CN106732244B - A kind of in-situ observation mineral microreactor and its processing method and purposes - Google Patents
A kind of in-situ observation mineral microreactor and its processing method and purposes Download PDFInfo
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- CN106732244B CN106732244B CN201510824796.7A CN201510824796A CN106732244B CN 106732244 B CN106732244 B CN 106732244B CN 201510824796 A CN201510824796 A CN 201510824796A CN 106732244 B CN106732244 B CN 106732244B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention provides a kind of in-situ observation mineral microreactor and its processing methods and purposes, the mineral microreactor includes reactor body, stirring system, observation system and heating system, reactor body includes autoclave body and kettle cover, stirring system includes power part and the agitating shaft that is fixed on power part, and observation system includes planar lens；Wherein, the power part of stirring system is sealingly fastened on kettle cover, and the agitating shaft being fixed on power part protrudes into the autoclave body of reactor body, and planar lens is set to the bottom of autoclave body, and heating system is coated on the autoclave body of reactor body.The device can realize the pattern on-line analysis of solution leaching process Minerals particle surface, be particularly suitable for high temperature, high-alkali and high-pressure solution system.
Description
Technical field
The invention belongs to electro-hydrometallurgy field, it is related to a kind of mineral microreactor and its processing method and purposes, especially
It is related to the mineral microreactor and its processing method and purposes of a kind of in-situ observation.
Background technique
Leaching is the important process process of field of hydrometallurgy, leaching process be a kind of mineral decompose, oxidation or reduction
Reaction process.Mineral apparent form can occur to change accordingly during the reaction, and this variation is close with chemical reaction process
Cut phase is closed, and therefore, the pattern variation for studying mineral surfaces has great importance for research mineral decomposable process.
Common mineral apparent form observation method is scanning electron microscope and metallographic microscope.Metallographic microscope due to
Have the characteristics that it is at low cost, easy to operate and high-efficient, be often used in observation mineral apparent form variation.But in leaching process
In want observation mineral surfaces pattern variation, need to stop to react, take out the isolated drying of fraction pulp mineral dust side
It can carry out metallographic microanalysis.If it is high temperature and pressure leaching process, then needs to reduce reactor temperature, release stress, to
It is down to after normal pressure and just may filter that separation solid.Since chemical reaction environment is changed, mineral are during separating treatment
Phenomena such as other reactions may occur, dissipate such as powder, gather simultaneously and adsorb, mineral apparent form can great changes will take place, this cannot
The real topography of reactive mineral can not accurately hold mineral response characteristic.
If can during the reaction in-situ observation mineral surfaces pattern change, can accurately hold mineral react into
Journey obtains the reaction rule of leaching of ores process.But existing reaction unit can not observe the change of mineral particle surface pattern in real time
Change, it is even more helpless for high temperature and pressure leaching process.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of in-situ observation mineral microreactor and its places
Reason method and purposes, the device can realize the pattern on-line analysis of solution leaching process Minerals particle surface, be particularly suitable for
High temperature, high-alkali and high-pressure solution system.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, the mineral microreactor includes anti-the present invention provides a kind of in-situ observation mineral microreactor
Device main body, stirring system, observation system and heating system are answered, reactor body includes autoclave body and kettle cover, and stirring system includes dynamic
Power component and the agitating shaft being fixed on power part, observation system includes planar lens；
Wherein, the power part of stirring system is sealingly fastened on kettle cover, and the agitating shaft being fixed on power part is stretched
Enter the autoclave body of reactor body, planar lens is set to the bottom of autoclave body, and heating system is coated on the autoclave body of reactor body.
The design principle of the in-situ observation mineral microreactor are as follows: reaction is added in the autoclave body of mineral microreactor and is situated between
Reactive mineral is cut into regular shape, is fixed on agitating shaft by matter, and agitating shaft is fixed on power part, passes through power part
The high speed rotation of motor strengthens liquid mass transfer in part.The agitating shaft for being placed with reactive mineral block is put into microreactor, it is micro- anti-
Device bottom is answered to be provided with observation system.In use, entire mineral microreactor is inverted in observation instrument (such as metallographic microscope)
Object lens windows above, mineral surfaces pattern is observed through observation system, in this manner it is possible to can see in situ while reaction
The variation of mineral surfaces pattern is surveyed, to effectively hold mineral decomposable process and reaction mechanism.
As a preferred solution of the present invention, it is tightly connected between the autoclave body and kettle cover by kettle cover seal washer.
Preferably, exhaust outlet, pressure gauge, air inlet and needle-valve are provided on the kettle cover.
Preferably, the exhaust outlet, pressure gauge, air inlet and needle-valve are tightly connected by screw thread and kettle cover.
As a preferred solution of the present invention, the power part of the stirring system includes motor and transmission shaft.
Preferably, cylinder shape groove is processed into the bottom of the agitating shaft.
Preferably, cylinder shape groove side processing screw hole is mainly placed in cylinder shape groove by nut fixation
In reactive mineral.
Preferably, placing response mineral on the agitating shaft, the reactive mineral are mineral block.
Preferably, the power part of stirring system is sealingly fastened on kettle cover by mechanical sealing parts.
Preferably, the revolving speed of the agitating shaft be 1500~3000r/min, such as 1500r/min, 1700r/min,
2000r/min, 2300r/min, 2500r/min, 2700r/min or 3000r/min etc..
As a preferred solution of the present invention, the planar lens is sealed at the bottom of autoclave body by lens seals washer
Portion.
Preferably, the planar lens compresses the bottom for being sealed at autoclave body by lens seals washer by nut.
Preferably, the lens seals washer is viton gasket.
Preferably, the planar lens is planar wave lens.
Preferably, the planar lens with a thickness of 5~7mm, such as 5mm, 5.5mm, 6mm, 6.5mm or 7mm etc..
Preferably, the material of the planar lens is calcirm-fluoride or sapphire.
As a preferred solution of the present invention, the heating system includes thermocouple sheath, heating mantle insulating layer, heating furnace silk
And temperature controller.
Preferably, the thermocouple sheath, heating furnace silk and heating mantle insulating layer are successively coated on reactor from inside to outside
The autoclave body of main body.
Preferably, the thermocouple sheath is nickel material, such as N6 nickel material, resistance to highly basic (pH > 14) corrosion.
Preferably, the heating system is heated using electrically heated mode, is heated by temperature controller.
As a preferred solution of the present invention, the design pressure of the mineral microreactor be 1~3Mpa, such as 1MPa,
1.5MPa, 2MPa, 2.5MPa or 3MPa etc., preferably 2Mpa.
Preferably, the design temperature of the mineral microreactor be 150~250 DEG C, such as 150 DEG C, 170 DEG C, 200 DEG C,
230 DEG C or 250 DEG C etc., preferably 200 DEG C.
The design pressure and design temperature can substantially meet conventional wet metallurgical leaching process.
As a preferred solution of the present invention, the autoclave body and kettle cover are nickel material, such as N6 nickel material, resistance to highly basic (pH >
14) corrode.
Second aspect, the present invention provides the processing methods of above-mentioned in-situ observation mineral microreactor, which is characterized in that institute
State processing method are as follows:
Reaction medium is added in the reactor body of mineral microreactor, reactive mineral is fixed on agitating shaft, then
It is put in autoclave body, autoclave body and kettle cover are tightly connected, and agitating shaft rotation are driven by the power part of stirring system, by entire mineral
Microreactor is inverted in observation instrument (such as above metallographic microscope window), can pass through the observation system of mineral microreactor
The variation of observing response mineral surfaces pattern.
As a preferred solution of the present invention, the revolving speed of the agitating shaft be 1500~3000r/min, such as 1500r/min,
1700r/min, 2000r/min, 2300r/min, 2500r/min, 2700r/min or 3000r/min etc..
The third aspect, the present invention provides the purposes of above-mentioned in-situ observation mineral microreactor, and being applied to temperature is 100
~200 DEG C of reaction system.
Preferably, it is applied to the reaction system that pressure is 0.5~2MPa.
Preferably, it is applied to the alkaline reaction system of pH > 14.
It preferably, is that pressure is the reaction system that pH is applied to temperature.
Compared with prior art, the invention has the following advantages:
In-situ observation mineral microreactor provided by the invention be applicable to temperature be 100~200 DEG C, pressure be 0.5~
2MPa, the reaction system of pH > 14 can be to the oxidation of mineral in the reaction system, reduction and decomposable processes in conjunction with metallographic microscope
Online observation is carried out, the mineral not apparent form variation of jljl phase constituent during the reaction is obtained, to the decomposable process of mineral
It is grasped in time, illustrates mineral decomposition mechanism, had a wide range of applications in field of hydrometallurgy.
Detailed description of the invention
Fig. 1 is in-situ observation mineral microreactor apparatus structure schematic diagram of the present invention；
Wherein, 1- heating furnace silk, 2- heating mantle insulating layer, 3- thermocouple sheath, 4- autoclave body, 5- exhaust outlet, 6- pressure gauge,
7- motor, 8- transmission shaft, 9- mechanical sealing parts, 10- air inlet, 11- needle-valve, 12- kettle cover seal washer, 13- lens seals
Washer, 14- planar lens, 15- kettle cover, 16- agitating shaft, 17- temperature controller.
Specific embodiment
Below in conjunction with several specific embodiments, exemplary illustration and help further understand the present invention, but embodiment has
Body details does not represent whole technical solutions under present inventive concept merely to illustrate the present invention, therefore should not be construed as to this
Total technical solution is invented to limit, it is some to be changed for the technician without departing from the unsubstantiality of inventive concept, such as to have
There is the technical characteristic of same or similar technical effect simply to change or replace, the category scope of the present invention.
Embodiment 1:
As shown in Figure 1, present embodiments providing a kind of in-situ observation mineral microreactor, the mineral microreactor includes
Reactor body, stirring system, observation system and heating system, reactor body include autoclave body 4 and kettle cover 15, stirring system packet
The agitating shaft 16 for including power part and being fixed on power part, observation system include planar lens 14；The power of stirring system
Component is sealingly fastened on kettle cover 15, and the agitating shaft 16 being fixed on power part protrudes into the autoclave body 4 of reactor body, plane
Lens 14 are set to the bottom of autoclave body 4, and heating system is coated on the autoclave body 4 of reactor body.
It is tightly connected between the autoclave body 4 and kettle cover 15 by kettle cover seal washer 12, the autoclave body 4 and kettle cover 15 are N6
Nickel material.
Be provided with exhaust outlet 5, pressure gauge 6, air inlet 10 and needle-valve 11 on the kettle cover 15, and exhaust outlet 5, pressure gauge 6,
Air inlet 10 and needle-valve 11 are tightly connected by screw thread and kettle cover 15.
The power part of the stirring system includes motor 7 and transmission shaft 8.
It is processed into cylinder shape groove, cylinder shape groove side processing screw hole, reactive mineral edge in the bottom of the agitating shaft 16
It is fixed in cylinder shape groove and with nut.
The power part of stirring system is sealingly fastened on kettle cover 15 by mechanical sealing parts 9.
The revolving speed of the agitating shaft 16 is 1500r/min, and agitating shaft is stirred by motor quick rotation, with strengthening reactor
Interior liquid mass transfer.
The planar lens 14 compresses the close bottom for being sealed at autoclave body 4 by nut by lens seals washer 13,
The lens seals washer is viton gasket, and planar lens 14 is planar wave lens, and with a thickness of 5mm, material is fluorination
Calcium or sapphire can be resistant to the corrosion of 30% or less strong base solution.
The heating system include thermocouple sheath 3, heating mantle insulating layer 2, heating furnace silk 1 and temperature control 17, it is described
Thermocouple sheath 3, heating furnace silk 1 and heating mantle insulating layer 2 are successively coated on the autoclave body 4 of reactor body from inside to outside.
The thermocouple sheath 3 is N6 nickel material.
The heating system is heated using electrically heated mode, is carried out in computer heating control kettle by temperature controller 17
Temperature.
The design pressure of the mineral microreactor is 2Mpa, and design temperature is 200 DEG C.
Embodiment 2:
A kind of in-situ observation mineral microreactor is present embodiments provided, in addition to the revolving speed of agitating shaft 16 is 2000r/min,
Planar wave lens thickness is 6mm, and planar wave lens material is calcirm-fluoride, and the design pressure of mineral microreactor is 1Mpa,
Design temperature is 150 DEG C outer, and other structures are in the same manner as in Example 1.
Embodiment 3:
A kind of in-situ observation mineral microreactor is present embodiments provided, in addition to the revolving speed of agitating shaft 16 is 2000r/min,
Planar wave lens thickness is 6mm, and the design pressure of mineral microreactor is 3Mpa, and design temperature is 250 DEG C outer, other structures
It is in the same manner as in Example 1.
Embodiment 4:
The in-situ observation of mineral reaction is carried out using device described in embodiment 1, operating method is as follows:
The sapphire plane lens 14 of wiped clean are fixed on to the bottom of autoclave body 4, and are carried out with lens seals washer 13
Sealing, reaction medium is added in reactor body to reaching the 60% of reactor volume, by reactive mineral be cut into diameter 5mm and
Length is that the regular cylindrical body of 10mm is embedded in the cylinder shape groove of agitating shaft 16 and is fixed with nut, and kettle cover 15 is connected
It is put into reactor with stirring system, adds kettle cover seal washer 12 and is fixed on autoclave body 14 with nut seal.
Entire mineral microreactor is upside down on metallographic microscope overhead support, mineral microreactor bottom lens are adjusted
At a distance from metallography microscope endoscope objective lens, fixed reaction unit.The enterprising port 10 of kettle cover is connected to reaction gas, closes exhaust valve 5,
Air inlet needle-valve 11 is opened, adjusts in kettle pressure to design value.It opens temperature controller 17 to be heated, reaches preset value to temperature
It opens motor 7 afterwards to be stirred to react, reaction stops stirring after a certain period of time, opens metallographic microscope, optical path is adjusted, to mineral
Surface topography carries out real-time online observation.
Embodiment 5:
The in-situ observation of mineral reaction, operating method and phase in embodiment 4 are carried out using device described in embodiment 2
Together.
Embodiment 6:
The in-situ observation of mineral reaction, operating method and phase in embodiment 4 are carried out using device described in embodiment 3
Together.
The result of integrated embodiment 1-6 can be seen that in-situ observation mineral microreactor provided by the invention and be applicable to
Temperature is 100~200 DEG C, and pressure is 0.5~2.0MPa, and the reaction system of pH > 14 can exist to mineral in conjunction with metallographic microscope
Oxidation, reduction in reaction system and decomposable process carry out online observation, and obtaining mineral, jljl phase constituent is not during the reaction
Apparent form variation, the decomposable process of mineral is grasped in time, illustrate mineral decomposition mechanism, field of hydrometallurgy tool
It is widely used.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office
Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.
Claims (29)
1. a kind of in-situ observation mineral microreactor, which is characterized in that the mineral microreactor includes reactor body, stirring
System, observation system and heating system, reactor body include autoclave body (4) and kettle cover (15), and stirring system includes power part
With the agitating shaft (16) being fixed on power part, observation system includes planar lens (14)；
Wherein, the power part of stirring system is sealingly fastened on kettle cover (15), and is fixed on the agitating shaft on power part
(16) autoclave body (4) of reactor body is protruded into, planar lens (14) is set to the bottom of autoclave body (4), and heating system is coated on instead
Answer the autoclave body (4) of device main body, placing response mineral on the agitating shaft (16).
2. in-situ observation mineral microreactor according to claim 1, which is characterized in that the autoclave body (4) and kettle cover
(15) it is tightly connected between by kettle cover seal washer (12).
3. in-situ observation mineral microreactor according to claim 1, which is characterized in that be provided on the kettle cover (15)
Exhaust outlet (5), pressure gauge (6), air inlet (10) and needle-valve (11).
4. in-situ observation mineral microreactor according to claim 3, which is characterized in that the exhaust outlet (5), pressure gauge
(6), air inlet (10) and needle-valve (11) are tightly connected by screw thread and kettle cover (15).
5. in-situ observation mineral microreactor according to claim 1, which is characterized in that the power part of the stirring system
Part includes motor (7) and transmission shaft (8).
6. in-situ observation mineral microreactor according to claim 1, which is characterized in that the bottom of the agitating shaft (16)
It is processed into cylinder shape groove.
7. in-situ observation mineral microreactor according to claim 6, which is characterized in that the cylinder shape groove side adds
Work screw hole.
8. in-situ observation mineral microreactor according to claim 1, which is characterized in that the power part of stirring system is logical
Mechanical sealing parts (9) are crossed to be sealingly fastened on kettle cover (15).
9. in-situ observation mineral microreactor according to claim 1, which is characterized in that the revolving speed of the agitating shaft (16)
For 1500~3000r/min.
10. in-situ observation mineral microreactor according to claim 1, which is characterized in that the planar lens (14) is logical
Cross the bottom that lens seals washer (13) is sealed at autoclave body (4).
11. in-situ observation mineral microreactor according to claim 1, which is characterized in that the planar lens (14) is logical
It crosses lens seals washer (13) and compresses the bottom for being sealed at autoclave body (4) by nut.
12. in-situ observation mineral microreactor according to claim 10, which is characterized in that the lens seals washer
It (13) is viton gasket.
13. in-situ observation mineral microreactor according to claim 1, which is characterized in that the planar lens (14) is
Planar wave lens.
14. in-situ observation mineral microreactor according to claim 1, which is characterized in that the planar lens (14)
With a thickness of 5~7mm.
15. in-situ observation mineral microreactor according to claim 1, which is characterized in that the planar lens (14)
Material is calcirm-fluoride or sapphire.
16. in-situ observation mineral microreactor according to claim 1, which is characterized in that the heating system includes heat
Thermowell (3), heating mantle insulating layer (2), heating furnace silk (1) and temperature controller (17).
17. in-situ observation mineral microreactor according to claim 16, which is characterized in that the thermocouple sheath (3),
Heating furnace silk (1) and heating mantle insulating layer (2) are successively coated on the autoclave body (4) of reactor body from inside to outside.
18. in-situ observation mineral microreactor according to claim 16, which is characterized in that the thermocouple sheath (3)
For nickel material.
19. in-situ observation mineral microreactor according to claim 16, which is characterized in that the heating system is using electricity
The mode of heating is heated, and is heated by temperature controller (17).
20. in-situ observation mineral microreactor according to claim 1, which is characterized in that the mineral microreactor
Design pressure is 1~3MPa.
21. in-situ observation mineral microreactor according to claim 1, which is characterized in that the mineral microreactor
Design pressure is 2MPa.
22. in-situ observation mineral microreactor according to claim 1, which is characterized in that the mineral microreactor
Design temperature is 150~250 DEG C.
23. in-situ observation mineral microreactor according to claim 1, which is characterized in that the mineral microreactor
Design temperature is 200 DEG C.
24. in-situ observation mineral microreactor according to claim 1, which is characterized in that the autoclave body (4) and kettle cover
It (15) is nickel material.
25. the processing method of -24 described in any item in-situ observation mineral microreactors according to claim 1, which is characterized in that
The processing method are as follows:
Reaction medium is added in the reactor body of mineral microreactor, reactive mineral is fixed on agitating shaft (16), then
It is put in autoclave body (4), autoclave body (4) and kettle cover (15) are tightly connected, and drive agitating shaft (16) by the power part of stirring system
Rotation, entire mineral microreactor is inverted in observation instrument, can be observed by the observation system of mineral microreactor anti-
Mineral surfaces pattern is answered to change.
26. the purposes of -24 described in any item in-situ observation mineral microreactors according to claim 1, which is characterized in that described
In-situ observation mineral microreactor is applied to the reaction system that temperature is 100~200 DEG C.
27. the purposes of -24 described in any item in-situ observation mineral microreactors according to claim 1, which is characterized in that described
In-situ observation mineral microreactor is applied to the reaction system that pressure is 0.5~2MPa.
28. the purposes of -24 described in any item in-situ observation mineral microreactors according to claim 1, which is characterized in that described
In-situ observation mineral microreactor is applied to the alkaline reaction system of pH > 14.
29. the purposes of -24 described in any item in-situ observation mineral microreactors according to claim 1, which is characterized in that described
It is 100~200 DEG C that in-situ observation mineral microreactor, which is applied to temperature, and pressure is 0.5~2MPa, the reaction system of pH > 14.
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| CN100999386A (en) * | 2006-11-03 | 2007-07-18 | 东华大学 | Method of manufacturing glass microractor by etching |
| CN102049231A (en) * | 2009-10-26 | 2011-05-11 | 荷兰癌症研究基金会 | Micro-reactor for observing particles in fluid |
| CN102636658A (en) * | 2012-04-09 | 2012-08-15 | 天津大学 | Automatic sample feeding tray for temperature-controllable type microreactor with magnetic stirring function |
| CN103182279A (en) * | 2012-03-30 | 2013-07-03 | 嘉兴学院 | Manufacture method of flake microchannel reactor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999386A (en) * | 2006-11-03 | 2007-07-18 | 东华大学 | Method of manufacturing glass microractor by etching |
| CN102049231A (en) * | 2009-10-26 | 2011-05-11 | 荷兰癌症研究基金会 | Micro-reactor for observing particles in fluid |
| CN103182279A (en) * | 2012-03-30 | 2013-07-03 | 嘉兴学院 | Manufacture method of flake microchannel reactor |
| CN102636658A (en) * | 2012-04-09 | 2012-08-15 | 天津大学 | Automatic sample feeding tray for temperature-controllable type microreactor with magnetic stirring function |
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Effective date of registration: 20220111 Address after: 033300 Wangjiazhuang village, Liulin Town, Liulin County, Luliang City, Shanxi Province Patentee after: Shanxi Stone Age New Material Technology Co.,Ltd. Address before: 100190 No. two, No. 1, North Haidian District, Beijing, Zhongguancun Patentee before: Institute of Process Engineering, Chinese Academy of Sciences |