CN111389312A - Efficient reactor for preparing monoclinic lead tungstate nano-belt crystal material - Google Patents
Efficient reactor for preparing monoclinic lead tungstate nano-belt crystal material Download PDFInfo
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- CN111389312A CN111389312A CN202010218667.4A CN202010218667A CN111389312A CN 111389312 A CN111389312 A CN 111389312A CN 202010218667 A CN202010218667 A CN 202010218667A CN 111389312 A CN111389312 A CN 111389312A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/32—Titanates; Germanates; Molybdates; Tungstates
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention discloses a high-efficiency reactor for preparing monoclinic lead tungstate nano-belt crystal materials, and mainly relates to the field of lead tungstate crystals. Including the reacting furnace, be equipped with the support frame in the reacting furnace, be equipped with the carriage of displacement around can on the support frame, be equipped with on the carriage and follow the crane of its left and right sides position, be equipped with the imbibition box that can go up and down on the crane, the bottom surface of imbibition box is equipped with the pipette for absorb and the dropping liquid. And a precise injection pump is arranged on the box body and is used for controlling the suction and discharge of the pipette. The invention has the beneficial effects that: the full-automatic mixing device has the advantages of high reaction efficiency, good crystal generation quality, no leakage of harmful substances and personnel safety protection.
Description
Technical Field
The invention relates to the field of lead tungstate crystals, in particular to a high-efficiency reactor for preparing monoclinic lead tungstate nano-belt crystal materials.
Background
In recent years, the demand for high-resolution electromagnetic energy meters has increased, and in addition, many of the high-precision scientific instruments today, such as medical CT scanners, core probe elements for equipment used in the fields of nuclear industrial geological exploration and archaeology, require the use of a large amount of high-quality scintillation crystal materials, which has made the search for a new generation of scintillation materials (tungstate crystals) quite active, PbWO4 crystals have been used in large hadron collider (L HC) high-resolution electromagnetic energy meters due to their unique luminescence and other properties, and can be applied to Positron Emission Tomography (PET) and other medical imaging applications.
In most manufacturing operations, the crystal formation process requires strict temperature control, and the temperature is generally selected to be 70-500 ℃ according to the desired product and formulation. The heating is required to be uniform, and the local part cannot be directly heated, so a water bath or an oil bath is adopted mostly, and the heating control is mature.
However, in many reactions, such as the preparation of typical monoclinic lead tungstate nano-ribbon crystal materials, one method involves the addition of another reactant or promoter after one of the reactants is preheated to a suitable temperature in the reaction solvent, which initiates the crystal formation, and this addition process imposes severe requirements on both the temperature of the solvent feedstock added and the manner of addition, such as dropwise addition at a rate of 0.8-2.0ml/min, in order not to disturb the solution and not to destroy the temperature. However, in a specific operation, the uniform dropping itself lengthens the time of the mixing stage, and the temperature of the solution to be added into the isothermal reaction solution is difficult to maintain in the slow dropping process. This is detrimental to the initial crystal formation and also to the ripening process.
Meanwhile, the uniform dropping of the water bath/oil bath under the high temperature condition is difficult to accurately control, and has a great risk for operators, so that although the temperature of the reaction liquid is easy to control in the initial reaction stage of the crystals, for the reaction in the dropping link, the lead tungstate crystals are easy to reflect initially, the degree of expectation of the result is greatly reduced due to the uncontrollable property of the link, and the data of the experimental conclusion are greatly interfered.
Further, since the initial contact of the reaction solution is very uneven, that is, the dropping position is very local to the whole reaction solution, stirring is not possible, but the requirement for reaction mixing is not satisfied. In addition, the lead tungstate crystal is a crystal grown in a heat-insulating cover in a single crystal furnace using a platinum crucible as a raw material. Whether the lead oxide and the tungsten oxide are added dropwise or mixed, the volatile toxic gas containing the lead oxide can bring harm to the health of researchers.
Disclosure of Invention
The invention aims to provide an efficient reactor for preparing monoclinic lead tungstate nano-belt crystal materials, which has the advantages of efficient reaction, good crystal generation quality, full-automatic mixing, no leakage of harmful substances and personnel safety protection.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the reaction box comprises a reaction furnace, wherein a heating cavity is arranged in the reaction furnace, a furnace door is arranged at an opening of the heating cavity, heat insulation cotton is arranged on the heating cavity and the inner wall of the furnace door, heat insulation grooves are formed in the bottom of the reaction furnace, heat insulation cotton pads are arranged on two sides of each heat insulation groove, a reaction box is arranged in each heat insulation groove, a door plate hinged with the bottom side is arranged on one side, close to the furnace door, of each reaction box, a plurality of partitions which are arranged equally are arranged in the depth direction of each reaction box, drawing grooves are formed among the partitions, drawing grooves are matched with sliding plates in a drawing mode, a plurality of mounting holes are formed in each sliding plate in the length direction of each sliding plate, reaction tubes are movably inserted into the mounting holes, a window is arranged on each drawing groove and used for exposing the mouths of the reaction tubes inserted into the sliding plates, a mounting surface is arranged on the top side end surface of each heat insulation cotton,
it is left be equipped with left guide rail on the support frame, the right side be equipped with right guide rail on the support frame, left side guide rail is in the below position of right guide rail, left side guide rail and right guide rail all extend along the direction of depth of reacting furnace, and is left still be equipped with on the support frame and set up side by side and the flexible lead screw that extends with the left guide rail, flexible lead screw passes through motor drive, be equipped with on the support frame and can be along gliding L type carriage around the support frame, the screw on the flexible lead screw is fixed at the carriage left end, the left end at the carriage is fixed to the slider on the left side guide rail, the right side top at the carriage is fixed to the slider on the right side guide rail, the carriage has the right angle and the L type that upwards extends, horizontal extension's translation guide rail about being equipped with on the carriage, be equipped with rather than side by side in the translation guide rail, the translation lead screw that extends in the same direction, translation lead screw passes through motor drive, screw on the translation lead screw and the translation guide rail all fix on the crane, be equipped with the lift rail, the lift rail is equipped with the lift table, the lift rail is equipped with the suction box, the suction box is used for suction liquid suction box body is carried out the pipette to the accurate injection.
Be equipped with bilateral symmetry's support bar on the lateral wall in pull groove, the extending direction of support bar is unanimous with the depth direction in pull groove, install the riding wheel on the support bar, the top of riding wheel is global to expose at the top side terminal surface in support bar, and rolls around the direction, also is unanimous with the depth direction in pull groove, the length of slide suits with the degree of depth in pull groove, the width of slide suits with the width in pull groove, and is greater than the distance between two support bars, can bear the weight of the top in the support bar, realizes the pull with the riding wheel around sliding fit.
Specifically, the L type carriage comprises a guide rail frame extending horizontally from left to right and a hanger rail frame extending upwards from right, the slide block on the right guide rail is fixed at the top end of the hanger rail frame, and the slide block on the left guide rail is fixed at the left end of the guide rail frame.
The top of crane is equipped with camera module for carry out the video recording to the reaction condition of below.
Compared with the prior art, the invention has the beneficial effects that:
through this device reaction, the dropwise add operation is followed in the past and is carried out the dropwise add to a certain reaction group, changes into and carries out dropwise add in turn to a plurality of reaction groups, has improved reaction efficiency greatly. Meanwhile, the capacity of single-group reaction is reduced, and the reaction is carried out in each reaction tube, so that the mixing effect after dripping is improved, and the crystal generation quality is improved. And the mixture is in sealed environment, guarantees no harmful substance to leak, protection personnel's safety.
Drawings
FIG. 1 is a perspective view of the structure of the present invention.
Fig. 2 is a perspective cross-sectional view of the present invention.
FIG. 3 is a perspective view showing the structure of the reaction cassette of the present invention.
FIG. 4 is a perspective view showing the structure of the reaction cassette of the present invention.
Fig. 5 is an enlarged view of the portion a of the present invention.
Reference numerals shown in the drawings:
1. a reaction furnace; 2. a furnace door; 3. a heat-insulating cotton pad; 4. a reaction box; 5. a door panel; 6. separating; 7. a supporting strip; 8. a riding wheel; 9. a slide plate; 10. a reaction tube; 11. a window; 12. a support frame; 13. a left guide rail; 14. a right guide rail; 15. a carriage; 16. a translation guide rail; 17. a lifting guide rail; 18. a camera module; 19. and a liquid suction box.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the present application.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.
Example (b): efficient reactor for preparing monoclinic lead tungstate nano-belt crystal material
Including reacting furnace 1, be equipped with the heating chamber in reacting furnace 1, the opening in heating chamber sets up furnace gate 2, it is cotton to set up the heat preservation on heating chamber and the 2 inner walls of furnace gate. The reaction furnace 1 is closed and then is in a sealed heating environment, and the temperature can be increased to 700 ℃.
The bottom of the reaction furnace 1 is provided with a heat preservation groove, and the two sides of the heat preservation groove are both provided with heat preservation cotton pads 3 for increasing the local constant temperature effect and ensuring the balance of the reaction temperature.
The heat preservation inslot is equipped with reaction box 4, reaction box 4 is close to 2 one sides of furnace gate and is equipped with door plant 5 with bottom side articulated, be equipped with the wall 6 of a plurality of impartial settings along the depth direction on the reaction box 4, separate reaction box 4 for 6 independent cells, define into the pull groove, be equipped with bilateral symmetry's support bar 7 on the lateral wall in pull groove, the extending direction of support bar 7 is unanimous with the depth direction in pull groove, install riding wheel 8 on the support bar 7, the global top terminal surface that exposes at support bar 7 in riding wheel 8, and roll direction around for, also unanimous with the depth direction in pull groove, conveniently lets the more smooth of pull with the cooperation of slide 9.
The pull inslot is equipped with rather than pull complex slide 9, be equipped with 8 mounting holes along its length direction on the slide 9, the reaction tube 10 is pegged graft in the mounting hole activity, the mouth of pipe of reaction tube 10 is equipped with the shelves piece, and is outside protruding for restrict the mouth of pipe of reaction tube 10 in the top of mounting hole, the length of slide 9 suits with the degree of depth in pull groove, the width of slide 9 suits with the width in pull groove, and is greater than the distance between two support bars 7, can bear the weight of the top of support bar 7, realizes the pull with riding wheel 8 front and back sliding fit.
The reaction tube 10 is used for containing a reaction solvent or a reactant.
On the top wall of the reaction cassette 4, a window 11 is provided corresponding to each of the drawing grooves, the window 11 being used to expose the mouth of the reaction tube 10 after the slide plate 9 is inserted. The liquid is convenient to absorb and drop.
The top side end face of the heat preservation cotton pad 3 is provided with an installation face, a support frame 12 extending in the front-back depth direction is fixed on the installation face, a left guide rail 13 is arranged on the left support frame 12, a right guide rail 14 is arranged on the right support frame 12, the left guide rail 13 is arranged at the position below the right guide rail 14, the left guide rail 13 and the right guide rail 14 both extend along the depth direction of the reaction furnace 1, a telescopic lead screw arranged in parallel with the left guide rail 13 and extending in the same direction is further arranged on the left support frame 12, and the telescopic lead screw is driven by a motor,
an L-type sliding frame 15 capable of sliding back and forth along the support frame 12 is provided on the support frame 12,
screw on the telescopic lead screw is fixed on carriage 15, the left end at carriage 15 is fixed to the slider on the left guide rail 13, the right side top at carriage 15 is fixed to the slider on the right side guide rail 14, carriage 15 has the L type that right angle and upwards extend for the right side, and is specific, L type carriage 15 is including controlling the guide rail frame that the level extends, and the hanger rail frame that the right side upwards extends, the top at hanger rail frame is fixed to the slider on the right side guide rail 14, the left end at guide rail frame is fixed to the slider on the left side guide rail 13, and this kind of structure can reduce resonance in the dropping liquid, keeps the precision of dropping liquid.
The horizontal extension's translation guide rail 16 about being equipped with on the guide rail frame, be equipped with in the translation guide rail 16 and set up side by side rather than, the translation lead screw of syntropy extension, the translation lead screw passes through motor drive, screw on the translation lead screw and the slider on the translation guide rail 16 are all fixed on the crane, be equipped with lifting rail 17 on the crane, sliding fit has the elevating platform about lifting rail 17, install electric push rod on the crane, electric push rod's output and elevating platform are connected, and the control goes up and down, the top of crane is equipped with camera module 18 for record a video to the reaction condition of below. The course of the reaction was recorded.
Be equipped with imbibition box 19 on the elevating platform, the bottom surface of imbibition box 19 is equipped with the pipette for absorb and the dropping liquid. And the Nanemite precision injection pump is arranged on the box body and is used for controlling the suction and the discharge of the pipette.
Reaction solution is put into the reaction tube 10 of a certain row or two rows, reactant is put into multirow reaction tube 10, after reaction solution is extracted through the pipette, the dropping liquid is carried out alternately between multirow a plurality of reaction tubes 10, the dropping liquid speed can reach 20ul per second, the dropping liquid is from alternately between a plurality of reaction tubes 10, and the dropping speed of each reaction tube 10 is kept to meet the reaction requirement.
Through this device reaction, the dropwise add operation is followed in the past and is carried out the dropwise add to a certain reaction group, changes into and carries out dropwise add in turn to a plurality of reaction groups, has improved reaction efficiency greatly. Meanwhile, the capacity of single-group reaction can be reduced, and the reaction can be carried out in each reaction tube 10, so that the mixing effect after dripping is improved, and the crystal generation quality is improved. And the mixture is in sealed environment, guarantees no harmful substance to leak, protection personnel's safety.
Claims (4)
1. A high-efficiency reactor for preparing monocline lead tungstate nano-belt crystal materials is characterized by comprising a reaction furnace, wherein a heating cavity is arranged in the reaction furnace, a furnace door is arranged at an opening of the heating cavity, heat-preservation cotton is arranged on the inner walls of the heating cavity and the furnace door, a heat-preservation groove is arranged at the bottom of the reaction furnace, heat-preservation cotton pads are arranged on two sides of the heat-preservation groove, a reaction box is arranged in the heat-preservation groove, a door plate hinged with the bottom side is arranged on one side, close to the furnace door, of the reaction box, a plurality of partitions which are arranged equally are arranged along the depth direction, pull grooves are formed between the partitions, a sliding plate is matched in the pull grooves in a pull mode, a plurality of mounting holes are formed in the sliding plate along the length direction of the sliding plate, reaction tubes are movably inserted in the mounting holes, a window is arranged on the top wall of the reaction box and corresponds to each, the top side end face of the heat-insulating cotton pad is provided with a mounting surface, a supporting frame extending in the front-back depth direction is fixed on the mounting surface,
it is left be equipped with left guide rail on the support frame, the right side be equipped with right guide rail on the support frame, left side guide rail is in the below position of right guide rail, left side guide rail and right guide rail all extend along the direction of depth of reacting furnace, and is left still be equipped with on the support frame and set up side by side and the flexible lead screw that extends with the left guide rail, flexible lead screw passes through motor drive, be equipped with on the support frame and can be along gliding L type carriage around the support frame, the screw on the flexible lead screw is fixed at the carriage left end, the left end at the carriage is fixed to the slider on the left side guide rail, the right side top at the carriage is fixed to the slider on the right side guide rail, the carriage has the right angle and the L type that upwards extends, horizontal extension's translation guide rail about being equipped with on the carriage, be equipped with rather than side by side in the translation guide rail, the translation lead screw that extends in the same direction, translation lead screw passes through motor drive, screw on the translation lead screw and the translation guide rail all fix on the crane, be equipped with the lift rail, the lift rail is equipped with the lift table, the lift rail is equipped with the suction box, the suction box is used for suction liquid suction box body is carried out the pipette to the accurate injection.
2. The efficient reactor for preparing the monoclinic lead tungstate nano-belt crystal material as claimed in claim 1, wherein the lateral wall of the drawing groove is provided with support bars which are bilaterally symmetrical, the extending direction of the support bars is consistent with the depth direction of the drawing groove, the support bars are provided with supporting wheels, the top peripheral surfaces of the supporting wheels are exposed on the top side end surfaces of the support bars, the rolling direction is front-back rolling and is consistent with the depth direction of the drawing groove, the length of the sliding plate is suitable for the depth of the drawing groove, the width of the sliding plate is suitable for the width of the drawing groove, the distance between the two support bars is greater than the distance between the two support bars, the support bars can be supported above the support bars, and the drawing is realized by sliding fit with the supporting wheels in front-back.
3. The efficient reactor for preparing monoclinic lead tungstate nano-belt crystal material as recited in claim 1, wherein the L type sliding frame comprises a left and right horizontally extending guide rail frame and a right upwardly extending hanger rail frame, the slide block on the right guide rail is fixed on the top end of the hanger rail frame, and the slide block on the left guide rail is fixed on the left end of the guide rail frame.
4. The efficient reactor for preparing the monoclinic lead tungstate nano-belt crystal material as claimed in claim 1, wherein a camera module is arranged at the top end of the lifting frame and used for recording the reaction condition below the lifting frame.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010218667.4A CN111389312A (en) | 2020-03-25 | 2020-03-25 | Efficient reactor for preparing monoclinic lead tungstate nano-belt crystal material |
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| CN202010218667.4A CN111389312A (en) | 2020-03-25 | 2020-03-25 | Efficient reactor for preparing monoclinic lead tungstate nano-belt crystal material |
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| CN1525175A (en) * | 2003-02-27 | 2004-09-01 | 霍夫曼-拉罗奇有限公司 | System for automatic opening of reagent vessels |
| CN202962450U (en) * | 2012-11-26 | 2013-06-05 | 浙江泛泰仪器有限公司 | Porous high temperature reactor |
| CN105312019A (en) * | 2015-10-21 | 2016-02-10 | 无锡科锋化工有限公司 | Chemical-engineering reaction kettle capable of achieving even liquid dropping and stirring |
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| CN110841587A (en) * | 2019-12-16 | 2020-02-28 | 山东豪迈机械制造有限公司 | Reaction device and reaction equipment |
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Application publication date: 20200710 |