is filled in the cylinder, the cylinder is communicated with a cavity in the operation box through a pipeline, and when the air suction pump 41 works, air in the operation box is sucked into the cylinder for adsorption treatment.
The array type liquid drop crystal preparation device also comprises an array liquid drop preparation module 2 and a crystal growth substrate module 3.
As shown in fig. 4, the array droplet preparation module 2 includes a plurality of droplet tubes having the same structure and arranged in an array, and the array droplet preparation module is used for dripping droplets to the crystal growth substrate module (in this embodiment, the crystal growth substrate module is a flat plate with a hydrophobic layer on the surface); when dropping liquid, the array liquid drop preparation module is positioned right above the crystal growth substrate module. The number and arrangement of the drip tubes can be changed as required. A piston 22 and a spring 21 are arranged in the dropping liquid pipe, and the bottom of the dropping liquid pipe is connected with a dropping liquid head; the array liquid drop preparation module also comprises at least one stepping motor 23, and the piston of the liquid drop tube is connected with the stepping motor through a connecting piece; when the stepping motor works, the pistons in the array liquid drop preparation module move synchronously, and the spring 21 is used for resetting the piston 22. In this embodiment, the array droplet preparation module 2 comprises 15 droplets tubes. When the array droplet preparation module 2 sucks the liquid, the droplet head is inserted into the solution, and the stepping motor operates to move the piston 22 upward, thereby sucking the liquid. During liquid dropping, the stepping motor works to enable the piston 22 to move downwards under the synergistic action of the spring restoring force and the stepping motor to extrude liquid drops, and the liquid drops are generated on the surface of the crystal growth substrate module (if the restoring force of the spring 21 meets the requirement of the liquid drops, the liquid drops can be extruded under the action of the spring 21 only).
As shown in fig. 5, the upper surface of the crystal growth substrate module is a smooth plane and the surface is subjected to hydrophobic treatment; the size specification of the substrate plate is 1000 multiplied by 600mm, and as a preferable scheme of the invention, the hydrophobic layer of the crystal growth substrate module is obtained by adopting a plasma technology to carry out hydrophobic treatment. The crystal growth substrate module may be horizontally placed within the crystal growth region and may be removed from the crystal growth region.
As shown in fig. 3, the operation box is a sealable cavity, a temperature and humidity control module is arranged in the operation box, a plurality of crystal growth areas 10 are arranged in the operation box, the crystal growth areas are separated by partition plates, and the gas between the crystal growth areas is communicated (for example, the partition plates may be hollow); the side of the operation box is provided with a base access door 11, and a sealing strip is arranged between the base access door and the box body of the operation box. The temperature and humidity control module comprises a controller 12, a heater 13, an air cooler 14, a humidifier 16 and a temperature and humidity sensor 15, the temperature and humidity sensor is connected with the controller and used for transmitting temperature and humidity detection data, and the controller is electrically connected with the heater, the air cooler and the humidifier. When the temperature and humidity sensor 15 detects that the temperature is too low, the controller 12 controls the heater 13 to heat, and when the temperature is too high, the air cooler 14 works to cool the operation box (when the ambient temperature is lower than the target temperature to be regulated, the air cooler can directly absorb and convey ambient air into the operation box to cool, and when the difference between the ambient temperature and the target temperature is small, the air cooler can adopt a small-sized refrigeration air conditioner). When the humidity is low, the humidifier 16 operates; when the humidity is high, dry air can be pumped by an air cooler or an air suction pump 41 to replace the air in the operation box.
As shown in FIG. 2, the preparation method of the array type droplet crystal of the present invention comprises the following steps:
1) preparing a crystal growth solution (which can be a supersaturated solution of a target product);
2) the array type liquid drop preparation module absorbs the crystal growth solution and moves the array type liquid drop preparation module to be right above the crystal growth substrate module; adjusting the distance between the array type liquid drop preparation module and the crystal growth substrate module to a set value;
3) the array type liquid drop preparation module quantitatively and accurately drops liquid drops on the crystal growth substrate module;
4) setting temperature and humidity set values in the operation box, horizontally conveying the crystal growth substrate module to a crystal growth area in the operation box, and then sealing the operation box; the temperature and humidity control module works to maintain the temperature and humidity in the operation box at a set value; the solvent absorption device is started to absorb the solvent volatilized in the operation box, so that the interference of the volatilized solvent is reduced;
5) and starting the crystal growth process, taking out the crystal growth substrate module after the growth is finished, and separating the crystal from the crystal growth substrate module.
The liquid drops are quantitatively dripped, and the crystal growth solution is uniform, so that uniform crystals can be obtained, the quality control is simple, and the problem of non-uniform crystal distribution is solved.
In the present invention, the movement of the array type droplet preparation module and the crystal growth substrate module may be operated by a three-dimensional operation platform, which may employ an XYZ operation platform of a 3D printing system, which may allow a part connected to the XYZ operation platform to be precisely moved. Of course, on the premise that the stability in the moving process on the crystal growth substrate module can be met, the crystal growth substrate module can be manually carried by an experimenter.
In the invention, concave holes with certain radian can be arranged in the surface of the crystal growth substrate module (hydrophobic treatment of the surface of the concave holes) so as to better bear liquid drops.
The whole preparation method is simple and convenient to operate, and the product can be quickly, economically and cheaply obtained; the quality of the crystal is accurately obtained by adjusting the volume of the array liquid drop, and the temperature and the humidity can accurately regulate and control the obtained target crystal form or crystal habit; and can be widely used for the growth and preparation of various crystals (nano, atom and molecule), and especially has more color in the direction of medicine preparation.
Claims (7)
1. An array type liquid drop crystal preparation device is characterized by comprising an operation box, an array liquid drop preparation module, a crystal growth substrate module and a solvent absorption device;
the operation box is a closable cavity, a temperature and humidity regulation module is arranged in the operation box, and the solvent absorption device is arranged on the operation box and communicated with the inside of the operation box; the operation box is internally provided with a plurality of layers of crystal growth areas which are separated by partition plates, and the gas between the crystal growth areas is communicated;
the upper surface of the crystal growth substrate module is subjected to hydrophobic treatment; the crystal growth substrate module can be horizontally placed in the crystal growth area and can be taken out of the crystal growth area;
the array liquid drop preparation module comprises a plurality of liquid drop tubes which have the same structure and are arranged in an array, and the array liquid drop preparation module is used for dropping liquid to the crystal growth substrate plate; when dropping liquid, the array liquid drop preparation module is positioned right above the crystal growth substrate module.
2. The apparatus of claim 1, wherein a base access door is provided on a side of the operation box, and a sealing strip is provided between the base access door and the box of the operation box.
3. The array type liquid drop crystal preparation device of claim 1, wherein the solvent absorption module comprises a cylinder and a suction pump connected with the cylinder, the cylinder is filled with a solid absorbent, and the cylinder is communicated with the cavity in the operation box.
4. The array type liquid drop crystal preparation device according to claim 1, wherein the temperature and humidity control module comprises a controller, a heater, an air cooler, a humidifier and a temperature and humidity sensor, the temperature and humidity sensor is connected with the controller for transmitting temperature and humidity detection data, and the controller is electrically connected with the heater, the air cooler and the humidifier.
5. The apparatus of claim 1, wherein the dropping tube has a piston therein, and the bottom of the dropping tube has a dropping head; the array liquid drop preparation module also comprises at least one stepping motor, and a piston of the liquid drop tube is connected with the stepping motor through a connecting piece; the pistons in the array droplet preparation module move synchronously.
6. The array type droplet crystal preparation apparatus of claim 1, wherein the upper surface of the crystal growth substrate module is a smooth plane.
7. A preparation method of an array type liquid drop crystal is characterized by comprising the following steps:
1) preparing a crystal growth solution;
2) the array type liquid drop preparation module absorbs the crystal growth solution and moves the array type liquid drop preparation module to be right above the crystal growth substrate module; adjusting the distance between the array type liquid drop preparation module and the crystal growth substrate module to a set value;
3) the array type liquid drop preparation module quantitatively and accurately drops liquid drops on the crystal growth substrate module;
4) setting temperature and humidity set values in the operation box, horizontally conveying the crystal growth substrate module to a crystal growth area in the operation box, and then sealing the operation box; the temperature and humidity control module works to maintain the temperature and humidity in the operation box at a set value; starting a solvent absorption device to absorb the solvent volatilized in the operation box;
5) and starting the crystal growth process, taking out the crystal growth substrate module after the growth is finished, and separating the crystal from the crystal growth substrate module.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202010005665.7A CN111139517A (en) | 2020-01-03 | 2020-01-03 | Preparation method and device of array type liquid drop crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010005665.7A CN111139517A (en) | 2020-01-03 | 2020-01-03 | Preparation method and device of array type liquid drop crystal |
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| CN111139517A true CN111139517A (en) | 2020-05-12 |
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| CN202010005665.7A Pending CN111139517A (en) | 2020-01-03 | 2020-01-03 | Preparation method and device of array type liquid drop crystal |
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2020
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Application publication date: 20200512 |