High-flux experiment liquid preparation system and method for catalytic materialTechnical Field
The invention relates to the field of a high-flux experimental preparation method system for a catalytic material, in particular to a high-flux pipetting mechanism and method and a high-flux preparation system for the catalytic material.
Background
High throughput pipetting mechanisms are extremely useful as fine research tools for laboratory personnel and are one of the basic operations for each study. At present, liquid transferring guns are mostly used in the processes of reagent proportioning and titration, the liquid taking and discharging processes of the instruments need manual operation, and the problems of liquid leakage, forgetting to rinse and the like easily occur. The invention aims at the fact that high-flux proportioning catalytic materials need 4-8 groups of auxiliary agents to prepare 25 different groups of mixed liquid for experiments, but high-flux proportioning is complex at present, liquid preparation processes are complex, multiple components need to be prepared through successive liquid extraction and titration, the volume of the prepared liquid required by titration for each liquid extraction is small, the prepared liquid cannot be stored, and the prepared liquid is only 2-6ml generally. Join in marriage the unable stirring of liquid, and the precision can not effectively be guaranteed, and can not provide the former stirring of joining in marriage the liquid, hardly get the control when joining in marriage the liquid and get the liquid volume to join in marriage that the liquid is accomplished back gained and can not carry out even stirring and evenly adhere to on the carrier to the accuracy nature of experimental result can not be guaranteed. Therefore, an automatic reagent proportioning workstation which is accurate in quantification, high in control precision, strong in working reliability, high in intelligent degree, capable of stirring for multiple times, economical and reasonable is constructed, and practical research significance and application value are achieved.
Disclosure of Invention
Aiming at the problems, the invention provides a mechanism and a method for stirring, taking and storing an auxiliary agent, a mechanism and a method for accurately preparing liquid with high flux and stirring mixed liquid, and a high-flux preparation system of a catalytic material.
The invention provides a high-flux liquid distribution system, which comprises a uniform mixing device (3), a liquid distribution test tube rack (4), a liquid distribution test tube (5), an accurate liquid taking and discharging mechanism (6), a plurality of auxiliary agent beakers (7), a magnetic stirring device (8) and a monitoring system, wherein the uniform mixing device is arranged on the upper surface of the auxiliary agent beaker; the auxiliary agent beakers (7) are placed on the magnetic stirring device (8), and the liquid preparation test tubes (5) are placed in the liquid preparation test tube rack (4) and are placed on the uniform mixing device (3) together;
the accurate liquid taking and discharging mechanism (6) comprises two first sliding blocks (111), two first lead screws (112), two first lead screw sliding tables (11), two first supports (12), a second support (14), a first cross beam (18), a second sliding block (151), a second lead screw (152), a second lead screw sliding table (15), a plurality of third lead screw sliding blocks (161), a plurality of third lead screws (162), a plurality of third lead screw sliding tables (16), a power part (comprising a motor and the like) and a liquid taking part (17);
the two first screw rod sliding tables (11) are arranged in parallel at intervals along a first direction A, and each first screw rod sliding table (11) is provided with a first sliding block (111) and a first screw rod (112); a first support (12) along a third direction C is fixed on each first sliding block (111), a second support (14) along a second direction is fixed between the top ends of the two first supports (12), a second lead screw sliding table (15) along the second direction is fixed on each second support (14), and each second lead screw sliding table (15) is provided with a second sliding block (151) and a second lead screw (152); the first cross beam (18) is fixed on the second sliding block (151) along a first direction A; a plurality of third screw rod sliding tables (16) which are parallel and are arranged along a third direction C are fixedly distributed on the surfaces of the two sides of the first cross beam (18), each third screw rod sliding table (16) is provided with a third screw rod sliding block (161) and a third screw rod (162), and meanwhile, each third screw rod sliding block (161) is also fixedly provided with a liquid taking part (17) along the third direction C; the matching relationship among the corresponding screw sliding table, the corresponding sliding block and the corresponding screw is as follows: the lead screw sliding table is provided with a guide rail along the corresponding length direction, the lead screw is parallel to the guide rail, the lead screw penetrates through the sliding block, the sliding block is matched with the guide rail and can freely slide along the guide rail, a lead screw pair structure is formed between the lead screw and the sliding block, and the sliding block can be driven to slide along the guide rail through the rotation of the lead screw; the first direction A is marked as an x-axis direction, the second direction B is marked as a y-axis direction, the third direction C is marked as a z-axis direction, and every two directions are perpendicular to each other; the uniform mixing device (3), the liquid preparation test tube rack (4), the liquid preparation test tube (5), the multiple auxiliary agent beakers (7) and the magnetic stirring device (8) are all positioned between the two first lead screw sliding tables (11) and below the second support (14); each lead screw is controlled to rotate by a motor; the liquid taking part (17) is preferably an injector with a downward needle, and the injector is matched with a corresponding stepping motor for use; or the liquid taking part (17) is: the injection pump (not shown in the figure) is connected to the upper part of the hose to provide power for liquid in the hose;
the uniform mixing device (3) comprises a lower workbench (31), a direct current motor (32) with a rotating shaft along a third direction, a motor flange plate (33) with a hole in the middle, three rocker arms (34), two optical axes (35), an upper workbench (36), three short shafts (37), two bearing seats and a bearing (38); the rocker arm (34) is of a flat plate structure with two axially parallel but perpendicular flat plate holes, namely a hole A and a hole B, and a space is arranged between the two holes; the direct current motor (32) is fixed on the lower workbench (31), a motor flange sheet (33) with a hole in the middle is positioned on the direct current motor (32), the rotating shaft of the direct current motor (32) vertically faces the hole of the motor flange sheet (33), and the motor flange sheet (33) is fixed with the lower workbench (31); the rotating shaft of the flow motor (32) is coaxially fixed with a hole A of a rocker arm, a short shaft (37) is coaxially inserted into another hole B, the hole B and the short shaft (37) can rotate relatively, and the top end of the short shaft (37) is fixed with the lower surface of the upper workbench (36); the top ends of the other short shafts (37) are respectively fixed with the lower surface of the upper workbench (36), the lower ends of the other short shafts are respectively and correspondingly inserted into a hole B of a rocker arm, the hole B and the correspondingly inserted short shaft (37) can rotate relatively, the upper end of an optical axis (35) is coaxially inserted and fixed in a hole A of the corresponding rocker arm, the lower end of the corresponding optical axis (35) is coaxially inserted and fixed in a bearing (38), and the bearing (38) is fixed on the lower workbench (31) through a bearing seat; three short shafts (37) are distributed in a triangular shape below the lower workbench (31).
The monitoring system comprises respective control elements or control devices for controlling the motor corresponding to the lead screw, the injection pump or the stepping motor and the direct current motor (32).
The test method comprises the following steps:
respectively placing the raw materials in different auxiliary agent beakers after preparation; the control device controls a piston connected with an injection pump or a stepping motor in the liquid taking part to do reciprocating motion, the injection pump or the piston is pulled to absorb liquid obtained in the auxiliary beaker and store the liquid in the injector, the control device controls a motor corresponding to the lead screw so as to control the injector to move along the directions of an x axis, a y axis and a z axis, the needle head of the injector reaches a corresponding liquid preparation test tube, and then the injection pump pushes the piston of the injector to titrate the liquid outwards through the control device;
respectively sucking auxiliary agents with different components from a plurality of auxiliary agent beakers, and storing the auxiliary agents in the injectors in mutually independent storage;
respectively transferring the mixture into a plurality of liquid preparation test tubes from an injector according to the component proportion designed by the experiment to mix so as to obtain a mixed liquid with a plurality of different component proportions,
the corresponding motor and the injection pump are accurately controlled through timer interruption in the liquid suction and discharge process to ensure the liquid taking and discharging amount and the accuracy of the experimental result.
The uniform mixing device is controlled to shake up the mixed solution, and the mixed solution is attached to the carrier when the carrier is placed in the solution preparation test tube (5).
The invention provides a high-flux preparation system of a catalytic material, which comprises a high-flux liquid distribution mechanism, a configuration mechanism and a platform monitoring system, wherein the configuration mechanism is used for obtaining the catalytic material with higher evaluation on the high-flux liquid distribution mechanism, and the platform monitoring system is used for carrying out dosage monitoring and real-time liquid distribution display on the catalytic material with high-flux ratio in the configuration mechanism.
The invention also provides a horizontal rotation oscillation system prepared from the high-flux catalytic material, which comprises a shaking table driven by the motion of a motor controlled by an upper computer to horizontally rotate and oscillate by the mixed liquid after the high-flux catalytic material is proportioned, so that the prepared catalytic material is driven to be fully shaken uniformly and attached to carriers such as alumina and the like.
Compared with the prior art, the high-flux liquid distribution mechanism disclosed by the invention can be used for automatically distributing liquid at high flux and automatically taking liquid in a three-dimensional direction, is high in automation degree, can be used for simultaneously configuring mixed liquid with various different component distribution ratios so as to meet the requirements of high-flux different components on liquid distribution as required, and can be used for accurately controlling the liquid taking and discharging amount by monitoring the work of the motor through the platform monitoring system, so that the accuracy of an experimental result is ensured.
In addition, the accurate liquid preparation mechanism is also provided with a liquid assisting device and a prepared uniform catalytic material mixing device, so that the obtained liquid is mixed more fully, and the experimental result is more accurate.
Compared with the prior art, the high-flux liquid preparation method can be used for simultaneously preparing the mixed liquid with different component proportion ratios, meets the requirement of high-flux proportioning catalytic materials, accurately controls the liquid taking and discharging amount by monitoring the work of the motor through the platform monitoring system, and ensures the accuracy of experimental results.
Compared with the prior art, the high-flux preparation system for the catalytic material can be used for automatic high-flux liquid preparation and liquid taking by moving in the three-dimensional direction, is high in automation degree, can meet the requirement of high-flux proportioning through the preparation of mixed liquid with various components in proportion, and can accurately control the liquid taking and discharging amount by monitoring the work of the motor through the platform monitoring system, so that the accuracy of an experimental result is ensured.
Compared with the prior art, the horizontal rotation oscillation system can fully shake the mixed liquid before liquid taking and after liquid discharging, meets the requirement of high-flux proportioning of the mixed liquid, accurately controls the liquid taking and discharging amount by monitoring the work of the motor through the platform monitoring system, and ensures the accuracy of experimental results.
Drawings
FIG. 1 is a schematic view of a high throughput dispensing configuration of a first embodiment of the present invention;
FIG. 2 is a schematic view of an electrical connection module of the precise liquid-fetching mechanism according to the first embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a first apparatus according to a first embodiment of the present invention;
FIG. 4 is a schematic view of a three-direction slide table structure of the first apparatus according to the first embodiment of the present invention;
FIG. 5 is a schematic view of a liquid-dispensing horizontal rotation oscillation structure according to a first embodiment of the present invention;
FIG. 6 is a flow chart of a high-throughput liquid dispensing method according to a second embodiment of the present invention.
High flux experiment joins in marriage liquid system 1,workstation 2, homogeneous mixing device 3, join in marriage liquid test-tube rack 4, join in marriage liquid test tube 5, theliquid mechanism 6 of putting is got to accurate liquid, auxiliary agent beaker 7,magnetic stirring device 8,first slider 111,first lead screw 112, first lead screw slip table 11,first support 12,second support 14,first crossbeam 18,second slider 151,second lead screw 152, second lead screw slip table 15, thirdlead screw slider 161, a plurality ofthird lead screw 162, third lead screw slip table 16, getliquid 17,lower workstation 31, a directcurrent motor 32, amotor flange piece 33, threerocking arm 34, twooptical axes 35, an upper table 36, threeminor axis 37.
Detailed Description
In order to make the purpose, technical solution and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
Referring to fig. 1, a high throughput pipetting mechanism 1 according to a first embodiment of the present invention includes aworktable 2, a uniform mixing device 3, a solution preparation test tube rack 4, a solution preparation test tube 5, an accurate solution taking anddischarging mechanism 6, a plurality of auxiliary agent beakers 7, amagnetic stirring device 8, and a platform monitoring system. The auxiliary agent beakers 2, the liquid preparation test tubes 5, the accurate liquid taking anddischarging mechanism 6, the control device (not shown) and the uniform mixing device 3 are all arranged on theworkbench 2. As a simplification, the working table 2 can be omitted, and the auxiliary agent beaker 7, the liquid preparation test tube 5, the liquid taking and discharging device 3, the control device and the uniform mixing device 3 are arranged on a bearing plane.
The plurality of auxiliary agent beakers 7 are used for storing stock solutions with different components independently, and the plurality of solution preparation test tubes 5 are used for storing a plurality of mixed solutions obtained by mixing the stock solutions with different components sucked in the auxiliary agent beakers 7 according to different component preparation ratios independently.
The platform monitoring system generally consists of an upper computer monitoring PC. Referring to fig. 2, the platform monitoring system is connected to a control device, the three-dimensional control element of the liquid taking and discharging mechanism is connected to the control device, the control device can feed back the rotation speed of the motor and the height of the liquid level ascending and descending through an autonomous design algorithm according to the movement distance of the sliding block in the three-dimensional direction, and the control device can control the working state of the motor in the three-dimensional direction according to the feedback of the platform monitoring system. The control device is preset with a preset value of liquid level descending height calculated according to the pre-fetching calculated liquid amount, the platform monitoring system sends a pulse signal to the control device, the control device controls the liquid fetching anddischarging device 6 to fetch liquid in the auxiliary agent beaker according to the signal, when the control device stops sending the pulse signal, the liquid fetching device stops fetching liquid, and the platform monitoring system displays the descending liquid level height and the liquid fetching amount of the liquid fetching device in real time. When the liquid is taken, the control device transmits an electric signal to each control element to control the position and the moving speed of the sliding block, the liquid taken from the auxiliary agent beaker is stored in the injection pump, the liquid taking and discharging device is controlled to match the taken liquid according to the grouping of experimental design, the injection pump is controlled to move above each liquid preparation test tube according to the setting of the platform monitoring system, the auxiliary agent is titrated into the liquid preparation test tubes by controlling the injection pump to inject the preset liquid amount, and the liquid in each injection pump is stored independently. It will be appreciated that the control module may also control the rate and location of the draw of the dope from the additive beaker by the tapping means 6. The platform monitoring system can also be provided with component proportion of various experimental designs, and the control device controls the liquid takingdevice 6 to accurately absorb stock solutions with different components from different auxiliary agent beakers according to the component proportion of each group of experimental designs, so that automatic liquid distribution is realized.
The volume of the auxiliary agent beaker 7 is 3-5 times of the volume of the liquid preparation test tube 5, the diameter of theauxiliary agent beaker 2 is 50-55mm, and the diameter of the liquid preparation test tube 5 is 28-38 mm. Preferably, the aid beaker 7 is a container with a volume of 20ml, and the number of the aid beaker is 4-8 so as to store the aid. The liquid preparation test tubes 5 are containers with the diameter of 35ml and the volume of 25ml, and the number of the liquid preparation test tubes is 25, so that 25 screens with different proportions can be simultaneously carried out, and the preparation requirement of high flux is met. The beaker auxiliary agent has a slightly larger volume so as to provide enough auxiliary agent for high-flux liquid preparation, and the liquid preparation test tube has a smaller volume than the beaker auxiliary agent so as to ensure that the liquid level height changes more sensitively, and the liquid level height can monitor and feed back when finding slight changes in time, thereby ensuring that the result is more accurate. As a deformation, the volume and the number of the auxiliary agent beakers and the liquid preparation test tubes can be designed according to the experimental requirements.
Referring to fig. 3, the precise liquid taking anddischarging device 6 includes twofirst sliders 111, twofirst screws 112, two first screw sliding tables 11, twofirst brackets 12, twofirst corner connectors 13, asecond bracket 14, afirst cross beam 18, asecond slider 151, twosecond screws 152, a second screw sliding table 15, eightthird screw sliders 161, eightthird screws 162, eight third screw sliding tables 16, a power component, and a liquid takingcomponent 17. Thefirst beam 18 is fixed to thesecond slider 15/1 along the first direction a, and the fastening connection between the first beam and thesecond slider 15/1 can be a screw connection, a welding connection, a riveting connection or an adhesive connection. The eight groups of third sliding blocks are respectively fixed on the surfaces of the two sides of the first cross beam in an array mode and fixed with the third screw rod sliding table along the third direction, and the third sliding blocks are connected with the first cross beam in a screw fastening mode. Therefore, the third slide table 16 can move in the first direction a, the second direction B and the third direction C, so as to facilitate the taking and placing of the liquid in a wide range.
Please refer to fig. 4. Two first lead screw slip tables 11 interval sets up onworkstation 2, and the axial direction of first lead screw slip table 11 is first direction A. Through the first screw sliding table 11, the firstscrew sliding block 111 and the first screw are formed into a screw pair through threads (or balls) to realize linear reciprocating motion. In the same way, thesecond slider 151, the twosecond lead screws 152 and the second lead screw sliding table 15 realize linear reciprocating motion, and the thirdlead screw slider 161, thethird lead screw 162 and the third lead screw sliding table 16 realize linear reciprocating motion.
The power part comprises 11 stepping motors, and the corresponding lead screws are connected with the power part through shaft couplings to drive the lead screws to rotate. Get and put liquid spare 17 and include syringe needle and hose, glue respectively to connect to 8 third slip table backs along the third direction to guarantee the liquid flow direction. The upper part of the hose is connected with a syringe pump (not shown) for providing power for the liquid in the hose.
Referring to fig. 5, the first embodiment of the present invention further provides a liquid preparation horizontal rotation oscillation uniform mixing device 3. The liquid distribution horizontal rotation oscillation uniform mixing device 3 comprises alower workbench 31, a directcurrent motor 32, amotor flange plate 33, threerocker arms 34, twooptical axes 35, anupper workbench 36, threeshort shafts 37, and two bearing seats and bearings 28. The stepping motor is connected with the control device through a control element, the pulse number of the stepping motor is controlled, the rotating speed of the motor is further controlled, and the motor and the bearing seat are fixedly connected in a mode that screws are connected on the working table top of the uniform mixing device 3. The motor shaft passes in the rocker hole and through holding screw fixed, and the bearing is embedded to the bearing frame in, and its cooperation mode is clearance fit. The optical axis and the rocker arm are connected by a set screw. Controlling means control motor rotates, and motor shaft connecting rocking arm is circular motion around the motor axial to drive other two rocking arms and be synchronous circular motion, thereby drive the horizontal rotation of workstation and vibrate, go up the workstation and be connected with joining in marriage the liquid test tube, both fastening connection's mode can be screw connection, welding, riveting or splice.
Referring to fig. 6, the second embodiment of the present invention further provides a high-throughput liquid distribution method, which uses the high-throughput liquid distribution mechanism 1 as described above, and the high-throughput liquid distribution method includes the following steps:
step S1: and uniformly stirring the beaker auxiliary agent in a mechanical stirring manner, a magnetic stirring manner, an ultrasonic stirring manner or a manual stirring manner. Preferably, the stirring mode of the beaker auxiliary agent is selected from magnetic stirring.
Step S2: the auxiliary agents with different components are respectively sucked from a plurality of beakers and stored in a plurality of injection pumps independently.
Step S3: according to a plurality of component distribution ratios designed by the platform monitoring system, different component auxiliaries sucked in the injection pump are titrated into a liquid preparation test tube according to preset auxiliaries and are mixed to obtain mixed liquid with a plurality of different component distribution ratios, and the component ratios of catalytic components obtained in each liquid preparation test tube are different from each other.
In the process of suction titration, the stepping motor is accurately controlled, the rotating speed and the number of pulses of the motor are monitored in the platform monitoring system, and meanwhile, the platform monitoring system displays the working state of the feedback motor in real time so as to realize accurate control of liquid taking and discharging amount.
Preferably, the high-throughput liquid preparation method may further include step S4;
step S4: and (3) uniformly mixing, namely uniformly mixing the mixed solution, wherein the uniform stirring mode can be mechanical stirring, magnetic stirring, ultrasonic stirring or manual stirring. Preferably, the means of uniform mixing is selected from mechanical stirring.
The invention also provides a high-flux preparation system of the catalytic material. The high-throughput pipetting mechanism 1 is adopted, and in the embodiment, the high-throughput pipetting mechanism 1 comprises 8 auxiliary agent beakers 7 with the volume of 20ml, 8 syringe pumps and 25 liquid preparation test tubes 5 with the diameter of 35ml and the volume of 25 ml. The high-flux preparation system of the catalytic material further comprises a configuration mechanism and a testing mechanism, wherein the configuration mechanism is used for carrying out condition configuration on the catalytic material on the mixed liquid obtained by the high-flux liquid distribution mechanism 1, and the testing mechanism is used for carrying out catalytic performance testing on the mixed liquid which is subjected to catalytic material configuration in the configuration mechanism.
For the configuration of the catalytic material, the component screening of the catalytic auxiliary agents with different component distribution ratios is usually carried out simultaneously, the catalytic materials with different ratios can obtain different catalytic performances, a person skilled in the art can select the corresponding component distribution ratios according to the catalytic performance test, the catalytic material is configured according to high flux to realize the attachment of the high flux component carrier, and the catalytic material required to be configured can realize the screening only by a small amount of catalytic material. In the following description, the stock solution refers to an auxiliary agent for preparing a catalytic material, which includes but is not limited to three components of ethylenediamine, silver oxalate and water to be screened, and may also be four or more components, and the auxiliary agents of different components may be prepared into catalytic materials with different properties according to different pre-designed proportions, wherein the auxiliary agents may be directly added into an auxiliary agent beaker, and the auxiliary agents in the beaker are respectively added into a solution preparation test tube in proportion through the proportions. The high-throughput liquid preparation process for preparing the catalytic material in high-throughput manner is described in detail below.
Ethylenediamine, silver oxalate and water were stored independently of each other in 8 additive beakers. And then, absorbing the ethylenediamine, the silver oxalate and the water from the auxiliary agent beaker into a syringe pump, taking the specific quantity distribution according to the component proportion designed in advance through experiments, taking the liquid by using a control device according to the different component proportions designed in advance, titrating the liquid into 25 liquid-distributing test tubes, and mixing the liquid and the test tubes to obtain 25 catalytic materials with different distribution ratios. It can be understood that the control device can control the liquid taking and discharging device to move in the three-dimensional direction, so that automatic proportioning is realized.
The 25 different component ratios can be designed for verifying the influence of the carrier attached by the mixed liquid with different ratios on the catalytic performance or for obtaining large-scale experimental data, such as: in order to verify the influence of a certain catalytic material on the catalytic performance of a certain reaction, 25 groups of different component ratios are designed in advance, and the weight ratio of ethylene diamine, silver oxalate and water is from 1: 1: 1. 1: 1: 2. 1: 2: 2, the preset volume of the catalytic mixed solution is 5ml, and the optimal component proportion is screened out according to the catalytic performance result of the catalytic material after the catalytic mixed solution is attached to the carrier. Because the volume of the catalytic mixed liquid prepared by the ethylenediamine, the silver oxalate and the water required by the test is smaller, the stepper motor needs to be accurately controlled, and the accuracy of the experimental result is ensured.
Compared with the prior art, the high-flux liquid-transferring mechanism can perform automatic high-flux proportioning and liquid taking in the three-dimensional direction, is high in automation degree, can simultaneously perform the preparation of mixed liquid with various different component proportioning ratios, meets the requirement of high-flux screening, and ensures the accuracy of an experimental result through the accurate pulse control of the stepping motor interrupted by the timer.
Additionally, the accurate liquid preparation mechanism is also provided with a magnetic stirring device and a horizontal rotating table uniform mixing device, so that the mixing is more sufficient, and the experimental result is more accurate.
Compared with the prior art, the high-flux liquid transfer method can be used for simultaneously preparing the mixed liquid with a plurality of component distribution ratios, meets the requirement of high-flux screening, and ensures the accuracy of an experimental result through the accurate pulse control of the stepping motor interrupted by the timer.
Compared with the prior art, the high-flux preparation system for the catalytic material can be used for automatically preparing high-flux liquid, can be used for moving liquid taking and discharging in the three-dimensional direction, is high in automation degree, can be used for preparing mixed liquid with various component distribution ratios at the same time, meets the requirement of high-flux screening, and ensures the accuracy of an experimental result through the accurate pulse control of the stepping motor interrupted by the timer.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit of the present invention are intended to be included within the scope of the present invention.