CN107664704A - A kind of online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization - Google Patents
A kind of online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization Download PDFInfo
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- CN107664704A CN107664704A CN201711196935.1A CN201711196935A CN107664704A CN 107664704 A CN107664704 A CN 107664704A CN 201711196935 A CN201711196935 A CN 201711196935A CN 107664704 A CN107664704 A CN 107664704A
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- 238000002474 experimental method Methods 0.000 title claims abstract description 34
- 238000005070 sampling Methods 0.000 title claims abstract description 29
- 230000033558 biomineral tissue development Effects 0.000 title claims abstract description 21
- 238000002156 mixing Methods 0.000 title claims abstract description 19
- 238000009434 installation Methods 0.000 title claims abstract description 17
- 239000000523 sample Substances 0.000 claims abstract description 74
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000012806 monitoring device Methods 0.000 claims abstract description 11
- 239000010902 straw Substances 0.000 claims description 12
- 230000008676 import Effects 0.000 claims description 6
- 239000010720 hydraulic oil Substances 0.000 claims description 5
- 241000208340 Araliaceae Species 0.000 claims 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims 1
- 235000003140 Panax quinquefolius Nutrition 0.000 claims 1
- 235000008434 ginseng Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 31
- 230000008569 process Effects 0.000 abstract description 28
- 238000001556 precipitation Methods 0.000 abstract description 19
- 230000007246 mechanism Effects 0.000 abstract description 17
- 230000005012 migration Effects 0.000 abstract description 15
- 238000013508 migration Methods 0.000 abstract description 15
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000004088 simulation Methods 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 239000012530 fluid Substances 0.000 description 21
- 239000007789 gas Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 14
- 229910052500 inorganic mineral Inorganic materials 0.000 description 12
- 239000011707 mineral Substances 0.000 description 12
- 238000011160 research Methods 0.000 description 10
- 239000011435 rock Substances 0.000 description 10
- 150000002500 ions Chemical class 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 230000006837 decompression Effects 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 229910052718 tin Inorganic materials 0.000 description 5
- 239000011135 tin Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 230000004075 alteration Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 239000011133 lead Substances 0.000 description 3
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000005094 computer simulation Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000001089 mineralizing effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910052758 niobium Inorganic materials 0.000 description 1
- -1 pH changes Substances 0.000 description 1
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- 230000003019 stabilising effect Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N2035/1027—General features of the devices
Abstract
The present invention discloses a kind of online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization, including high-temperature high-pressure reaction kettle, reactor heating and heat-insulating device, reactor pressure charging system, on-line automatic feed arrangement, on-line period device, multi-parameter monitoring device, computer, high-temperature high-pressure reaction kettle is embedded in reactor heating and heat-insulating device, the pressure inlet of reactor pressure charging system connects with high-temperature high-pressure reaction kettle, on-line automatic feed arrangement and on-line period device connects with high-temperature high-pressure reaction kettle, the probe of multi-parameter detector is stretched into on-line period device sampling bottle, computer is connected with multi-parameter detector and thermocouple and reactor heating and heat-insulating device.The present invention controls on-line automatic feed arrangement and multi-parameter monitoring device with computer, hydrolysis and the migration of precipitation experiments simulation formation of ore deposits processes element, the kinetic mechanism of precipitation in high-temperature high-pressure reaction kettle, there is safe and reliable, high temperature high voltage resistant, can intermittently or serially feed, the characteristics of automaticity is high.
Description
Technical field
The invention belongs to technical field of experiment equipment, and in particular to a kind of safe and reliable, high temperature high voltage resistant, can interval or
The online sample introduction sampling complete mixing flow analogue experiment installation of the high HTHP Diagenesis And Mineralization of continuous charging, automaticity.
Background technology
Activation of the material in hydrothermal solution, migration, precipitation are mineralization geological process critically important in nature.People for a long time
More theories and experimental study that phase balance relations are carried out from thermodynamics in terms of, the theory in complete many traditionally,
Though these achievements help to understand and deepen mineralization, but still have significant limitation, and reach balance in closed system
Still gap is very remote between the actual conditions of steady-state model and nature.In fact, many geochemical process belong to it is irreversible
Thermodynamic process, in its motion process with country rock extensive energy and mass exchange activity occur for hydrothermal solution in the earth's crust, these ground
Matter effect all in opening, flowing, it is nonequilibrium under the conditions of.Therefore, certain pressure, temperature, pH, concentration of medium, fugacity are simulated
The Chemical Kinetics experimental study of current system dissolving and precipitation is mutually tied with current system scale-model investigation Deng under the conditions of
The research work of conjunction, research work can be just set to turn to the system side of open remote poised state by the closed system of stable state
Face, it is drawn close major step to the actual conditions of nature, provide foundation for understanding ore deposit mechanism, make geology from wooden
Static observation move towards dynamic experimental study living.
Comparatively, experimental geochemistry is a very young subject.Since last century, different researchers is into ore deposit
Mechanism is studied from different perspectives, with the mechanism of epuilibrium thermodynamics methods experiment study of rocks, ore and mineral formation, is borrowed
Helped thermodynamic (al) instrument-balance, static, closing concept, it is complete it is many traditionally learn in theory.Also once to it is some into
The understanding of ore deposit geologic process has in-depth, but still has significant limitation.Because the geologic process such as hydrothermal solution is place in the earth's crust
In an open system, it is nonequilibrium under the conditions of.Hydrothermal solution has extensive ability and material in its motion process, with surrounding
Exchange.Now, increasing geochemistry process have been found be chemical reaction velocity control process, it is then, non-equilibrium
Thermodynamics and chemical kinetics research geochemical field open a new research direction, much it is experimentally confirmed that non-flat
Weighing apparatus non-linear process is of great importance to Study on ore, mineral formation.
Ore-forming element is migrated and how migrated in geological process in what manner, is all geochemical educational circles all the time
Most basic problem in science, and the problem of fluid migration Mechanism Study can not avoid.Generally, it is considered that the geology dominated in fluid
During, element mainly exists and migrated with corrdination type complex compound and more acid type complex compounds.Central ion and dentate
The environmental factor such as the internal factors such as property, activity, ligand field stabilization energy and temperature, pressure, pH, oxygen fugacity, sulfur fugacity all influences
The stability of complex compound, and migration of elements form and its stability influence and the precipitation mechanism that govern mineral, then is added
Upper complex compound is the main form that element migrates in hydrothermal solution, and it is always that mineral deposit scholar and geochemical scholars pay close attention to that it, which is studied,
Focus.
In addition to theoretical calculation and computer simulation, domestic and foreign scholars are existed using mineral dissolution degree method measure ore-forming element mostly
Existence form in hydrothermal solution.However, mineral dissolution degree principal measure is that element can be with the amount of dissolution in source region, element in fluid
Migration amount and migration yardstick need to by stable migration form --- the stability of complex compound determines, and for such as Pb, Zn
Stability of the chloro-complex in BIFhosted gold deposit still lacks related and reliable infrastest data.At present, Hydrolyze method pair is utilized
The research of migration of element form be concentrated mainly on it is difficult return molten or do not return in molten high valence elements, such as Nb, Ta, Ti, Sn, but for easy
The stability constant that molten lead zinc is only capable of finding lead zinc complex in pure water at 25 DEG C is returned, after lacking the non-magma that carbonate rock holds ore deposit
Under raw hot-liquid type Lead-zinc Deposits Temperature-pressure Conditions（50~350 DEG C, 1~100MPa）NaCl-H2Related experiment number in O systems
According to.
In addition, the main reason for ore-forming element precipitates from hydrothermal solution includes：Cooling, boiling, dilution, pH changes, oxygen
Change reduction Eh changes, fluid mixing and water/petrofacies interaction of wall rock alteration etc. occurs.Compared with above-mentioned other factorses, fluid
It is blended in the formation of all kinds of hydrothermal deposits and has all played important function, may be to the formation mechenism in announcement Large-super Large mineral deposit
It is significant.But current various precipitation mechanisms are based primarily upon mineralogy, petrology, isotope geochemistry, micro member
Plain geochemistry, Geochemistry of Fluid Inclusions, computer simulation and propose, there is no into the checking in terms of ore deposit experiment, especially
Dynamic process to precipitation is even more to know little about it, therefore the expansion of precipitation kinetics experiment is probably to further investigate such mineral deposit
Another breach of mineralization machanism.
Pressure is usually higher during Ore-forming geology, especially by construction control based on mineral deposit in, stress into
The effect of ore deposit is often relatively more significant, thus is up to 100MPa into the operating pressure needed for ore deposit experiment, and temperature is general
Up to 300 DEG C or so, existing high-temperature high-pressure reaction kettle is caused to be difficult to reach a high temperature mostly the requirement of high pressure.Although there is part energy
Enough reach the reactor of above-mentioned HTHP requirement, but due to simulation mineral precipitation during, need different temperatures, pressure, concentration,
PH two kinds and secondary, the multiple or continuous on-line mixing charging with upper fluid；And migration of element process is being simulated, to prevent two
Returning for valency element is molten, needs on-line period to be analyzed.But the reactor that can bear HTHP at present does not possess online add
Material and the function of sampling, and lack the automatic pool control to whole analogue experiment installation, seriously hinder to first into ore deposit
Element migration and the research of precipitation mechanism.
The content of the invention
Present invention the problem of existing for prior art and deficiency, there is provided a kind of safe and reliable, high temperature high voltage resistant, can
The intermittently or serially online sample introduction sampling complete mixing flow analogue experiment installation of the high HTHP Diagenesis And Mineralization of charging, automaticity.
What the present invention was realized in：Including high-temperature high-pressure reaction kettle, reactor heating and heat-insulating device, reactor supercharging system
System, on-line automatic feed arrangement, on-line period device, multi-parameter monitoring device, computer, the kettle of the high-temperature high-pressure reaction kettle
Reactor heating and heat-insulating device is embedded in, the pressure inlet of the reactor pressure charging system connects with high-temperature high-pressure reaction kettle, described
On-line automatic feed arrangement and on-line period device is connected by pipeline with high-temperature high-pressure reaction kettle, the multi-parameter detector
Probe, which is stretched into the sampling bottle of on-line period device, carries out on-line checking, the computer be connected with multi-parameter detector signal and
It is connected respectively with the thermocouple and reactor heating and heat-insulating device of high-temperature high-pressure reaction kettle by temperature controller.
The present invention solves element hydrolysis and the mineral that existing apparatus can not complete the Diagenesis And Mineralization under high-temperature and high-pressure conditions
Precipitation mechanism simulated experiment, using on-line automatic feed arrangement and on-line period device combination high-temperature high-pressure reaction kettle, realize high
Auto feed and online discharging under warm condition of high voltage, feeding quantity and reading multi-parameter monitoring device is controlled to monitor in real time by computer
The parameters such as the pH of solution, temperature, electrical conductivity, ion concentration are taken out, are to be ground under Semi-open system with hydrolysising experiment and precipitation experiments
Study carefully migration of elements, precipitation kinetics mechanism provides the foundation.Meanwhile the present apparatus is applicable not only to non-Magmatic Hydrothermal Deposit,
Hot-liquid type, metamorphic-hydrothermal solution type, the copper of compound hot-liquid type, lead, zinc, molybdenum, gold, tungsten, tin, iron polymetallic deposit are such as constructed, and
Be also applied for Magmatic Hydrothermal Deposit, as Porphyry Copper, molybdenum, gold deposit and pyromagma hot-liquid type tungsten, tin, copper deposit element
Migration and precipitation mechanism are into ore deposit experimental study.Particularly on-line automatic feed arrangement can be squeezed into by plunger pump into autoclave
Fluid within 30MPa, flow of fluid can be driven using plunger pump, and give fluid enough pressure, so as to relatively truer
The fluid of certain pressure enters the decompression boiling occurred during metallogenic space, with other fluids mixes or enclose in simulation mineralizing process
The processes such as raw reaction occur for rock；By preheating apparatus, the fluid temperature (F.T.) that can be achieved to squeeze into is by two-way within 200 °C
To feed arrangement as multichannel can not only simulate certain certain pressure, concentration, temperature fluid enter metallogenic space when
Decompression boiling and Water-rock interaction process, can also simulate two kinds of different pressures, temperature, the fluid of concentration be mixed into ore deposit process and
Its water rock interaction process.And on-line period device includes autoclave by back-pressure controller stabilising system pressure with holding
With Fluid pressure stable in pipeline, for adjusting the pressure of whole reaction system, make it possible on-line period, so as to
Monitor and study into ore deposit and the dynamic process of wall rock alteration.It is of the invention to study the cold of reaction initial state and final state with traditional
Envelope formula autoclave is compared with the not thunder kettle of its miniature version, can be simulated suitable with nature minerogentic condition dynamic into ore deposit mistake
Journey, as fluid is mixed into the process of ore deposit, increasing research shows, fluid mixing is that Large-super Large hydrothermal deposit is formed
Most possible process, and cold seal kettle before is can not also to simulate the process anyway, and cold seal kettle also can not mould
Fluid analogy enters the process of decompression boiling after metallogenic space.Although cold seal kettle can simulate wall rock alteration, because can only study
Its initial state and final state, so can not also study the dynamic process of wall rock alteration.So on-line automatic feed arrangement of the invention
So that fluid mixing and the simulation of decompression boiling are achieved, and on-line period device then makes Diagenesis And Mineralization experimental study from wooden
The flexible more closing to reality of ivory-towered static research steering dynamic studies.Maximum temperature and pressure of the present invention reach
350 DEG C and 100MPa.Therefore, the present invention has safe and reliable, high temperature high voltage resistant, can intermittently or serially feed, automate journey
Degree is high.
Brief description of the drawings
Fig. 1 is principle schematic diagram of the present invention；
Fig. 2 is the reactor boosting system arrangement principle schematic of the present invention；
Fig. 3 is the high-temperature high-pressure reaction kettle overlooking the structure diagram of the present invention；
The kettle that Fig. 4 is the present invention is connected enlarged partial sectional view with kettle cover；
In figure：1- high-temperature high-pressure reaction kettles, 11- kettlies, 12- kettle covers, 13- chucks, 14- safety valves I, 15- pressure gauges I, 16- enters
Sample pipe, 17- probe tubes, 18- thermocouple jacks, the explosion-proof snap rings of 19-, the strong magnetic stick of 1A- high temperature, 1B- high-pressure pipes, 1C-
Explosion-proof O-ring, 2- reactor heating and heat-insulating devices, 3- reactor pressure charging systems, 31- high-pressure gas cylinders, 32- hydraulic systems, 33-
High pressure pressurized cylinder, 34- high-pressure decompression valves, 35- stop valves I, 36- high pressure gauges, 37- hydraulic oil pipes, 38- high-pressure air pipes, 4- are online
Automatic feeder, 41- reservoirs, 42- automatic samplers, 43- plunger pumps, 44- preheaters, 45- check valves I, 46- decompressions
Valve, 47- stop valves II, 48- gas cylinders, 49- flow controllers, 4A- check valves II, 4B- safety valves II, 4C- triple valves, 5- are online
Sampler, 51- sampling bottles, 52- back-pressure controllers, 53- pressure gauges II, 6- multi-parameter monitoring devices, 7- computers, 8- temperature controls
Device processed, 9- thermocouples.
Embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples, but the present invention is not subject in any way
Limitation, based on present invention teach that any changes and modifications made, belong to protection scope of the present invention.
As shown in Fig. 1,2,3 and 4, the present invention includes high-temperature high-pressure reaction kettle 1, reactor heating and heat-insulating device 2, reactor
Pressure charging system 3, on-line automatic feed arrangement 4, on-line period device 5, multi-parameter monitoring device 6, computer 7, the HTHP
The kettle 11 of reactor 1 is embedded in reactor heating and heat-insulating device 2, and the pressure inlet and high temperature of the reactor pressure charging system 3 are high
Pressure reactor 1 is connected, and the on-line automatic feed arrangement 4 and on-line period device 5 are connected by pipeline and high-temperature high-pressure reaction kettle 1
Logical, the probe of the multi-parameter detector 6, which is stretched into the sampling bottle 51 of on-line period device 5, carries out on-line checking, the calculating
Machine 7 be connected with the signal of multi-parameter detector 6 and by temperature controller 8 respectively with the thermocouple 9 of high-temperature high-pressure reaction kettle 1 and anti-
Kettle heating and heat-insulating device 2 is answered to connect.
The high-temperature high-pressure reaction kettle 1 includes kettle 11, kettle cover 12, chuck 13, safety valve I 14, pressure gauge I 15, sample introduction
Pipe 16, probe tube 17, thermocouple jack 18, the kettle cover 12 are placed in the upper end of kettle 11 and connected by chuck 13, the kettle cover
12 set gradually sample feeding pipe 16, probe tube 17, thermocouple jack 18, and the thermocouple 9 stretches into kettle 11 from thermocouple jack 18,
The pressure gauge I 15 is directly arranged at kettle cover 12 and connects kettle 11 or be arranged at the connecting pipe of sample feeding pipe 16, described online
Automatic feeder 4 is connected by sample feeding pipe 16 and on-line period device 5 by probe tube 17 with high-temperature high-pressure reaction kettle 1.
The top that the sample feeding pipe 16 is extended in kettle 11, the bottom that the probe tube 17 is extended in kettle 11.
The kettle cover 12 is in the U-typed body structure with outer edge in Straw hat structure and kettle 11, and the chuck 13 is connected in
The straw hat edge of kettle cover 12 and the outer edge of kettle 11, the straw hat edge lower end of the kettle cover 12 is provided with annular groove I and kettle
The outer edge upper end of body 11 is provided with corresponding annular boss.
The chuck 13 is in " outer edge of ［ " shape buckle structure, described one end of chuck 13 and kettle 11 is hinged and the other end
Screw is provided with, the straw hat edge upper end of the kettle cover 12 is provided with taper hole corresponding with the screw of chuck 13, the kettle cover 12
It is fixedly connected with kettle 11 through multiple chucks 13 for being connected in edge by the screw being positioned at through screw in taper hole.
The edge interval of the kettle cover 12 and kettle 11 between chuck 13 is connected with pastes with edge upper end and lower end respectively
The explosion-proof snap ring 19 closed.
Groove II is provided with the outer edge upper end annular boss of the kettle 11, explosion-proof O is provided with the groove II
Shape ring 1C.
The bottom of kettle 11 is provided with mechanical magnetic couple agitating device, the height of the mechanical magnetic couple agitating device
Warm strong magnetic stick 1A is arranged at the bottom in kettle 11.
The reactor pressure charging system 3 includes high-pressure gas cylinder 31, hydraulic system 32, high pressure pressurized cylinder 33, high pressure relief
Valve 34, the hydraulic oil pipeline of the hydraulic system 32 are connected with the drive end of high pressure pressurized cylinder 33, the high pressure pressurized cylinder 33
Pressurized end import is connected with high-pressure gas cylinder 31 and exported by pipeline and the high-pressure pipe 1B on sample feeding pipe 16 or kettle cover 12
Connection, the control system of the hydraulic system 32 electrically connect with computer 7.
The probe of the multi-parameter detector 6 includes pH combination electrodes, conductivity electrode and/or particular ion concentration and visited
Head, the pH combination electrodes, conductivity electrode and particular ion concentration probe input port corresponding to multi-parameter detector 6 respectively
Connect, the parameter such as the pH of sample, conductance, ion concentration, is moved so as to further investigate in 7 real-time monitoring reaction course of computer
The kinetic mechanism moved and precipitated.
The present invention has at least been independently arranged two sets of online automatic feeders 4, and the on-line automatic feed arrangement 4 includes logical
Reservoir 41 that piping is sequentially connected, automatic sampler 42, plunger pump 43, preheater 44, check valve I 45, the and of pressure-reducing valve 46
Stop valve II 47, the outlet of the stop valve II 47 are connected by pipeline with sample feeding pipe 16, the automatic sampler 42 and/or post
Plug pump 43, preheater 44 electrically connect with computer 7.
The feed arrangement 4 also include be sequentially connected by pipeline gas cylinder 48, stop valve II 47, flow controller 49 and
The air supply system that the 4A of check valve II is formed, the outlet of the 4A of check valve II is connected by pipeline with sample feeding pipe 16.
The on-line period device 5 includes sampling bottle 51, nanoscale filter disc, back-pressure controller 52 and pressure gauge II 53, institute
The import for stating back-pressure controller 52 is connected by pipeline and exported with probe tube 17 and connected by pipeline with sampling bottle 51, the back of the body
Pressure gauge II 53 is connected between the inlet pipeline and probe tube 17 of pressure controller 52, the nanoscale filter disc, which is fixedly installed on, to be taken
The entrance of sample pipe 17 or outlet.
Operation principle and the course of work of the present invention：
The present invention solves element hydrolysis and the mineral precipitation that existing apparatus can not complete the Diagenesis And Mineralization under high-temperature and high-pressure conditions
Mechanism simulation is tested, and using on-line automatic feed arrangement and on-line period device and is combined high-temperature high-pressure reaction kettle, is realized high temperature
Auto feed and online discharging under condition of high voltage, controlling feeding quantity and reading multi-parameter monitoring device by computer, monitoring takes in real time
Go out the parameters such as the pH of solution, temperature, electrical conductivity, ion concentration, be to be studied under Semi-open system with hydrolysising experiment and precipitation experiments
Migration of elements, precipitation kinetics mechanism provide the foundation.Meanwhile the present apparatus is applicable not only to non-Magmatic Hydrothermal Deposit, such as
The polymetallic deposits such as hot-liquid type, metamorphic-hydrothermal solution type, the copper of compound hot-liquid type, lead, zinc, molybdenum, gold, tungsten, tin, iron are constructed, and
Moved suitable for Magmatic Hydrothermal Deposit, such as element of Porphyry Copper, molybdenum, gold deposit and pyromagma hot-liquid type tungsten, tin, copper deposit
Move and precipitation mechanism is into ore deposit experimental study.Maximum temperature and pressure of the present invention reach 350 DEG C and 100MPa.Further, high temperature is high
The kettle cover of pressure reactor is placed in kettle upper end and connected by chuck, and kettle cover sets gradually sample feeding pipe, probe tube, thermocouple and inserted
Hole, thermocouple stretch into kettle from thermocouple jack, and pressure gauge I is directly arranged at kettle cover and connects kettle or be arranged at sample feeding pipe
Connecting pipe, on-line automatic feed arrangement are connected by sample feeding pipe and on-line period device by probe tube and high-temperature high-pressure reaction kettle
It is logical；It by the way that reactor is arranged into two-piece unit formula, can both simplify design, be easy to the internal setting strong magnetic stick of such as high temperature
Deng auxiliary equipment, it is also beneficial to clean and removes the sediment reserved after experiment, and various external connections is set on kettle cover
Pipe and hole, also to realize online input and output material, entering outlet and necessary monitoring device provides installation foundation, and it can also maintain high pressure
Necessary security under environment.Further, kettle cover is in the U-typed body structure with outer edge in Straw hat structure and kettle, chuck
It is connected in the straw hat edge of kettle cover and the outer edge of kettle, the straw hat edge lower end of kettle cover is provided with the outer of annular groove and kettle
Edge upper end is provided with corresponding annular boss；By the way that kettle and kettle cover are set into corresponding outer edge respectively, so as to
Chuck can be made kettle and kettle cover is formed one by being connected in its outer edge, realized for kettle and kettle cover and high pressure resistant lay base
Plinth, and annular groove and annular boss are correspondingly arranged respectively in outer edge, the high voltage performance of high temperature and high pressure kettle can be improved,
The security under hyperbaric environment is improved, and there is certain sealing property.Further, chuck is in " ［ " shape lock knot
The outer edge of structure, chuck one end and kettle is be hinged and the other end is provided with screw, and the straw hat edge upper end of kettle cover is provided with and pressed from both sides
Taper hole corresponding to the screw of set, kettle cover is with kettle through multiple chucks for being connected in edge by being positioned at through screw in taper hole
Screw is fixedly connected；The buckle structure that chuck is arranged to be hinged with kettle, speed during kettle cover dismounting can be accelerated, and
It can prevent chuck from losing, taper hole corresponding with chuck screw is set in the edge upper end of kettle cover in addition, be able to will be pressed from both sides by screw
Set is fixed in taper hole, so as to improve the reliability that kettle cover is connected with kettle, and then increases the security under hyperbaric environment.More
Further, edge interval of the kettle cover with kettle between chuck is connected with the explosion-proof card being bonded respectively with edge upper end and lower end
Ring, groove II is provided with the outer edge upper end annular boss of kettle, explosion-proof O-ring is provided with groove II；Pass through explosion-proof card
Ring can further increase the high voltage bearing reliability of high-temperature high-pressure reaction kettle, and by setting groove II in annular boss and preventing
Quick-fried O-ring, high-pressure leakage can be prevented to forming safe and reliable sealing between kettle and kettle cover.Further, autoclave body bottom is set
There is a mechanical magnetic couple agitating device, under the strong magnetic stick of high temperature of mechanical magnetic couple agitating device is arranged in kettle
Portion；The uniformity of mixed liquor when stirrer in kettle can improve experiment, and in kettle stirrer completely in kettle static seal chamber
Internal rotating, do not stretch out outside kettle, thoroughly solve the leakage problem that packing seal can not overcome, reaction medium is in exhausted
To in the state of closing, without any leakage and pollution.Further, the hydraulic oil pipe of the hydraulic system of reactor pressure charging system
Road is connected with the drive end of high pressure pressurized cylinder, and the pressurized end import of high pressure pressurized cylinder, which is connected and exported with high-pressure gas cylinder, passes through pipe
Road connects with the high-pressure pipe on sample feeding pipe or kettle cover, and the control system of hydraulic system is with calculating mechatronics；Pass through low pressure
Hydraulic-driven high pressure pressurized cylinder, the gas boosting that high-pressure gas cylinder exports to required pressure is set to input high-temperature high-pressure reaction kettle
Interior, so as to maintain the experimental pressure in kettle, compact overall structure, charging efficiency are high, safe and reliable.Further, multi-parameter detects
The probe of instrument includes pH combination electrodes, conductivity electrode and/or particular ion concentration probe, pH combination electrodes, conductivity electrode
And particular ion concentration probe input port connection corresponding to multi-parameter detector respectively；Set by multi-parameter detector different
Electrode and probe, be capable of the heterogeneity parameter of On-line sampling system reaction solution as needed, be Migration of Ore-forming Elements and heavy
The research of shallow lake mechanism improves necessary guarantee.Further, two sets of online automatic feeders have at least been independently arranged, online
Reservoir that automatic feeder includes being sequentially connected by pipeline, automatic sampler, plunger pump, preheater, check valve I, subtract
Pressure valve and stop valve II, the outlet of stop valve II are connected by pipeline with sample feeding pipe, and automatic sampler is with calculating mechatronics；It is logical
Cross various valves and ensure that online sample introduction under condition of high voltage, and pass through computer and control automatic sampler and/or plunger pump, preheating
Device, can control flow velocity, the flow of sample introduction by computer, and plunger pump and preheater can also control the pressure for adding sample（0
~30MPa）With temperature (0~200 DEG C), so as to simulate element different pressures, temperature, flow velocity fluid in transport kinetics
With metallogenic mechanics process during entrance metallogenic space.Further, feed arrangement also includes the gas being sequentially connected by pipeline
The air supply system that bottle, stop valve II, flow controller and check valve II are formed, the outlet of check valve II passes through pipeline and sample feeding pipe
Connection；Can be the specific gas for providing and maintaining as needed various concentrations in kettle by setting online air supply system, so as to
So that simulated experiment process is more true and reliable.Further, on-line period device includes sampling bottle, back-pressure controller and pressure gauge
II, the import of back-pressure controller is connected by pipeline and exported with probe tube and connected by pipeline with sampling bottle, back-pressure controller
Inlet pipeline and probe tube between be connected with pressure gauge II；Back-pressure controller is set by on-line period device, can protected
While demonstrate,proving high-temperature high-voltage reaction in kettle, on-line period is completed, so as to ensure that having in the continuity and course of reaction of reaction
Effect measurement so that effective control is formed to simulated experiment process, is advantageous to the research to migration of element and precipitation mechanism.To sum up
Described, the present invention has safe and reliable, high temperature high voltage resistant, can intermittently or serially fed, automaticity height.
As shown in Figures 1 to 4, when simulated experiment starts, first start computer 7 and temperature controller 8, controlled by computer 7
Temperature controller 8 processed makes electric-heating-wire-heating high-temperature high-pressure reaction kettle 1 in reactor heating and heat-insulating device 2 to predetermined temperature；Together
Shi Qidong reactors pressure charging system 3, argon gas in high-pressure gas cylinder 31 is passed through by high pressure pressurized cylinder 33 according to default pressure value, used
The argon gas that the low-pressure hydraulic oil driving high pressure pressurized cylinder 33 of hydraulic system 32 makes to be passed through is pressurized, and the argon gas after supercharging passes through high-voltage tube
Road is passed through high-temperature high-pressure reaction kettle 1 through high-pressure pipe 1B and is allowed to stop after pressure reaches preset pressure in kettle, completes to start dress
It is standby.Then start on-line automatic feed arrangement 4 and on-line period device 5, controlled certainly according to default experimental measuring by computer 7
Dynamic injector 42 discharges, and after the pressurization of plunger pump 43 and preheater 44 are heated through sample feeding pipe 16 into kettle injection experimentses with prewired
Put solution；Flow controller 49 can also be started if necessary by high pressure gas such as the injection oxygen in gas cylinder 48, hydrogen, sulphur, carbon dioxide
Body is injected in kettle by sample feeding pipe 16, to control the gas fugacity such as hydrogen in kettle, oxygen, sulphur, carbon dioxide.It is reacted in kettle predetermined
After time, back-pressure controller 52 is opened, in being reacted in kettle or the sampled pipe 17 of reacted solution and back-pressure controller 52 subtract
Flowed out to after pressure in sampling bottle 51, the various electrodes being arranged in sampling bottle 51 and probe send measured value to multi-parameter monitoring
Instrument 6, multi-parameter monitoring device 6 are uploaded to computer 7 after measured value is handled, computer 7 is according to default program by temperature control
The numerical value of thermocouple 9 and multi-parameter monitoring device 6 that device 8 processed uploads detect numerical value and calculated, then by after detected value and/or calculating
Numerical value shown.
Claims (10)
1. a kind of online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization, it is characterised in that including high temperature height
Press reactor（1）, reactor heating and heat-insulating device（2）, reactor pressure charging system（3）, on-line automatic feed arrangement（4）, it is online
Sampler（5）, multi-parameter monitoring device（6）, computer（7）, the high-temperature high-pressure reaction kettle（1）Kettle（11）It is embedded in anti-
Answer kettle heating and heat-insulating device（2）, the reactor pressure charging system（3）Pressure inlet and high-temperature high-pressure reaction kettle（1）Connection, it is described
On-line automatic feed arrangement（4）And on-line period device（5）Pass through pipeline and high-temperature high-pressure reaction kettle（1）Connection, more ginsengs
Number detector（6）Probe stretch into on-line period device（5）Sampling bottle（51）Middle carry out on-line checking, the computer（7）
With multi-parameter detector（6）Signal connects and passed through temperature controller（8）Respectively with high-temperature high-pressure reaction kettle（1）Thermocouple
（9）With reactor heating and heat-insulating device（2）Connection.
2. the online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization according to claim 1, its feature
It is the high-temperature high-pressure reaction kettle（1）Including kettle（11）, kettle cover（12）, chuck（13）, safety valve I（14）, pressure gauge I
（15）, sample feeding pipe（16）, probe tube（17）, thermocouple jack（18）, the kettle cover（12）It is placed in kettle（11）Upper end simultaneously passes through
Chuck（13）Connection, the kettle cover（12）Set gradually sample feeding pipe（16）, probe tube（17）, thermocouple jack（18）, the heat
Galvanic couple（9）From thermocouple jack（18）Stretch into kettle（11）, the pressure gauge I（15）It is directly arranged at kettle cover（12）And connect kettle
Body（11）Or it is arranged at sample feeding pipe（16）Connecting pipe, the on-line automatic feed arrangement（4）Pass through sample feeding pipe（16）And
Line sampler（5）Pass through probe tube（17）With high-temperature high-pressure reaction kettle（1）Connection.
3. the online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization according to claim 2, its feature
It is the kettle cover（12）In Straw hat structure and kettle（11）In the U-typed body structure with outer edge, the chuck（13）Clamping
In kettle cover（12）Straw hat edge and kettle（11）Outer edge, the kettle cover（12）Straw hat edge lower end be provided with annular it is recessed
Groove I and kettle（11）Outer edge upper end be provided with corresponding annular boss.
4. the online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization according to claim 3, its feature
It is the chuck（13）In " ［ " shape buckle structure, the chuck（13）One end and kettle（11）Outer edge it is be hinged and another
End is provided with screw, the kettle cover（12）Straw hat edge upper end be provided with and chuck（13）Screw corresponding to taper hole, it is described
Kettle cover（12）With kettle（11）Through multiple chucks for being connected in edge（13）Consolidated by the screw being positioned at through screw in taper hole
Fixed connection.
5. the online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization according to claim 4, its feature
It is the kettle cover（12）With kettle（11）In chuck（13）Between edge interval be connected with respectively with edge upper end and lower end
The explosion-proof snap ring of fitting（19）.
6. complete mixing flow analogue experiment installation is sampled according to the online sample introduction of the HTHP Diagenesis And Mineralization of claim 2,3,4 or 5,
It is characterized in that the kettle（11）Bottom is provided with mechanical magnetic couple agitating device, the mechanical magnetic couple agitating device
The strong magnetic stick of high temperature（1A）It is arranged at kettle（11）Interior bottom.
7. the online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization according to claim 6, its feature
It is the reactor pressure charging system（3）Including high-pressure gas cylinder（31）, hydraulic system（32）, high pressure pressurized cylinder（33）, high pressure
Relief valve（34）, the hydraulic system（32）Hydraulic oil pipeline and high pressure pressurized cylinder（33）Drive end connection, the high pressure
Pressurized cylinder（33）Pressurized end import and high-pressure gas cylinder（31）Connect and outlet passes through pipeline and sample feeding pipe（16）Or kettle cover
（12）On high-pressure pipe（1B）Connection, the hydraulic system（32）Control system and computer（7）Electrical connection.
8. the online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization according to claim 7, its feature
It is the multi-parameter detector（6）Probe include pH combination electrodes, conductivity electrode and/or particular ion concentration probe,
The pH combination electrodes, conductivity electrode and particular ion concentration probe respectively with multi-parameter detector（6）Corresponding input port
Connection.
9. the online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization according to claim 6, its feature
It is at least to be independently arranged two sets of online automatic feeders（4）, the on-line automatic feed arrangement（4）Including passing through pipeline
The reservoir being sequentially connected（41）, automatic sampler（42）, plunger pump（43）, preheater（44）, check valve I（45）, pressure-reducing valve
（46）With stop valve II（47）, the stop valve II（47）Outlet pass through pipeline and sample feeding pipe（16）Connection, it is described to enter automatically
Sample device（42）And/or plunger pump（43）, preheater（44）With computer（7）Connection.
10. the online sample introduction sampling complete mixing flow analogue experiment installation of HTHP Diagenesis And Mineralization according to claim 9, its feature
It is the on-line period device（5）Including sampling bottle（51）, nanoscale filter disc, back-pressure controller（52）And pressure gauge II
（53）, the back-pressure controller（52）Import pass through pipeline and probe tube（17）Connect and outlet passes through pipeline and sampling bottle
（51）Connection, the back-pressure controller（52）Inlet pipeline and probe tube（17）Between be connected with pressure gauge II（53）, it is described
Nanoscale filter disc is fixedly installed on probe tube（17）Entrance or outlet.
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| CN109801544A (en) * | 2019-01-31 | 2019-05-24 | 燕山大学 | A kind of carbonate rock forming environment condition simulation experimental provision and its application method |
| CN110187058A (en) * | 2019-05-13 | 2019-08-30 | 中国地质大学（武汉） | A kind of experimental provision of artificial synthesized fluid inclusion |
| CN111721799A (en) * | 2020-07-22 | 2020-09-29 | 西南石油大学 | Device and method for catalyzing pyrolysis of thickened oil into coke through clay mineral |
| CN113341105A (en) * | 2021-06-01 | 2021-09-03 | 东华理工大学 | Sandstone-type uranium ore mineralization simulation device |
| CN115212837A (en) * | 2022-07-26 | 2022-10-21 | 西安交通大学 | Ammonium bicarbonate high-temperature high-pressure pyrolysis gasification experimental device |
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