CN211142241U

CN211142241U - Multifunctional single crystal cultivation equipment

Info

Publication number: CN211142241U
Application number: CN201922482828.6U
Authority: CN
Inventors: 莫俊
Original assignee: Hangzhou Yuzheng Medicine Technology Co ltd
Current assignee: Hangzhou Yuzheng Medicine Technology Co ltd
Priority date: 2019-12-30
Filing date: 2019-12-30
Publication date: 2020-07-31
Anticipated expiration: 2029-12-30

Abstract

The utility model discloses a multifunctional single crystal cultivation device, which comprises an anhydrous anaerobic operating system, a plurality of groups of cultivation devices and a temperature control box; the culture device is arranged in the temperature control box; the anhydrous anaerobic operation system comprises a double-row pipe, a vacuumizing device, a nitrogen tank and a tail gas receiving device, wherein the double-row pipe comprises an A pipe and a B pipe, the A pipe is communicated with the vacuumizing device through an A valve, one end of the B pipe is communicated with the nitrogen tank through a B valve, and the other end of the B pipe is communicated with the tail gas receiving device through a C valve; the culture device comprises a sample tube A and a sample tube B which are communicated through a thin tube; the sample tube B is respectively communicated with the tube A and the tube B of the double-row tube through a three-way tube, and a double-inclined three-way piston is arranged on the three-way tube. The multifunctional single crystal cultivation equipment of the utility model can carry out a plurality of different crystallization modes, and the various crystallization modes can be synchronously developed, thereby improving the single crystal cultivation efficiency; for samples with poor stability, the device can be used for carrying out single crystal culture under the protection of nitrogen, and the application range is wide.

Description

Multifunctional single crystal cultivation equipment

Technical Field

The utility model relates to the technical field of experimental instruments, concretely relates to equipment is cultivateed to multi-functional single crystal.

Background

The single crystal, that is, the particles inside the crystal are regularly and periodically arranged in three-dimensional space, or the whole crystal is composed of the same spatial lattice in three-dimensional direction, and the arrangement of particles in space in the whole crystal is long-range order. The entire crystal lattice of a single crystal is continuous, and has important industrial applications, and the single crystal has wide applications in structural analysis in fields such as coordination chemistry, inorganic material chemistry, metal organic chemistry, and in particular, chiral drug development. The single crystal growth is of great significance because it is necessary to grow a good single crystal by analyzing the single crystal structure using the single crystal diffraction technique.

Currently, there are various methods for single crystal cultivation, including a volatilization method, a diffusion method, a temperature difference method, a contact method, and an autoclave method. The methods commonly used in the laboratory are generally achieved by cooling crystallization, volatilization crystallization, diffusion crystallization; crystal growth is affected by various external factors such as temperature change, pressure of solvent volatilization, etc. In the laboratory for growing single crystals, the external conditions are often difficult to control, resulting in a low success rate of growing single crystals. Chinese patent 201420444653.4 discloses a multifunctional volatilization crystallizer which is convenient for changing different single crystal culture modes and can perform speed-controlled temperature-controlled volatilization crystallization, speed-controlled temperature-controlled diffusion crystallization and cooling crystallization. However, this device is not suitable for poorly stable compounds. Chinese patent 201620576464.1 provides a single crystal cultivation device with controllable conditions, which can control the temperature and pressure conditions of single crystal cultivation, and the user can monitor the growth condition of single crystal remotely, but the single crystal cultivation method is single.

SUMMERY OF THE UTILITY MODEL

The utility model aims to provide a multifunctional single crystal cultivation device which can carry out a plurality of different crystallization modes, and the various crystallization modes can be synchronously developed, thereby improving the single crystal cultivation efficiency; moreover, the device can be used for carrying out single crystal culture on a sample with poor stability under the protection of nitrogen, and has a wide application range.

The technical scheme of the utility model: a multifunctional single crystal culture device comprises an anhydrous anaerobic operating system, a temperature control box and a plurality of groups of culture devices; the culture device is arranged in the temperature control box; the waterless and anaerobic operation system comprises a double-row pipe, a vacuumizing device, a nitrogen tank and a tail gas receiving device, wherein the double-row pipe comprises a pipe A and a pipe B; the pipe A is communicated with a vacuumizing device through a valve A, one end of the pipe B is communicated with a nitrogen tank through a valve B, and the other end of the pipe B is communicated with a tail gas receiving device through a valve C; the culture device comprises a sample tube A and a sample tube B, wherein the sample tube A is communicated with the sample tube B through a thin tube; the sample tube B is respectively communicated with the tube A and the tube B of the double-row tube through a three-way tube, and a double-inclined three-way piston is arranged on the three-way tube.

Compared with the prior art, the multifunctional single crystal cultivation equipment can realize single crystal cultivation in various different modes, such as various crystallization modes of volatilization crystallization, diffusion crystallization, cooling crystallization and the like, and has high practicability; moreover, the equipment can synchronously develop various different crystallization modes by arranging a plurality of groups of culture devices, thereby improving the efficiency of single crystal culture; furthermore, the utility model discloses a multi-functional single crystal cultivation equipment can carry out the evacuation and fill nitrogen gas and handle whole cultivation system through setting up anhydrous anaerobic operating system, consequently to the poor stability's sample, can develop the single crystal through the protection of nitrogen gas and cultivate for the application scope that the single crystal was cultivateed is more extensive.

As optimization, the tubule is the slope setting, just the position of B sample cell and tubule intercommunication compares A sample cell and tubule intercommunication and wants the height. The position design of the height difference between the sample tube A and the sample tube B is more favorable for the upward movement of gas in the volatilization crystallization, diffusion crystallization or cooling crystallization processes.

Preferably, the sample tube A and the sample tube B are both sealed by screw plugs. The spiral plug has strong sealing performance, so that in the process of single crystal culture, a better pipe opening sealing effect can be achieved by using the spiral plug, the external gas is prevented from entering to influence the crystallization, the spiral plug does not have the hidden danger of oxidation, the growth of crystals in a sample tube is not influenced, and the quality of single crystal culture is ensured; in addition, the spiral plug is low in price and beneficial to controlling the cost.

And preferably, a D valve is arranged on the thin tube. When crystals appear in the culture process, the D valve can be controlled to control the aperture size so as to adjust the crystallization speed, so that the crystals can grow to proper size, and the single crystal culture efficiency is ensured.

And optimally, a camera is arranged on the inner wall of the temperature control box and is connected with a computer. At the moment, a worker can observe the growth state of the crystal in the culture process through the camera, and can adjust the growth state of the crystal in time when feeling that the growth state of the crystal is not correct or has defects, so that the efficiency and the quality of single crystal culture are improved; and set up just need not the staff to watch on the device side constantly after the camera and observe, practiced thrift manpower resources.

Drawings

FIG. 1 is a schematic structural view of a multifunctional single crystal growing apparatus of the present invention;

FIG. 2 is a schematic structural view of a double-inclined three-way piston in the multifunctional single crystal cultivation apparatus of FIG. 1.

The labels in the figures are: 1-anhydrous anaerobic operation system, 11-double-row pipe, 111-A pipe, 112-B pipe, 12-vacuumizing device, 13-nitrogen tank, 14-tail gas receiving device, 15-A valve, 16-B valve and 17-C valve; 2-culture device, 21-A sample tube, 22-B sample tube, 23-tubule, 24-spiral plug and 25-D valve; 3-temperature control box; 4-three-way pipe, 41-double inclined three-way piston; 5-camera.

Detailed Description

The following description is made with reference to the accompanying drawings and examples, but not to be construed as limiting the invention.

Referring to fig. 1 and 2, the multifunctional single crystal cultivation apparatus of the present invention comprises an anhydrous oxygen-free operation system 1, a temperature control box 3 (a temperature controller can be optionally installed inside the temperature control box 3 to adjust the temperature; a water inlet and outlet interface is also arranged on the temperature control box 3 to be connected with a temperature control water pump and adjust the temperature through the temperature control water pump), and a plurality of groups of cultivation devices 2 (the number of the cultivation devices 2 can be set according to the needs of the user, and the number of the cultivation devices 2 in this embodiment is 3 groups); the culture device 2 is arranged in the temperature control box 3; the anhydrous and anaerobic operation system 1 comprises a double-row pipe 11, a vacuumizing device 12, a nitrogen tank 13 and a tail gas receiving device 14, wherein the double-row pipe 11 comprises an A pipe 111 and a B pipe 112; the pipe A111 is communicated with the vacuumizing device 12 through a valve A15, one end of the pipe B112 is communicated with the nitrogen tank 13 through a valve B16, and the other end of the pipe B is communicated with the tail gas receiving device 14 through a valve C17; the culture device 2 comprises an A sample tube 21 and a B sample tube 22, wherein the A sample tube 21 is communicated with the B sample tube 22 through a tubule 23; the sample tube B22 is respectively communicated with the tube A111 and the tube B112 of the double-row tube 11 through a three-way tube 4, and a double-inclined three-way piston 41 is arranged on the three-way tube 4.

As a specific example: the tubule 23 is obliquely arranged, and the position of the B sample tube 22 communicated with the tubule 23 is higher than the position of the A sample tube 21 communicated with the tubule 23. The position design of the height difference between the sample tube A21 and the sample tube B22 is more beneficial to the upward movement of the gas in the volatilization crystallization, diffusion crystallization or cooling crystallization process.

As a specific example: the sample tube A21 and the sample tube B22 are both sealed by screw plugs 24. The spiral plug 24 has strong sealing performance, so that in the process of single crystal culture, the spiral plug 24 can achieve better pipe opening sealing effect, prevent external gas from entering and influencing crystallization, and the spiral plug 24 has no hidden trouble of oxidation, cannot influence the growth of crystals in a sample tube, and ensures the quality of single crystal culture; in addition, the plug screw 24 is inexpensive, which is advantageous for cost control.

As a specific example: the thin tube 23 is provided with a D valve 25. When crystals appear in the process of single crystal cultivation, the D valve 25 can be controlled to control the pore size of the thin tube 23 so as to adjust the crystallization speed, so that the crystals can grow to a proper size, and the single crystal cultivation efficiency is ensured.

As a specific example: the inner wall of the temperature control box 3 is provided with a camera 5, and the camera 5 is connected with a computer. At the moment, a worker can observe the growth state of the crystal in the culture process through the camera 5, and can adjust the growth state of the crystal in time when the growth state of the crystal is not correct or defects exist, for example, the optimal conditions required by culturing different single crystals can be achieved by controlling corresponding conditions, and the efficiency and the quality of single crystal culture are improved; and set up camera 5 after just not needing the staff to watch on the device side constantly and observe, practiced thrift manpower resources.

The experimental process of single crystal culture comprises the following steps:

firstly, opening the valve A15, closing the valve B16 and the valve C17, rotating a double-inclined three-way piston 41 on the three-way pipe 4 to communicate the whole culture device 2 with the vacuumizing device 12, and vacuumizing; after a period of time, closing the valve A15, stopping vacuumizing, slowly opening the valve B16 and the valve C17, and rotating a double-inclined three-way piston 41 on the three-way pipe 4 to communicate the whole culture device 2 with the nitrogen tank 13; the operation is repeated for many times like this, and the air in the whole system is replaced as much as possible. After the replacement is finished, only the valve B16 is opened, and the double-inclined three-way piston 41 on the three-way pipe 4 is rotated, so that the whole culture device is communicated with the nitrogen tank 13, the nitrogen is kept to be released continuously, and the whole system is in a nitrogen protection state.

Then, the single crystal is grown, and depending on the crystallization method, the crystallization method may be a volatile crystallization method, a diffusion crystallization method, a cooling crystallization method, or the like, or different crystallization methods may be performed simultaneously. A volatilization crystallization method, wherein a proper amount of sample solution is added into the sample tube A21, the height of the sample solution is not more than the height of the position of the tubule 23, then the sample tube A21 is sealed by a screw plug 24, and the temperature is set by a temperature control box 3 (the temperature can be set to about 40 ℃); the D valve 25 is adjusted to control the aperture size of the thin tube 23 so as to control the speed of the volatilization crystallization. A diffusion crystallization method, wherein a proper amount of diffusion solvent is added into the sample tube A21, a proper amount of sample solution is added into the sample tube B22, the heights of the diffusion solvent and the sample solution are not more than the height of the position where the tubule 23 is located, then the sample tube A21 and the sample tube B22 are sealed through the screw plug 24, and the temperature is set through the temperature control box 3 (the temperature can be set to be about 40 ℃); the D valve 25 is adjusted to control the aperture size of the thin tube 23 so as to control the speed of the volatilization crystallization. A cooling crystallization method, wherein a proper amount of sample solution is added into the sample tube A21, so that the sample solution does not exceed the height of the position where the thin tube 23 is located, then the sample tube A21 and the sample tube B22 are sealed through the screw plug 24, and the temperature is set through the temperature control box 3 (the temperature is set to about 70 ℃, then the temperature is reduced to about 30 ℃ according to a certain cooling speed, and crystals are obtained through temperature cooling); the D valve 25 is adjusted to control the aperture size of the thin tube 23 so as to control the speed of the volatilization crystallization.

The above general description of the invention and the description of its specific embodiments in this application should not be construed as limiting the scope of the invention. Those skilled in the art can add, reduce or combine the technical features disclosed in the general description and/or the specific embodiments (including the examples) to form other technical solutions within the scope of the present application according to the disclosure of the present application without departing from the components of the present invention.

Claims

1. A multifunctional single crystal cultivation device is characterized in that: comprises an anhydrous anaerobic operating system (1), a temperature control box (3) and a plurality of groups of culture devices (2); the culture device (2) is arranged in the temperature control box (3); the waterless and anaerobic operation system (1) comprises a double-row pipe (11), a vacuumizing device (12), a nitrogen tank (13) and a tail gas receiving device (14), wherein the double-row pipe (11) comprises an A pipe (111) and a B pipe (112); the pipe A (111) is communicated with a vacuumizing device (12) through a valve A (15), one end of the pipe B (112) is communicated with a nitrogen tank (13) through a valve B (16), and the other end of the pipe B is communicated with a tail gas receiving device (14) through a valve C (17); the culture device (2) comprises an A sample tube (21) and a B sample tube (22), and the A sample tube (21) is communicated with the B sample tube (22) through a thin tube (23); the sample tube B (22) is respectively communicated with the tube A (111) and the tube B (112) of the double-row tube (11) through a three-way tube (4), and a double-inclined three-way piston (41) is arranged on the three-way tube (4).

2. The multifunctional single crystal cultivation apparatus of claim 1, wherein: the thin tube (23) is obliquely arranged, and the position of the communication between the sample tube B (22) and the thin tube (23) is higher than the position of the communication between the sample tube A (21) and the thin tube (23).

3. The multifunctional single crystal cultivation apparatus of claim 2, wherein: the sample tube A (21) and the sample tube B (22) are sealed through screw plugs (24).

4. The multifunctional single crystal cultivation apparatus of claim 1, wherein: and a D valve (25) is arranged on the thin tube (23).

5. The multifunctional single crystal cultivation apparatus of claim 1, wherein: the inner wall of the temperature control box (3) is provided with a camera (5), and the camera (5) is connected with a computer.