CN212142549U - Hydrothermal-heat treatment automatic experiment platform - Google Patents

Hydrothermal-heat treatment automatic experiment platform Download PDF

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Publication number
CN212142549U
CN212142549U CN202020440659.XU CN202020440659U CN212142549U CN 212142549 U CN212142549 U CN 212142549U CN 202020440659 U CN202020440659 U CN 202020440659U CN 212142549 U CN212142549 U CN 212142549U
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China
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hydrothermal
platform
spiral arm
stand
reaction kettle
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CN202020440659.XU
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Chinese (zh)
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谭兆钧
原现杰
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North China University of Water Resources and Electric Power
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North China University of Water Resources and Electric Power
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Abstract

An object of the utility model is to provide a hydrothermal-automatic experiment platform of heat treatment, including substrate material processing area, weigh hydrothermal district and heat treatment district, still include the stand, use the stand as the centre of a circle, the projection of substrate material processing area, weighing hydrothermal district and heat treatment district is on the same arc surface with the stand as the centre of a circle, is provided with the transportation spiral arm on the stand that substrate material processing area corresponds, transports the spiral arm and winds the stand rotation, and the rotation spiral arm tip is provided with supporting platform, is provided with the electro-magnet on the supporting platform bottom plate; the slicer controller, the hydrothermal reaction kettle heating equipment and the heating equipment of the tube furnace are all electrically connected with the central controller. The utility model discloses with the basement material processing, weigh hydrothermal and the three sub-flow set of thermal treatment as an organic whole, adopt automatic operation, promoted efficiency by a wide margin when improving the precision.

Description

Hydrothermal-heat treatment automatic experiment platform
Technical Field
The utility model belongs to chemistry experiment field specifically relates to a hydrothermal-thermal treatment automation experiment device.
Background
The desire of the public to blue sky and white cloud makes the research of new energy become popular. The Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER) in the field of electrocatalysis are the theoretical basis for preparing hydrogen, fuel cells, lithium air batteries and other next-generation energy sources [13-15], so that the research on various hydrogen evolution and oxygen evolution catalytic materials is also concerned. Such as phosphides, selenides, sulfides, etc., represented by NiCoP, the preparation process of such materials has in common the following "hydrothermal-thermal treatment" scheme, as shown in fig. 1.1 [16-20 ]. The 'hydrothermal-thermal treatment' process has strong universality and high operation standardization degree, so the process is taken as an entry point, an unmanned thinking tide is introduced into an electrocatalysis experiment, and an unmanned 'hydrothermal-thermal treatment' experiment platform is explored and researched.
According to the artificial experimental experience, the 'hydrothermal-thermal treatment' experiment is decomposed into: substrate material treatment, drug treatment, hydrothermal experiment and heat treatment.
The method comprises three steps of processing and cutting a substrate material, cleaning and drying. For example, the preparation of self-supporting hydrogen evolution and oxygen evolution catalysts, nickel foam, copper foam, carbon paper and the like are required as substrate materials. Taking foamed nickel as an example, the hydrothermal experiment can be carried out after cutting, cleaning and drying. Generally, firstly, cutting foamed nickel by using a scissors or a slicing machine, then repeatedly cleaning the foamed nickel by using acetone, dilute hydrochloric acid, distilled water, ethanol and the like, and finally drying the foamed nickel in a vacuum oven to obtain a clean sample, wherein the process of completing the description of two lines in the literature can be completed in 2-3 hours; the reason for this is that the three devices, the slicer, the ultrasonic cleaning machine and the vacuum oven, work independently and require the intervention of researchers to complete the corresponding tasks.
The medicine treatment relates to the weighing of medicines, and for granular medicines, the adhesion degree of the medicines is different, some medicine particles are easy to separate, and some hydrate particles are easy to agglomerate. Weighing is not easy, and particularly when the weight is in milligram order, accurate weighing requires considerable patience. Taking the preparation process of NiCoP as an example, a certain amount of nickel chloride, cobalt chloride, ammonium fluoride and urea are weighed firstly, then distilled water is added and stirred uniformly, and the obtained solution is used for a subsequent hydrothermal experiment. The weighing process has the difficulty that the chemicals are bonded to different degrees, such as urea particles are easy to separate, and ammonium fluoride or some hydrate particles are easy to agglomerate. At present, an accurate weighing device, namely a weighing device with a weight sensor and a display, is adopted, and everyone needs to be very patiently worried when weighing various medicines. The operation time is too long, and the manual influence is large during the operation.
The hydrothermal equipment adopts a reaction kettle.
The heat treatment is generally carried out in a tube furnace. The tube furnaces commonly used at present are novel high-performance high-energy-saving electric furnaces developed by adopting international advanced technology, and have various tube furnace types such as single tube, double tube, horizontal type, openable type, vertical type, single temperature zone, double temperature zone, three temperature zone and the like. The method is mainly applied to experiments and small-batch production of universities and colleges, scientific research institutions, industrial and mining enterprises and the like. The device has the advantages of safety, reliability, simple operation, high temperature control precision, good heat preservation effect, large temperature range, high temperature uniformity of the hearth, multiple temperature zones, optional atmosphere, vacuum-pumping furnace type and the like. A single set point or 30 segment programmable controller may be selected. The energy-saving ceramic fiber material and the double-layer structure can reduce the surface temperature to normal temperature. The temperature equalizing area is long, the operation is simple and convenient, the sealing is reliable, the comprehensive performance index is higher, and the temperature equalizing device is at the leading level in China. The furnace tube can be made of heat-resistant steel, quartz glass, ceramic tube, etc. Use the tube furnace among the heat treatment process, present ordinary tube furnace sets up the quartz capsule including the box that has heating function in the box and holds the chamber, and the box both sides are sealed by sealed ring flange, and the quartz capsule is placed and is held the intracavity at the quartz capsule, and the crucible is placed in the quartz capsule. The quartz tube accommodating cavity of the tube furnace is large, and the crucible is a common crucible, so that only a crucible with a diameter much smaller than the inner diameter of the quartz tube is selected. Taking the preparation of the NiCoP catalyst as an example, the NiCoO nano rod obtained by hydrothermal method is washed and dried, and then is put into a tube furnace together with sodium hypophosphite powder, and the NiCoP hydrogen evolution catalyst is obtained by annealing under the protection of argon. At present, if a common tube furnace is used in the heat treatment process, a crucible containing a sample is difficult to keep stable when being placed in a quartz tube, and sealing flanges on two sides of the quartz tube are difficult to install.
Disclosure of Invention
According to the artificial experimental experience, the 'hydrothermal-thermal treatment' experiment is decomposed into: the method comprises three sub-processes of substrate material treatment, drug treatment, hydrothermal experiment and heat treatment, and a sub-process module is designed according to a modularization idea to independently complete the tasks.
An object of the utility model is to provide an automatic experiment platform of hydrothermal-heat treatment, with the basement material processing, weigh hydrothermal and the three sub-flow set of heat treatment as an organic whole, adopt automatic operation, promoted efficiency by a wide margin when improving the precision.
The purpose of the utility model is realized with the following mode:
a hydrothermal-thermal treatment automatic experiment platform comprises a substrate material treatment area, a weighing hydrothermal area, a thermal treatment area and an upright post, wherein the upright post is used as a circle center, the projections of the substrate material treatment area, the weighing hydrothermal area and the thermal treatment area are arranged on the same arc surface which takes the upright post as the circle center, a transfer spiral arm is arranged on the upright post corresponding to the substrate material treatment area, the transfer spiral arm rotates around the upright post, a supporting platform is arranged at the end part of the transfer spiral arm, and an electromagnet is arranged on a bottom plate of the supporting platform; the base material processing area comprises an oven, the oven is a vacuum oven, a slicer, a transmission device and a cleaning device are arranged in the vacuum oven, the transmission device is arranged in the oven at the lower part of the slicer, the cleaning device is arranged in the oven corresponding to a discharge port of the transmission device, the slicer is arranged on the wall of the vacuum oven, a feed port is arranged on the wall corresponding to the slicer, a sealing cover is arranged at the feed port, the slicer comprises a slicing platform, the slicing platform is arranged on the rear wall of the vacuum oven, a notch is arranged on the slicing platform, a cutting tool is arranged at the upper part corresponding to the notch and is arranged on the rear wall of the vacuum oven through a telescopic device, a first photoelectric sensor is arranged at the lower part of the side surface of the cutting tool close to the ultrasonic cleaning device, a solution injection port is arranged at the top part of the vacuum oven corresponding to the cleaning, the liquid discharge pipe extends out of the vacuum oven, the cleaning device is an ultrasonic cleaning machine, a reticular supporting platform is further arranged in a cleaning tank of the ultrasonic cleaning machine and comprises a supporting frame, the supporting frame comprises a top plate and a bottom frame, the same sides of the top plate and the bottom frame are fixedly connected through two supporting columns, a net plate is hinged to the bottom frame end far away from the supporting columns, a steel wire rope is fixed to the net plate end close to the supporting columns, the top of the steel wire rope is connected to an electric hoist, the electric hoist is fixed to the lower surface of the top plate, the top plate of the supporting frame is arranged right below an electromagnet and is a permanent magnet, the magnetism of the permanent magnet is attracted to the magnetism of the electromagnet, and a slicer driving device, a first photoelectric sensor of a slicer, a gravity sensor, an ultrasonic generator of the ultrasonic cleaning device and the vacuum oven and the; the weighing hydrothermal area comprises weighing equipment and a hydrothermal reaction kettle, the hydrothermal reaction kettle is arranged on the stand column through a spiral arm, the heat treatment area is provided with a tubular furnace, the tubular furnace is arranged on the stand column through the spiral arm, and the slicer controller, the hydrothermal reaction kettle (heating equipment) and the tubular furnace (heating equipment) are electrically connected with the central controller.
According to the hydrothermal-thermal treatment automatic experiment platform, the weighing hydrothermal area is provided with the weighing device and the hydrothermal reaction kettle, and the inner cavity of the hydrothermal reaction kettle is larger than the net-shaped supporting platform.
Above-mentioned hydrothermal-automatic experiment platform of thermal treatment, the bearing is established to the cover on the stand, and the bearing inner circle is fixed on the stand, and bearing outer lane cover is equipped with the rim plate, transports the spiral arm and fixes in the rim plate lower part, still includes gear motor, and the carousel is established to the cover on gear motor's the output shaft, and the carousel meshes with the upper portion of rim plate to realize transporting the spiral arm and rotate around the stand, gear motor is connected with central controller electricity.
According to the hydrothermal-thermal treatment automatic experiment platform, the end part of the transfer spiral arm is also provided with the lifting mechanism, the bottom end of the lifting mechanism is fixed with the electromagnet, and the electromagnet is electrically connected with the central controller.
According to the hydrothermal-thermal treatment automatic experiment platform, the lifting mechanism is an electric push rod or an electric lead screw structure or a hydraulic push rod arranged at the end part of the transfer spiral arm, the electromagnet is fixed at the bottom of the electric push rod or fixed at the bottom of an action piece of the electric lead screw structure or the bottom of the hydraulic push rod, and a motor of the electric push rod or a driving motor of the electric lead screw or a hydraulic oil control part of the hydraulic push rod is electrically connected with the central controller.
The hydrothermal-heat treatment automatic experiment platform comprises the following steps:
a. the method comprises a substrate material treatment process, a water weighing process and a heat treatment process, wherein the substrate material treatment process, the water weighing process and the heat treatment process are firstly arranged, an upright post is installed, projections of the substrate material treatment process, the water weighing process and the heat treatment process are arranged on the same arc surface with the upright post as the center of a circle, the projections of the substrate material treatment process, the water weighing process and the heat treatment process are arranged on the same arc surface with the upright post as the center of a circle, a transfer rotary arm is installed on the upright post corresponding to the substrate material treatment process, the transfer rotary arm rotates around the upright post, a supporting platform;
b. the base material processing procedure is to arrange cutting, cleaning and drying in the same container, namely the drying is a vacuum oven, a slicing machine and an ultrasonic cleaning machine are arranged in the vacuum oven, a reticular supporting platform is arranged in the ultrasonic cleaning machine, a top plate of the reticular supporting platform is a permanent magnet attracted with an electromagnet on the supporting platform, and the base material is sliced on the slicing machine and then is conveyed to a screen plate in a cleaning tank through a conveying device for ultrasonic cleaning;
c. weighing hydrothermal process: the weighing hydrothermal area is provided with a weighing device and a hydrothermal reaction kettle, the weighing device weighs a prepared precursor reagent and then pours the precursor reagent into the hydrothermal reaction kettle, the transfer rotary arm rotates to the upper surface of the ultrasonic cleaning machine to open a power supply of the electromagnet to suck the net-shaped supporting platform, then the transfer rotary arm continuously rotates to the upper surface of the hydrothermal reaction kettle, the reaction kettle is opened, the power supply of the electromagnet is disconnected, a cleaned and dried substrate material falls into the hydrothermal reaction kettle along with the net-shaped supporting platform, then a reaction kettle cover is covered to carry out the hydrothermal reaction of the precursor, a hydrothermal reaction solvent is poured out after the hydrothermal reaction of the precursor, a reagent required for phosphorization is added, the reaction kettle cover is covered to carry out phosphorization, and the reaction;
d. a heat treatment process: and starting an electromagnet power supply to suck the net-shaped supporting platform, then rotating the rotary arm to a crucible in a heat treatment area to be placed, starting the electric hoist, sliding the substrate material subjected to hydrothermal phosphorization into the crucible, and pushing the crucible into a tubular furnace to perform heat treatment.
In the hydrothermal-thermal treatment automatic experiment platform, the second photoelectric switch is arranged at the bottom of the wheel disc corresponding to the transfer spiral arm, the transfer spiral arm drives the cleaned and dried substrate material to rotate, when the reactor is sensed by the second photoelectric switch, the electromagnet is electrified, meanwhile, the electromagnet falls downwards under the action of the lifting mechanism, the falling distance is determined by the positions of the initially installed transfer spiral arm, the reaction kettle and the tubular furnace and then is input into the center to the controller, the falling distance after reaching the reaction kettle is just the current of the electromagnet which is cut off when the falling distance falls into the central controller at the bottom of the reaction kettle, simultaneously starting a lifting mechanism to ascend, after the lifting mechanism removes the electromagnet from the reaction kettle, tightly covering the reaction kettle cover, performing precursor hydrothermal reaction, wherein the time of the precursor hydrothermal reaction is also preset in a controller, and opening the reaction kettle cover after the precursor hydrothermal reaction; similarly, the lifting mechanism is started to descend, the electromagnet is started at the same time, the lifting mechanism ascends after the base material of the precursor hydrothermal reaction is absorbed, the central controller drives the spiral arm to rotate towards the base material area, the second photoelectric switch senses the cleaning device, descends, the net-shaped supporting platform is placed into the ultrasonic cleaning tank for ultrasonic cleaning, the base material is repeatedly conveyed after the ultrasonic cleaning, and the net-shaped supporting platform is conveyed into the reaction kettle again; pouring a phosphating agent into a reaction kettle, covering the reaction kettle cover to perform a phosphating hydrothermal reaction, wherein the reaction time is preset in a controller, after the phosphating reaction, opening the reaction kettle cover, starting a lifting mechanism to fall down, simultaneously starting an electromagnet power supply to enable the electromagnet to suck a net-shaped supporting platform and then ascend, enabling a base material belt after the hydrothermal reaction to leave the reaction kettle, then rotating again, sensing a crucible of the tubular furnace by a photoelectric switch to stop rotating, enabling the electromagnet to be powered all the time in the process, starting the lifting mechanism to enable the net-shaped supporting platform to fall down, wherein the falling distance is preset, controlling the lifting mechanism to fall down by the controller, after falling, pulling a screen plate to rotate by an electric hoist which opens an operator by the controller, enabling the base material after the reaction on the screen plate to slide into the crucible of the tubular furnace, then pushing the crucible into a quartz tube in the tubular furnace, covering an end cover of the tubular furnace, and (4) performing heating treatment.
By adopting the technical scheme, the beneficial effects of the utility model are that:
the shape of the quartz accommodating cavity is consistent with that of the quartz tube, so that the quartz tube can be heated uniformly during heating, and the heat loss is small. The sealing member can be conveniently installed and has good sealing effect. Meanwhile, the shape of the crucible is matched with that of the quartz tube, so that the crucible can be conveniently placed in the quartz tube and is easy to keep stable.
Drawings
Fig. 1 is a diagram of the region treatment of the present invention.
Fig. 2 is a schematic structural diagram of the present invention.
Fig. 3 is the structure schematic diagram of the vacuum drying box after the front wall is deleted.
FIG. 4 is a schematic view of the ultrasonic cleaning machine of FIG. 3 with the front wall removed
Fig. 5 is a schematic structural view of a mesh support platform.
Fig. 6 is a schematic structural view of a mesh support platform.
Fig. 7 is a schematic structural view of the weighing apparatus of the present invention.
FIG. 8 is a schematic structural view of the heat treatment apparatus of the present invention.
FIG. 9 is a schematic view of a sealing door structure of the heat treatment apparatus.
FIG. 10 is a schematic view showing the structure of a crucible for a quartz tube of a heat treatment apparatus.
FIG. 11 is a schematic view of a crucible structure.
Detailed Description
As shown in fig. 1-11, an automatic experimental platform for hydrothermal-thermal treatment comprises a substrate material treatment area a, a weighing hydrothermal area B, a thermal treatment area C, an upright column, and a support platform, wherein projections of the substrate material treatment area, the weighing hydrothermal area and the thermal treatment area are projected on the same arc surface with the upright column as the center of circle, a transfer arm E is arranged on the upright column corresponding to the substrate material treatment area, the transfer arm rotates around the upright column, a support platform F is arranged at the end of the transfer arm, and an electromagnet G is arranged on the bottom plate of the support platform; the base material processing area comprises an oven, the oven is a vacuum oven 9, a slicing machine, a conveying device and a cleaning device are arranged in the vacuum oven, the conveying device 6 is arranged in the oven at the lower part of the slicing machine, the cleaning device 8 is arranged in the oven corresponding to a discharge port of the conveying device, the slicing machine is arranged on the box wall of the vacuum oven, a feed inlet 1 is formed in the box wall corresponding to the slicing machine, a sealing cover is arranged at the feed inlet, the slicing machine comprises a slicing platform, the slicing platform is installed on the rear wall 9 of the vacuum oven, a notch 4 is formed in the slicing platform, a cutting tool 3 is arranged on the upper part corresponding to the notch, the cutting tool is arranged on the rear wall of the vacuum oven through a telescopic device, the cutting tool is fixed at the bottom of a. A first photoelectric sensor H is arranged at the lower part of the side surface of the cutting tool close to the ultrasonic cleaning device, a solution injection port is arranged at the top of the vacuum oven corresponding to the cleaning device, a liquid discharge pipe with a valve is arranged at the bottom of the cleaning device, the liquid discharge pipe extends out of the vacuum oven, the cleaning device is an ultrasonic cleaning machine, still be provided with netted supporting platform 5 in ultrasonic cleaner's the washing tank, netted supporting platform includes support frame 12, the support frame includes roof 13 and underframe, roof and underframe are served with one side through two pillars 14 fixed connection, it has otter board 15 to keep away from the underframe of pillar and articulate, the otter board end that is close to the pillar is fixed with wire rope 16, wire rope's top is connected to on the electric block 17, electric block fixes on the lower surface of roof, the roof board is the permanent magnet, distance between two pillars is greater than the width of conveyer belt, and the conveyer belt discharge gate is just to between two pillars. The reticular supporting platform is a running device, so that the cutting, cleaning and drying of the substrate material can be conveniently carried out. The magnetism of the permanent magnet is attracted with that of the electromagnet, and the slicer driving device, the first photoelectric sensor of the slicer, the gravity sensor, the ultrasonic generator of the ultrasonic cleaning device and the vacuum oven are electrically connected with the electric hoist of the reticular supporting platform; the weighing hydrothermal area comprises weighing equipment and a hydrothermal reaction kettle, the hydrothermal reaction kettle is arranged on the stand column through a spiral arm, the heat treatment area is provided with a tubular furnace, the tubular furnace is arranged on the stand column through the spiral arm, and the slicer controller, the hydrothermal reaction kettle (heating equipment) and the tubular furnace (heating equipment) are electrically connected with the central controller.
The utility model discloses a cover establishes the bearing on the stand, and the bearing inner race is fixed on the stand, and bearing inner race cover is equipped with the rim plate, transports the spiral arm and fixes in the rim plate lower part, still includes gear motor, and the carousel is established to the cover on gear motor's the output shaft, and the carousel meshes with the upper portion of rim plate to realize transporting the spiral arm and rotate around the stand, gear motor is connected with the central controller electricity.
The utility model discloses tip at the transportation spiral arm still is provided with elevating system, elevating system's bottom mounting electro-magnet, the electro-magnet is connected with the central controller electricity.
The utility model discloses an elevating system is for installing electric putter or electric screw structure or hydraulic pressure push rod at the transport spiral arm tip, and the electro-magnet is fixed in the electric putter bottom or is fixed in the bottom of electric screw structure action piece or hydraulic pressure push rod's bottom, and electric putter's motor or electric screw's driving motor or hydraulic pressure push rod's hydraulic oil control part is connected with the central controller electricity.
The working process of the substrate material treatment is as follows:
when needing to cut into slices and wash, the top cap of vacuum drying case is opened, slicer in the vacuum drying case adopts the current slicer sold in the market, the cutting tool and the section platform of slicer all set up in the vacuum drying case, the base material passes through manual work or traction equipment and enters into on section platform 2 through feed inlet 1, the side that the cutting tool is close to ultrasonic cleaning device is provided with photoelectric sensor, photoelectric sensor senses when the base material, controller control slicer drive arrangement cuts the action, cut the base material into required size, fall on conveyer, be provided with gravity sensor in the conveyer, conveyer senses the change of gravity back signal transfer to controller, the controller starts conveyer, the base material after will cutting conveys to ultrasonic cleaning device, the base material enters into ultrasonic cleaning device. When the conveying device senses gravity, the controller prompts the conveying device to convey the substrate material, and when the conveying device does not sense the gravity, the controller controls the conveying device to stop, and simultaneously prompts the ultrasonic cleaning device to perform ultrasonic cleaning, the time of the ultrasonic cleaning is set to be different according to different experiments or working conditions, the cleaning is stopped after the time is up, a valve (an electromagnetic valve) on the liquid discharge pipe is prompted to discharge the cleaning solution, and then the valve is closed. Then the cutting driving device is dismantled, the top cover is covered, the vacuum oven starts to carry out vacuum drying operation, and the drying time can be preset according to experiments or working conditions.
The utility model discloses a weigh hydrothermal district and arrange weighing device and hydrothermal reaction kettle, hydrothermal reaction kettle inner chamber is greater than netted supporting platform, makes things convenient for netted supporting platform business turn over reation kettle.
The utility model discloses a weighing device is automatic reagent weighing platform, including accurate weigher 16-1, the chassis of accurate weigher is embedded to be established weighing transducer, is provided with reagent conveyor 3-1 on the upper portion of chassis, and reagent conveyor includes reagent pipe 4-1 of splendid attire reagent, and the one end of reagent pipe is provided with injector 6-1, and the other end of reagent pipe sets up discharging pipe 2-1, and the pipe diameter of discharging pipe is less than the pipe diameter of reagent pipe, the injector is differential screw mechanism, moves in the reagent pipe by the drive of first actuating mechanism injector to release the discharging pipe with the reagent, fall and weigh on the chassis; the chassis of the weighing device is provided with an adjusting device 12-1, the adjusting device comprises a shell 13-1 covered outside the weighing device, the top of the shell is of a frame structure, one end of the shell is provided with a residue outlet 18-1, a propeller is arranged in the shell and comprises a push rod 15-1, the push rod penetrates through the side surface of the shell and extends into the shell, the end part of the push rod extending into the shell is provided with a push plate 14-1, the bottom surface of the push plate on the horizontal plane and the upper surface of the chassis are in the same plane, the size of the bottom of the push plate is consistent with the size of the upper surface of the chassis, so that when reagents are redundant, the push rod moves towards the accurately weighed chassis and drives the push plate to push medicines on the chassis to move towards the residue outlet, the adjusting device also comprises a second driving mechanism 7-1, and the push rod moves towards the chassis under the driving of the, when the pushing rod is moved continuously, the pushing rod pushes out the reagent on the chassis and falls into a reagent recovery hopper 18-1 arranged right below the excess material outlet. Therefore, the purpose of adjusting the amount of the reagent on the chassis is achieved, the first driving mechanism and the second driving mechanism are electrically connected with the controller, and the further weight sensor is also electrically connected with the controller.
For convenient operation, the injector and the adjusting device of the present invention are respectively arranged on both sides of the precise weighing apparatus, and can also be arranged on the same side.
Furthermore, the adjusting device is a differential screw transmission mechanism, the outer surface of a push rod extending out of the shell is provided with threads, a second driven wheel disc 11-1 is sleeved on the push rod, the second driven wheel disc is in threaded fit with the push rod, a second driving mechanism 7-1 is fixed on a rack 1-1, an output shaft of the second driving mechanism is sleeved with a second driving wheel 8-1, the second driving wheel is meshed with the second driven wheel disc 11-1 through a second driving wheel 10-1, the outer diameter of the second driven wheel disc and the outer diameter of the second driving wheel are both smaller than that of the second driving wheel 10-1, the second driving wheel is arranged on a bearing seat through a bearing, the bearing seat 9-1 is fixed on the rack, the second driven wheel disc 11-1 and the push rod 15-1 form a screw pair, and the second driving wheel 8-1, The second transmission wheel 10-1 and the second driven wheel disc 11-1 form a driving mechanism of the differential screw transmission mechanism.
Furthermore, the injector is a differential screw transmission mechanism and comprises a piston rod 19-1, the end part of the piston rod is provided with a piston matched with the reagent tube, the end part of the reagent tube is provided with an end cover 5-1, a gap is arranged between the piston rod and the end cover or the piston rod and the end cover are in threaded fit, the end cover 5-1 is fixed on the frame 1, the piston rod extends out of the end cover, the piston rod is a screw rod of the differential screw mechanism, the piston rod extending out of the end cover is driven to rotate by a first driving mechanism, the first driving mechanism and a second driving frame have the same structure and are not shown in the figure, the specific structure of the injector comprises a first driven wheel disc which is sleeved on the piston rod extending out of the end cover and is matched with the piston rod, the first driven wheel disc is in threaded fit with the piston rod, the first driven wheel disc and the piston rod form a screw pair of the differential screw transmission mechanism, a, the first driving mechanism is fixed on the rack, the outer diameter of the first driven wheel disc and the outer diameter of the first driving wheel are smaller than the outer diameter of the first driving wheel, the first driving wheel and the first driven wheel disc form a driving mechanism of the differential screw transmission mechanism, the first driving wheel is arranged on a bearing seat through a bearing, and the bearing seat is fixed on the rack.
The utility model discloses be connected by toper pipe 3-1 between 4-1 of reagent pipe and the discharging pipe 2-1, the vertical screenshot of toper pipe is right trapezoid, and the right angle line coincides with the bottom of reagent pipe mutually, and the pipe diameter of toper pipe reduces gradually to the pipe diameter of discharging pipe consistent like this, can enter into the discharge gate when guaranteeing the injector promotes reagent without any stopping, and the discharging pipe diameter is less than the reagent pipe diameter moreover, guarantees that the volume of a ejection of compact is less, the convenient control load.
The specific working process of the automatic weighing device is as follows:
reagent is loaded into the reagent tube, the first driving mechanism is controlled by the controller, so that the piston rod of the injector and the discharge hole move slowly, the reagent is pushed out and falls onto the chassis of the precise weighing device, weight information is displayed on the display of the precise weighing device, meanwhile, the weight information is transmitted to the weighing controller, if the weight is insufficient, the first driving mechanism is inspired to continue working, and if the weight is good, the first driving mechanism is stopped by the controller. If the weight exceeds the required weight, the controller starts a second driving mechanism of the adjusting mechanism to enable the push rod to move towards the chassis and the excess material outlet, so that the reagent in the chassis is pushed to move towards the excess material outlet, part of the reagent is pushed out to fall into the reagent recovery hopper, and when the accurate weighing device displays that the weight is right, the controller stops the second driving mechanism. And finishing the weighing of the reagent.
The utility model discloses a heat treatment device is tube furnace, including last box and lower box, go up and all be provided with the recess in box 1-2 and the lower box 2-2, go up the box and form quartz capsule with the internal recess cooperation of lower box and hold chamber 3-2, all be provided with sealing member in the both sides of the recess of box under, the shape that the quartz capsule held the chamber is unanimous with the quartz capsule shape, sealing member is including the support ring 4-2 of fixing at the box both sides down, and the position of support ring is corresponding with the position that the quartz capsule held the both ends in chamber, installs sealing door 5-2 on the support ring, and sealing door includes end cover 6-2, is provided with on the end cover and holds the breather pipe 7-2 that the chamber communicates with the quartz capsule, and the end cover is threaded connection with the support ring, and the cover is equipped with the.
In order to limit and play a role of dust prevention at the same time, the end cover of the utility model is also provided with a cover plate 9-2, the outer diameter of the cover plate is the same as that of the support ring, and the cover plate completely covers the end part of the support ring.
The end cover of the utility model is also provided with a rotary handle 10-2, which is convenient for installation and disassembly.
The utility model discloses set up quartz capsule 11-2 in the quartz capsule holds the intracavity, place crucible 12-2 in the quartz capsule, the bottom of crucible is the plane shape, the both sides face of crucible be with quartz capsule shape assorted arcwall face, when placing the crucible like this, keep the crucible steady easily, can place into the quartz capsule with the crucible convenient and fast ground moreover.
The experimental method of the hydrothermal-heat treatment automatic experimental platform comprises the following steps:
a. the method comprises a substrate material treatment process, a water weighing process and a heat treatment process, wherein the substrate material treatment process, the water weighing process and the heat treatment process are firstly arranged, an upright post is installed, projections of the substrate material treatment process, the water weighing process and the heat treatment process are arranged on the same arc surface with the upright post as the center of a circle, the projections of the substrate material treatment process, the water weighing process and the heat treatment process are arranged on the same arc surface with the upright post as the center of a circle, a transfer rotary arm is installed on the upright post corresponding to the substrate material treatment process, the transfer rotary arm rotates around the upright post, a supporting platform;
b. the base material processing procedure is to arrange cutting, cleaning and drying in the same container, namely the drying is a vacuum oven, a slicing machine and an ultrasonic cleaning machine are arranged in the vacuum oven, a reticular supporting platform is arranged in the ultrasonic cleaning machine, a top plate of the reticular supporting platform is a permanent magnet attracted with an electromagnet on the supporting platform, and the base material is sliced on the slicing machine and then is conveyed to a screen plate in a cleaning tank through a conveying device for ultrasonic cleaning;
c. weighing hydrothermal process: the weighing hydrothermal area is provided with a weighing device and a hydrothermal reaction kettle, the weighing device weighs a prepared precursor reagent and then pours the precursor reagent into the hydrothermal reaction kettle, the transfer rotary arm rotates to the upper surface of the ultrasonic cleaning machine to open a power supply of the electromagnet to suck the net-shaped supporting platform, then the transfer rotary arm continuously rotates to the upper surface of the hydrothermal reaction kettle, the reaction kettle is opened, the power supply of the electromagnet is disconnected, a cleaned and dried substrate material falls into the hydrothermal reaction kettle along with the net-shaped supporting platform, then a reaction kettle cover is covered to carry out the hydrothermal reaction of the precursor, a hydrothermal reaction solvent is poured out after the hydrothermal reaction of the precursor, a reagent required for phosphorization is added, the reaction kettle cover is covered to carry out phosphorization, and the reaction;
d. a heat treatment process: and starting an electromagnet power supply to suck the net-shaped supporting platform, then rotating the rotary arm to a crucible in a heat treatment area to be placed, starting the electric hoist, sliding the substrate material subjected to hydrothermal phosphorization into the crucible, and pushing the crucible into a tubular furnace to perform heat treatment.
The device is further improved, the second photoelectric switch is arranged at the bottom of the wheel disc corresponding to the transfer rotary arm, the transfer rotary arm drives the cleaned and dried substrate material to rotate, when the reactor is sensed by the second photoelectric switch, the electromagnet is electrified, the electromagnet falls downwards under the action of the lifting mechanism, the falling distance is determined by the positions of the initially installed transfer rotary arm, the reaction kettle and the tube furnace and then is input to the controller, the current of the electromagnet is cut off when the electromagnet falls into the central controller at the bottom of the reaction kettle after reaching the reaction kettle, the lifting mechanism is started to ascend, the cover of the reaction kettle is tightly covered after the electromagnet is removed from the reaction kettle by the lifting mechanism, the hydrothermal reaction of a precursor is carried out, the hydrothermal reaction time of the precursor is also preset in the controller, and the cover of the reaction kettle is opened after the hydrothermal reaction of the precursor; similarly, the lifting mechanism is started to descend, the electromagnet is started at the same time, the lifting mechanism ascends after the base material of the precursor hydrothermal reaction is absorbed, the central controller drives the spiral arm to rotate towards the base material area, the second photoelectric switch senses the cleaning device, descends, the net-shaped supporting platform is placed into the ultrasonic cleaning tank for ultrasonic cleaning, the base material is repeatedly conveyed after the ultrasonic cleaning, and the net-shaped supporting platform is conveyed into the reaction kettle again; pouring a phosphating agent into a reaction kettle, covering the reaction kettle cover to perform a phosphating hydrothermal reaction, wherein the reaction time is preset in a controller, after the phosphating reaction, opening the reaction kettle cover, starting a lifting mechanism to fall down, simultaneously starting an electromagnet power supply to enable the electromagnet to suck a net-shaped supporting platform and then ascend, enabling a base material belt after the hydrothermal reaction to leave the reaction kettle, then rotating again, sensing a crucible of the tubular furnace by a photoelectric switch to stop rotating, enabling the electromagnet to be powered all the time in the process, starting the lifting mechanism to enable the net-shaped supporting platform to fall down, wherein the falling distance is preset, controlling the lifting mechanism to fall down by the controller, after falling, pulling a screen plate to rotate by an electric hoist which opens an operator by the controller, enabling the base material after the reaction on the screen plate to slide into the crucible of the tubular furnace, then pushing the crucible into a quartz tube in the tubular furnace, covering an end cover of the tubular furnace, and (4) performing heating treatment.
What has been described above is only the preferred embodiments of the present invention, and it should be noted that, for those skilled in the art, without departing from the overall concept of the present invention, a plurality of changes and improvements can be made, and these should also be regarded as the protection scope of the present invention, and these will not affect the effect of the present invention and the utility of the patent.

Claims (5)

1. The hydrothermal-thermal treatment automatic experiment platform comprises a substrate material treatment area, a weighing hydrothermal area and a thermal treatment area, and is characterized in that: the device is characterized by further comprising an upright post, wherein the upright post is used as a circle center, the projections of the substrate material processing area, the weighing hydrothermal area and the heat treatment area are arranged on the same arc surface with the upright post as the circle center, a transfer spiral arm is arranged on the upright post corresponding to the substrate material processing area, the transfer spiral arm rotates around the upright post, a supporting platform is arranged at the end part of the transfer spiral arm, and an electromagnet is arranged on a bottom plate of the supporting platform; the base material processing area comprises an oven, the oven is a vacuum oven, a slicer, a transmission device and a cleaning device are arranged in the vacuum oven, the transmission device is arranged in the oven at the lower part of the slicer, the cleaning device is arranged in the oven corresponding to a discharge port of the transmission device, the slicer is arranged on the wall of the vacuum oven, a feed port is arranged on the wall corresponding to the slicer, a sealing cover is arranged at the feed port, the slicer comprises a slicing platform, the slicing platform is arranged on the rear wall of the vacuum oven, a notch is arranged on the slicing platform, a cutting tool is arranged at the upper part corresponding to the notch and is arranged on the rear wall of the vacuum oven through a telescopic device, a first photoelectric sensor is arranged at the lower part of the side surface of the cutting tool close to the ultrasonic cleaning device, a solution injection port is arranged at the top part of the vacuum oven corresponding to the cleaning, the liquid discharge pipe extends out of the vacuum oven, the cleaning device is an ultrasonic cleaning machine, a reticular supporting platform is further arranged in a cleaning tank of the ultrasonic cleaning machine and comprises a supporting frame, the supporting frame comprises a top plate and a bottom frame, the same sides of the top plate and the bottom frame are fixedly connected through two supporting columns, a net plate is hinged to the bottom frame end far away from the supporting columns, a steel wire rope is fixed to the net plate end close to the supporting columns, the top of the steel wire rope is connected to an electric hoist, the electric hoist is fixed to the lower surface of the top plate, the top plate of the supporting frame is arranged right below an electromagnet and is a permanent magnet, the magnetism of the permanent magnet is attracted to the magnetism of the electromagnet, and a slicer driving device, a first photoelectric sensor of a slicer, a gravity sensor, an ultrasonic generator of the ultrasonic cleaning device and the vacuum oven and the; weigh hydrothermal district and include weighing equipment and hydrothermal reaction kettle, hydrothermal reaction kettle passes through the spiral arm setting on the stand, and heat treatment district is provided with the tube-type furnace, and the tube-type furnace passes through the spiral arm setting on the stand, and slicer controller, hydrothermal reaction kettle and tube-type furnace all are connected with central controller electricity.
2. The hydrothermal-thermal treatment automated experimental platform of claim 1, wherein: the weighing hydrothermal area is provided with a weighing device and a hydrothermal reaction kettle, and the inner cavity of the hydrothermal reaction kettle is larger than the net-shaped supporting platform.
3. The hydrothermal-thermal treatment automated experimental platform of claim 1, wherein: the bearing is established to the cover on the stand, and the bearing inner circle is fixed on the stand, and bearing inner race cover is equipped with the rim plate, transports the spiral arm and fixes in the rim plate lower part, still includes gear motor, and the carousel is established to the cover on gear motor's the output shaft, and the carousel meshes with the upper portion of rim plate to the realization is transported the spiral arm and is rotatory around the stand, and gear motor is connected with central controller electricity.
4. The hydrothermal-thermal treatment automated experimental platform of claim 3, wherein: the end part of the transfer spiral arm is also provided with a lifting mechanism, the bottom end of the lifting mechanism is fixed with an electromagnet, and the electromagnet is electrically connected with the central controller.
5. The hydrothermal-thermal treatment automated experimental platform of claim 4, wherein: the lifting mechanism is an electric push rod or an electric lead screw structure or a hydraulic push rod arranged at the end part of the transfer spiral arm, the electromagnet is fixed at the bottom of the electric push rod or at the bottom of an action part of the electric lead screw structure or at the bottom of the hydraulic push rod, and a motor of the electric push rod or a driving motor of the electric lead screw or a hydraulic oil control part of the hydraulic push rod is electrically connected with the central controller.
CN202020440659.XU 2020-03-31 2020-03-31 Hydrothermal-heat treatment automatic experiment platform Withdrawn - After Issue CN212142549U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111389322A (en) * 2020-03-31 2020-07-10 华北水利水电大学 Hydrothermal-heat treatment automatic experiment platform

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111389322A (en) * 2020-03-31 2020-07-10 华北水利水电大学 Hydrothermal-heat treatment automatic experiment platform

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