CN106811773A - Supercritical composite electroforming system recycling device - Google Patents
Supercritical composite electroforming system recycling device Download PDFInfo
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- CN106811773A CN106811773A CN201710068972.8A CN201710068972A CN106811773A CN 106811773 A CN106811773 A CN 106811773A CN 201710068972 A CN201710068972 A CN 201710068972A CN 106811773 A CN106811773 A CN 106811773A
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- control valve
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- 238000005323 electroforming Methods 0.000 title claims abstract description 93
- 239000002131 composite material Substances 0.000 title claims abstract description 87
- 238000004064 recycling Methods 0.000 title abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 131
- 238000001514 detection method Methods 0.000 claims abstract description 56
- 239000002245 particle Substances 0.000 claims abstract description 54
- 238000000926 separation method Methods 0.000 claims abstract description 41
- 239000007787 solid Substances 0.000 claims abstract description 41
- 239000011246 composite particle Substances 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims description 49
- 238000004062 sedimentation Methods 0.000 claims description 23
- 238000010521 absorption reaction Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 13
- 238000003760 magnetic stirring Methods 0.000 claims description 13
- 239000002699 waste material Substances 0.000 claims description 13
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 4
- 239000008246 gaseous mixture Substances 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229960004643 cupric oxide Drugs 0.000 claims description 3
- 239000013589 supplement Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 21
- 238000001035 drying Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000003860 storage Methods 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 106
- 239000012530 fluid Substances 0.000 description 12
- 239000010432 diamond Substances 0.000 description 11
- 229910003460 diamond Inorganic materials 0.000 description 11
- 238000012545 processing Methods 0.000 description 7
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 5
- 239000002956 ash Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000002923 metal particle Substances 0.000 description 5
- 238000007747 plating Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000001351 cycling effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000003252 repetitive effect Effects 0.000 description 4
- 238000004070 electrodeposition Methods 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 208000020442 loss of weight Diseases 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 210000005056 cell body Anatomy 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/16—Regeneration of process solutions
- C25D21/18—Regeneration of process solutions of electrolytes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention provides a supercritical composite electroforming system recycling device, which comprises a control valve bank, a gas filter, a gas storage, an electroforming liquid storage, a magnetic pump, an electroforming liquid detection and allocation assembly, a composite particle recoverer, a high-pressure pump, CO2A gas cylinder and a pressure gauge; the gas filter comprises a gas-liquid separation chamber, a gas filtering chamber and a gas drying chamber; the gas filter is connected with the reaction kettle and the gas storage device and is used for recovering gas; the magnetic pump is connected with the electroforming solution memory; the electroforming liquid detection and blending assembly comprises an ion detection tank, an ion measuring instrument and a composite electroforming liquid blending tank, wherein the composite electroforming liquid blending tank is used for recovering and blending the composite electroforming liquid; composite particle recoverer for recovering useful solids in composite electroforming liquidParticles; the working method mainly comprises the steps of gas recovery, solid particle recovery, impurity removal of electroforming solution, blending and preparing composite electroforming solution for recycling and the like. The invention can improve the use efficiency of the electroforming solution, reduce the pollution to the environment and reduce the economic cost of composite electroforming.
Description
The application is Application No. 201510241096.5, and the applying date is on May 12nd, 2015, and invention and created name is
The divisional application of the application for a patent for invention of " overcritical composite electroformed system recycle device and its method of work ".
Technical field
The present invention relates to electrochemical deposition processing technique field, and in particular to a kind of overcritical composite electroformed system reclaims profit
With device and its method of work.
Background technology
At present, with MEMS（MEMS, Micro-Electro-Mechanical System）Technology it is at full speed
Development and the active demand to high-performance composite materials, composite electroformed technology will all play the part of important angle in current or even future
Color.
Supercritical fluid（Supercritical Fluid）Refer to that pure material is in critical point（Critical pressure and critical
Temperature）During the above, the one kind for being showed is between liquid and gaseous fluid.In recent years, composite electroformed technology is faced with super
Boundary's fluid technique is combined, and is a study hotspot for preparing High performance nanometer composite material.At present, the electricity under supercritical environment
Deposition prepares nano composite material with the existing finding of the process and device of micro-workpiece.If Authorization Notice No. is CN
The Chinese patent literature of 101092716B discloses a kind of trickle electroforming technique of supercritical fluid and its device, and it is with SCF-
CO2For plating environment carries out the shaping of micro-structure part, metal plating layer surface depositing homogeneous as obtained by the method, without product
Knurl, and cast layer tissue is fine and closely woven smooth；And for example publication No. is a kind of overcritical for the Chinese patent literature of CN 102146573A is proposed
The method that fluid electrotyping forming prepares nano composite material, it is mainly the electro-deposition under mechanical agitation subsidiary conditions and prepares metal
Based nano composite material.However, foregoing invention does not consider the recycling to overcritical electroforming solution.Supercritical CO2It is compound
Electroforming system includes CO2Gas, chemical plating fluid and compound particle.Electroforming is finished in exhaust process, and liquid easily follows gas to arrange
Go out and enter pipeline and valve, the liquid plating solution after the compound particle of the inside and solidification can block pipeline and valve, severe attrition electricity
The service life of casting device；And, CO2Being directly discharged into air can aggravate Global Greenhouse Effect；And chemical plating fluid is dirty to environment
Dye influence is obvious, is directly discharged into the Nature, is all a kind of disaster to surface water and soil；Compound particle in electroplating process not
Electroformed layer can be fully entered, in the solution can also a remaining part, moreover especially nano level cost is to prepare compound particle very much
Height, thus the compound particle recycling that will be cast in liquid is relatively inexpensive.
The content of the invention
The purpose of the present invention is：For supercritical CO2Composite electroformed system, there is provided CO can be reclaimed when one kind is used2Gas
Particle is fixed required for body, electroforming solution and electroforming as a means of recycling, so as to the service efficiency, the reduction that effectively improve electroforming solution are right
The pollution of environment, the overcritical composite electroformed system recycle device and its method of work that reduce composite electroformed financial cost.
The technical scheme is that：Overcritical composite electroformed system recycle device of the invention, including reactor,
Reactor has leakage fluid dram, exhaust outlet and air inlet；It is structurally characterized in that：Also include that control valve group, pneumatic filter, gas are deposited
Reservoir, electroforming solution memory, magnetic drive pump, electroforming solution detection allotment component, composite particles recover, high-pressure pump, CO2Gas cylinder and pressure
Power table；
Above-mentioned control valve group includes gas liquid mixture discharge control valve, electroforming solution discharge control valve, the input control of reactor gas
Valve processed and gas supply control valve；
Pneumatic filter includes that the gas-liquid separation chamber that sets gradually from top to bottom and mutually ventilate, the gentle soma in gas filtration room are dry
Room；Gas-liquid separation chamber discharges control valve and is connected with the exhaust outlet of reactor by the gas liquid mixture of control valve group；
Gas reservoir is provided with recovery gas input port, tonifying Qi input port and air supply opening；The recovery gas input port of gas reservoir with
The gas hothouse of pneumatic filter is connected；The tonifying Qi input port of gas reservoir by high-pressure pump and gas supply control valve with
CO2Gas cylinder is connected；The air supply opening of gas reservoir is connected by reactor gas input control valve with the air inlet of reactor
Connect；
Electroforming solution memory is provided with inlet, liquid outlet and magnetic stirring apparatus；Magnetic stirring apparatus is arranged on electroforming solution memory
Bottom；The inlet of electroforming solution memory is discharged control valve and is connected with the leakage fluid dram of reactor by electroforming solution；
Magnetic drive pump is provided with inlet, liquid outlet and detachable absorption filter element；The inlet of magnetic drive pump and electroforming solution memory
Liquid outlet is connected；
Electroforming solution detection allotment component includes ion detection groove, ion gauge and composite electroformed liquid surge-tank；Ion detection groove
It is provided with inlet, liquid outlet, detection liquid outlet and waste discharge mouth；The inlet of ion detection groove is connected with the liquid outlet of magnetic drive pump
Connect；Ion gauge is connected by the detection liquid outlet of ion detection groove with ion detection groove；The waste discharge mouth of ion detection groove
For discharging waste liquid；The liquid outlet of ion detection groove is connected with composite electroformed liquid surge-tank；
Composite particles recover is used to reclaim the useful solid particle in the composite electroformed liquid of reactor releasing；Composite particles are reclaimed
Device includes burning unit, sedimentation separation unit, is cleaned and dried unit and detection unit；
High-pressure pump and CO2Gas cylinder is used for as CO in gas reservoir2To supplementing CO in gas reservoir when not enough2Gas；Pressure gauge
For detecting the air pressure in reactor, pressure gauge is arranged between reactor gas input control valve and the air inlet of reactor；
The lower end of the gas-liquid separation chamber of above-mentioned pneumatic filter is provided with gaseous mixture input port；It is provided with gas-liquid separation room and is dipped down
One group of oblique baffle plate, the downward-sloping angular range of baffle plate is 8~16 °；Cupric oxide solid is filled with gas filtration room；Gas mistake
Adding thermal resistance is provided between the inside and outside wall of filter chamber；Gas hothouse is provided with gas recovery delivery outlet；Filling in gas hothouse
There is solid calcium chloride；
The inwall of above-mentioned gas reservoir is provided with for controlling gas reservoir that operationally internal temperature is cold 2 DEG C of circulation
But water pipe；
The rotating speed when magnetic stirring apparatus of above-mentioned electroforming solution memory works is 400~600r/min.
Further scheme is：Above-mentioned magnetic drive pump is MP Micro magnetic driving pumps；The detachable absorption filter element of magnetic drive pump is
Stainless steel filter core or collapsible micropore filter element, filter core outer wrap double-layer filter cloth.
Further scheme also has：The unit that burns of above-mentioned composite particles recover is used for by the removable of magnetic drive pump
The solid particle for unloading the recovery of formula absorption filter element carries out burning disposal；
Sedimentation separation unit includes composite particles centrifugal settler；Sedimentation separation unit is used to enter the incineration ashes for burning unit
Row centrifugal sedimentation is separated so that the solid particle in incineration ashes needed for composite electroformed liquid configuration is separated with heavy metal particles；
The solid particle that being cleaned and dried unit is used for needed for being configured to the composite electroformed liquid isolated is cleaned and dried；
Composite electroformed liquid after detection unit is used for cleaning-drying configures whether required solid particle meets recycling mark
Standard is detected.
The method of work of above-mentioned overcritical composite electroformed system recycle device, comprises the following steps：
1. gas is reclaimed：Open the gas liquid mixture discharge control valve of control valve group so that reactor constant temperature is depressurized to one greatly
Air pressure, mixed gas inside reactor are carried by the gas-liquid separation chamber of pneumatic filter, the gentle body hothouse in gas filtration room
Gas reservoir interior circulation is collected in after pure treatment to use；
2. solid particle is reclaimed：
The first step：Electroforming solution discharge control valve is opened, the composite electroformed liquid in reactor is collected in electroforming solution memory, opened
The magnetic stirring apparatus of dynamic electroforming solution memory, makes the insoluble solid particle in composite electroformed liquid effectively disperse to suspend；
Second step：Magnetic drive pump extracts the composite electroformed liquid in electroforming solution memory, and composite electroformed liquid is by the detachable of magnetic drive pump
Formula absorption filter element is flowed in ion detection groove after filtering, into step 3.；Solid particle in composite electroformed liquid is by magnetic drive pump
Detachable absorption filter element be collected into it is a certain amount of after transfer to composite particles recover process；
3rd step：Solid particle in the composite electroformed liquid collected by the detachable absorption filter element of magnetic drive pump is successively through compound
The burning unit of grain recover carries out burning disposal, sedimentation separation unit to be carried out centrifugal sedimentation separation, is cleaned and dried the clear of unit
The purity detecting dried with detection unit is washed, the solid particle needed for obtaining the composite electroformed liquid configuration of recyclable recycling；
Detection solid particle not up to standard puts into sedimentation separation cell processing again；
3. electroforming solution goes the removal of impurity：The electroforming solution that solid particle is eliminated after the detachable absorption filter element filtering of magnetic drive pump is flowed into
After ion detection groove, by the composition and concentration of various ions in ion gauge detection electroforming solution, remove as required wherein micro-
Amount foreign ion, the ion that supplement electroforming solution needs, obtains satisfactory electroforming solution；
4. composite electroformed liquid is allocated：By step 2. in obtain composite electroformed liquid configuration needed for solid particle and step 3. in
The electroforming solution for obtaining is deployed into the composite electroformed liquid for meeting electroforming requirement according to set proportion in composite electroformed liquid surge-tank
For recycling.
Further scheme is：Above-mentioned step 1. in, gas filtration room work when temperature control at 200 degrees Celsius；
Temperature when gas hothouse works is normal temperature.
Further scheme is：In above-mentioned step the 3rd step 2., during the burning cell operation of composite particles recover
At 500 DEG C, the burning time is 5~10min to temperature control；Above-mentioned sedimentation separation unit includes composite particles centrifugal settler；
The rotating speed of composite particles centrifugal settler is controlled in 100~150r/min.
Further scheme also has：Above-mentioned step 3. in, the concentration value accuracy of detection of ion gauge reaches
0.0001mol/L；Trace impurity ion is removed with electrochemical process.
The present invention has positive effect：（1）Overcritical composite electroformed system recycle device of the invention, by setting
Pneumatic filter is put, the CO in overcritical electroforming system can be effectively reclaimed2Gas is used for repetitive cycling, it is to avoid CO2Gas
Being directly discharged into air can aggravate Global Greenhouse Effect；Reactor can be prevented effectively from by the setting of gas filter simultaneously to arrange
Electroforming solution causes discharge duct to block with gas into pipeline during gas, substantially increases the service life of pipeline and valve.（2）This
The overcritical composite electroformed system recycle device of invention, can effectively be reclaimed by the design of structure, when using and used
Composite electroformed liquid and wherein useful solid particle use for repetitive cycling, so as to improve electroforming solution in composite electroformed liquid
With the utilization rate of solid particle, composite electrodeposition processing cost is effectively reduced.（3）Overcritical composite electroformed system of the invention is returned
Receipts utilize device, and it is made by reclaiming used composite electroformed liquid and wherein useful solid particle repetitive cycling when in use
With can not only reduce processing cost, and be effectively reduced processing-waste and waste residue pollution on the environment, environmental protection.
Brief description of the drawings
Fig. 1 is structural representation of the invention, and it is also show in figure with the reactor of overcritical composite electroformed device
Air-liquid annexation；
Fig. 2 is the structural representation of pneumatic filter in Fig. 1；
Fig. 3 is the structural representation of the composite particles recover in Fig. 1.
Reference in above-mentioned accompanying drawing is as follows：
Reactor 100,
Control valve group 1, gas liquid mixture discharge control valve 1-1, electroforming solution discharge control valve 1-2, the input control of reactor gas
Valve 1-3, gas supply control valve 1-4；
Pneumatic filter 2, gas-liquid separation chamber 21, baffle plate 21-1, gas filtration room 22, gas hothouse 23,
Gas reservoir 3
Electroforming solution memory 4,
Magnetic drive pump 5,
Electroforming solution detection allotment component 6, ion detection groove 61, ion gauge 62, composite electroformed liquid surge-tank 63,
Composite particles recover 7, burning unit 71, sedimentation separation unit 72, cleaning-drying unit 73, detection unit 74,
High-pressure pump 8,
CO2Gas cylinder 9,
Pressure gauge 10.
Specific embodiment
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
（Embodiment 1）
See Fig. 1 to Fig. 3, the overcritical composite electroformed system recycle device of the present embodiment is applied to overcritical composite electroformed
Processing unit (plant), the core devices of overcritical composite electroformed device are reactor 100, reactor 100 have leakage fluid dram, exhaust outlet and
Air inlet.
The overcritical composite electroformed system recycle device of the present embodiment, mainly by control valve group 1, pneumatic filter 2,
Gas reservoir 3, electroforming solution memory 4, magnetic drive pump 5, electroforming solution detection allotment component 6, composite particles recover 7, high-pressure pump
8、CO2Gas cylinder 9 and pressure gauge 10 are constituted.
Control valve group 1 includes that gas liquid mixture discharge control valve 1-1, electroforming solution discharge control valve 1-2, reactor gas are defeated
Enter to control valve 1-3 and gas supply control valve 1-4.
Pneumatic filter 2 includes that the gas-liquid separation chamber 21 that sets gradually and ventilate from top to bottom, gas filtration room 22 are gentle
Body hothouse 23.The lower end of gas-liquid separation chamber 21 is provided with gaseous mixture input port；It is provided with gas-liquid separation chamber 21 and connect successively arrangement
One group of baffle plate 21-1, the downward-sloping angular ranges of baffle plate 21-1 be 8~16 °；It is solid filled with cupric oxide in gas filtration room 22
Body, and leave certain hole；Adding thermal resistance is set between the inside and outside wall of gas filtration room 22 so that temperature control during its work
At 200 degrees Celsius；Gas hothouse 23 is provided with gas recovery delivery outlet；Solid calcium chloride is filled with gas hothouse 23, and
Leave certain hole；Temperature when gas hothouse 23 works is normal temperature；The gaseous mixture input port of gas-liquid separation chamber 21 is by control
The gas liquid mixture discharge control valve 1-1 of valve group processed 1 is connected with the exhaust outlet of reactor 100.
Gas reservoir 3 has recovery gas input port, tonifying Qi input port and air supply opening；The recovery gas of gas reservoir 3 is defeated
Entrance is connected with the gas recovery delivery outlet of the gas hothouse 23 of pneumatic filter 2；The tonifying Qi input port of gas reservoir 3
By high-pressure pump 8 and gas supply control valve 1-4 and CO2Gas cylinder 9 is connected；The air supply opening of gas reservoir 3 passes through reactor gas
Input control valve 1-3 is connected with the air inlet of reactor 100.The inwall of gas reservoir 3 is provided with circulating cooling water pipe；For
Operationally internal temperature is 2 DEG C or so to control gas reservoir 3.
Electroforming solution memory 4 is provided with inlet, liquid outlet and magnetic stirring apparatus, and magnetic stirring apparatus is arranged on electroforming solution storage
The bottom of device 4, the rotating speed of magnetic stirring apparatus is 400~600r/min during work.The inlet of electroforming solution memory 4 passes through electroforming
Liquid discharge control valve 1-2 is connected with the leakage fluid dram of reactor 100.
Magnetic drive pump 5 is provided with inlet, liquid outlet and detachable absorption filter element, and detachable absorption filter element is arranged on magnetic force
The inside of pump 5；Magnetic drive pump 5 preferably uses MP Micro magnetic driving pumps；Filter core selects stainless steel filter core or collapsible micropore filter element, filter core
Outer wrap double-layer filter cloth.The inlet of magnetic drive pump 5 is connected with the liquid outlet of electroforming solution memory 4.
Electroforming solution detection allotment component 6 includes ion detection groove 61, ion gauge 62 and composite electroformed liquid surge-tank 63.
Ion detection groove 61 is provided with inlet, liquid outlet, detection liquid outlet and waste discharge mouth；The inlet and magnetic drive pump of ion detection groove 61
5 liquid outlet is connected；Ion gauge 62 is connected by the detection liquid outlet of ion detection groove 61 with ion detection groove 61；
The waste discharge mouth of ion detection groove 61 is used to discharge waste liquid；The liquid outlet of ion detection groove 61 is connected with composite electroformed liquid surge-tank 63
Connect.
Composite particles recover 7 is used to reclaim the useful solid particle in the composite electroformed liquid of the releasing of reactor 100.It is compound
Particle recover 7 is main to be made up of burning unit 71, sedimentation separation unit 72, cleaning-drying unit 73 and detection unit 74.
Burning unit 71 is used to carry out at burning the solid particle that the detachable absorption filter element by magnetic drive pump 5 is reclaimed
Reason plays a part of decrement loss of weight to remove the organic matter in solid particle and moisture, and incineration ashes are comprising heavy metal particles
With the solid particle needed for the configuration of composite electroformed liquid；Temperature control is burned when unit 71 works at 500 DEG C or so, the time is 5~
10min。
The core devices of sedimentation separation unit 72 are composite particles centrifugal settler；The bottom of composite particles centrifugal settler
Circular electromagnets are set；Solvent selects distilled water or deionized water.Sedimentation separation unit 72 is used for the burning to burning unit 71
Product carries out centrifugal sedimentation separation so that solid particle and heavy metal particles point in incineration ashes needed for composite electroformed liquid configuration
From；The waste residue that sedimentation separation unit 72 sinks to the bottom is processed using conventional anodes mud processing mode, and heavy metal therein is carried out
Refine.
The solid particle that being cleaned and dried unit 73 is used for needed for being configured to the composite electroformed liquid isolated is cleaned and dried；
The solid particle needed for the configuration of composite electroformed liquid after 74 pairs of cleaning-dryings of detection unit is detected, if Testing index meets electricity
Casting requires, is sent to composite electroformed liquid surge-tank 63 and recycles；If Testing index is not up to electroforming requirement, continued
Input sedimentation separation unit 72 is processed.
High-pressure pump 8 and CO2Gas cylinder 9 is used for as CO in gas reservoir 32To supplementing CO in gas reservoir 3 when not enough2Gas
Body.
Pressure gauge 10 is arranged between reactor gas input control valve 1-3 and the air inlet of reactor 100；Pressure gauge 10
For detecting the air pressure in reactor 100.
The overcritical composite electroformed system recycle device of the present embodiment is when in use to overcritical composite electroformed system
Recycling process, illustrated as a example by being the composite electroformed liquid of Ni-based diamond in reactor 100：
After hours, due to the heat-insulating property of reactor 100, the temperature of overcritical electroforming system is tieed up for electroforming in reactor 100
Hold in operating temperature；Slow to open gas liquid mixture discharge control valve 1-1, the mixed gas in reactor 100 flow to gas mistake
Filter 2, at 200 degrees Celsius, the temperature of gas hothouse 23 is normal temperature to the temperature control of gas filtration room 22 of pneumatic filter 2,
Central micro hydrogen and water vapour are removed by mixed gas after the gentle body hothouse 23 in gas filtration room 22, purification is reached
Effect；As gas liquid mixture discharge control valve 1-1 openings are increased, the liquid electroforming solution in reactor 100 can be with mixing
Gas sprays and enters gas-liquid separation chamber 21, the one group of effective ground resistance of baffle plate 21-1 set in gas-liquid separation chamber 21 of gas-liquid separation chamber 21
Every liquid, meanwhile, baffle plate 21-1 has downward angle of inclination, is conducive to remaining in the electroforming solution on baffle plate 21-1 in itself weight
Reactor 100 is slid back step by step under power effect；Mixed gas after vapor-liquid separation are by the gentle body hothouse in gas filtration room 22
After 23, it is collected in through in overcooled gas reservoir 3, the internal temperature control of gas reservoir 3 is at 2 DEG C or so；When gas is deposited
CO in reservoir 32When not enough, can be by CO2Gas cylinder 9 is supplemented.
Electroforming solution discharge control valve 1-2 is opened, the composite electroformed liquid in reactor 100 is collected in electroforming solution memory 4,
After being collected into a certain amount of, start the magnetic stirring apparatus of electroforming solution memory 4 to larger rotating speed, make insoluble in composite electroformed liquid
Property solid particle effectively disperse suspend；Magnetic drive pump 5 extracts the composite electroformed liquid in electroforming solution memory 4, and composite electroformed liquid passes through
The detachable absorption filter element of magnetic drive pump 5 is flowed in ion detection groove 61 after filtering；Diamond particles in composite electroformed liquid and
The earth of positive pole effectively is intercepted by the detachable absorption filter element of magnetic drive pump 5, and diamond particles and earth of positive pole mixture are collected
Reach it is a certain amount of after be put into the burning unit 71 of composite particles recover 7 and carry out burning disposal, burn the temperature control of unit 71 and exist
500 DEG C or so, the time is 5~10min；The organic matter and moisture in effectively removal mixture are burned, decrement loss of weight is played
Effect；Incineration ashes are crossed into water in sedimentation separation unit 72 to clean, is put into composite particles centrifugal settler, centrifugal settler
Rotating speed it is slower, control in 100~150r/min；Because by burning disposal, the solid particle in mixture is only comprising a huge sum of money
Metal particles and diamond particles, in the presence of sedimentation liquid and centrifugal force, diamond particles can be suspended in solution due to lightweight
Upper strata, and heavy metal particles are in lower floor because quality is big, and with certain magnetic, easily adsorbed by bottom electromagnet；
Take upper strata aaerosol solution and be filtrated to get diamond particles, cleaned drying unit 73 is cleaned and dried to obtain diamond particles powder
End；The purity of the diamond particles powder that detection unit 74 pairs is obtained detects, if meeting electroforming requirement, sends into compound electric
Casting liquid surge-tank 63 is recycled；If not up to electroforming requirement, being continued input sedimentation separation unit 72 carries out repeating sieve
Select removal process.The remaining waste residue of centrifugal settler bottom can be carried out by conventional anodes mud processing mode to heavy metal therein
Refine and reclaim.
Ion gauge 62 is pumped into each ion in the composite electroformed liquid in ion detection groove 61 after being filtered to magnetic drive pump 5
Composition and content are detected；Micro metal impurities ion to being detected in composite electroformed liquid is gone using electrochemical method
Remove；Can be supplemented with nickel sulfate, nickel chloride or nickel hydroxide for nickel ion, control pH value so that composite electroformed liquid reaches
Parameter Conditions to needed for electroforming；Deployed composite electroformed liquid is imported in composite electroformed liquid surge-tank 63, and addition includes reclaiming
Diamond particles in interior a certain amount of diamond particles, by certain pretreatment, obtain meeting the compound of electroforming requirement
Electroplate liquid, is used with repetitive cycling.
The recycle device of the overcritical composite electroformed system of the present embodiment, its method of work mainly includes following step
Suddenly：
1. gas is reclaimed：Open the gas liquid mixture discharge control valve 1-1 of control valve group 1 so that the constant temperature of reactor 100 is depressurized to
One atmospheric pressure, gas-liquid separation chamber 21, the gas filtration room 22 of mixed gas inside reactor 100 by pneumatic filter 2
The interior circulation of gas reservoir 3 is collected in after the gentle purification processes of body hothouse 23 to use；
Wherein, the operating pressure of reactor is 8~20MPa, and operating temperature is 35~70 DEG C；The internal temperature of gas reservoir 3
Control is at 2 DEG C or so；
Gas exhausting valve should be opened slowly；The temperature control of gas filtration room 22 reacts dehydrogenation at 200 DEG C or so for replacing
Gas；
Electroforming solution is Ni-based or copper-based composite casting liquid, and pH value is 2~6, and hard composite particles are diamond, SiC and Al2O3Deng,
Particle diameter is nanoscale.
2. solid particle is reclaimed：
The first step：Electroforming solution discharge control valve 1-2 is opened, the composite electroformed liquid in reactor 100 is collected in electroforming solution storage
In device 4, start the magnetic stirring apparatus of electroforming solution memory 4, make the insoluble solid particle effectively dispersion in composite electroformed liquid outstanding
It is floating；The rotating speed of magnetic stirring apparatus is 400~600r/min in electroforming solution memory；
Second step：Magnetic drive pump 5 extracts the composite electroformed liquid in electroforming solution memory 4, and composite electroformed liquid is removable by magnetic drive pump 5
Unloading in flow to ion detection groove 61 after the filtering of formula absorption filter element, into step 3.；Solid particle in composite electroformed liquid is by magnetic force
The detachable absorption filter element of pump 5 be collected into it is a certain amount of after transfer to composite particles recover 7 to process；
3rd step：Solid particle in the composite electroformed liquid collected by the detachable absorption filter element of magnetic drive pump 5 is successively through compound
The burning unit 71 of particle recover 7 carries out burning disposal, sedimentation separation unit 72 to be carried out centrifugal sedimentation separation, is cleaned and dried list
Unit 73 cleaning-drying and the purity detecting of detection unit 74, obtain recyclable recycling composite electroformed liquid configuration needed for
Solid particle；
, at 500 DEG C, the time of burning is 5~10 minutes to burn temperature control when unit 71 works；The sedimentation separation unit 72
The rotating speed of composite particles centrifugal settler is controlled in 100~150r/min.
3. electroforming solution goes the removal of impurity：The electroforming of solid particle is eliminated after the detachable absorption filter element filtering of magnetic drive pump 5
After liquid flows into ion detection groove 61, the composition and concentration of various ions in electroforming solution are detected by ion gauge 62, as required
Removal wherein trace impurity ion, the ion that supplement electroforming solution needs, obtains satisfactory electroforming solution；Detection is not up to standard to consolidate
Body particle puts into sedimentation separation unit 72 and processes again；
The concentration value of ion gauge 62 can be accurate to 0.0001mol/L；Trace impurity ion is removed with electrochemical process.
4. composite electroformed liquid is allocated：By step 2. in obtain composite electroformed liquid configuration needed for solid particle and step
3. the electroforming solution obtained in is deployed into and meets the compound of electroforming requirement according to set proportion in composite electroformed liquid surge-tank 63
Electroforming solution is for recycling.
Above example is the explanation to specific embodiment of the invention, rather than limitation of the present invention, relevant technology
The technical staff in field without departing from the spirit and scope of the present invention, can also make various conversion and change and obtain
To corresponding equivalent technical scheme, therefore all equivalent technical schemes should be included into patent protection model of the invention
Enclose.
Claims (1)
1. a kind of overcritical composite electroformed system recycle device, including reactor（100）, reactor（100）With discharge opeing
Mouth, exhaust outlet and air inlet；It is characterized in that：Also include control valve group（1）, pneumatic filter（2）, gas reservoir（3）, electricity
Casting liquid memory（4）, magnetic drive pump（5）, electroforming solution detection allotment component（6）, composite particles recover（7）, high-pressure pump（8）、CO2
Gas cylinder（9）And pressure gauge（10）；
Described control valve group（1）Including gas liquid mixture discharge control valve（1-1）, electroforming solution discharge control valve（1-2）, reaction
Kettle gas input control valve（1-3）With gas supply control valve（1-4）；
Pneumatic filter（2）Including the gas-liquid separation chamber for setting gradually from top to bottom and mutually ventilate（21）, gas filtration room（22）
Gentle body hothouse（23）；Gas-liquid separation chamber（21）By control valve group（1）Gas liquid mixture discharge control valve（1-1）With it is anti-
Answer kettle（100）Exhaust outlet be connected；
Gas reservoir（3）It is provided with recovery gas input port, tonifying Qi input port and air supply opening；Gas reservoir（3）Recovery gas it is defeated
Entrance and pneumatic filter（2）Gas hothouse（23）It is connected；Gas reservoir（3）Tonifying Qi input port pass through high-pressure pump
（8）With gas supply control valve（1-4）With CO2Gas cylinder（9）It is connected；Gas reservoir（3）Air supply opening by reactor gas it is defeated
Enter to control valve（1-3）With reactor（100）Air inlet be connected；
Electroforming solution memory（4）It is provided with inlet, liquid outlet and magnetic stirring apparatus；Magnetic stirring apparatus is arranged on electroforming solution memory
（4）Bottom；Electroforming solution memory（4）Inlet by electroforming solution discharge control valve（1-2）With reactor（100）Discharge opeing
Mouth is connected；
Magnetic drive pump（5）It is provided with inlet, liquid outlet and detachable absorption filter element；Magnetic drive pump（5）Inlet deposited with electroforming solution
Reservoir（4）Liquid outlet be connected；
Electroforming solution detection allotment component（6）Including ion detection groove（61）, ion gauge（62）With composite electroformed liquid surge-tank
（63）；Ion detection groove（61）It is provided with inlet, liquid outlet, detection liquid outlet and waste discharge mouth；Ion detection groove（61）Feed liquor
Mouth and magnetic drive pump（5）Liquid outlet be connected；Ion gauge（62）By ion detection groove（61）Detection liquid outlet with from
Sub- detect tank（61）It is connected；Ion detection groove（61）Waste discharge mouth be used for discharge waste liquid；Ion detection groove（61）Liquid outlet
With composite electroformed liquid surge-tank（63）It is connected；
Composite particles recover（7）For reclaiming reactor（100）Useful solid particle in the composite electroformed liquid released；It is compound
Particle recover（7）Including burning unit（71）, sedimentation separation unit（72）, be cleaned and dried unit（73）And detection unit
（74）；
High-pressure pump（8）And CO2Gas cylinder（9）For working as gas reservoir（3）Interior CO2To gas reservoir when not enough（3）Interior supplement
CO2Gas；Pressure gauge（10）For detecting reactor（100）Interior air pressure, pressure gauge（10）It is arranged on the input of reactor gas
Control valve（1-3）With reactor（100）Air inlet between；
Described pneumatic filter（2）Gas-liquid separation chamber（21）Lower end be provided with gaseous mixture input port；Gas-liquid separation chamber（21）
Inside it is provided with one group of downward-sloping baffle plate（21-1）, baffle plate（21-1）Downward-sloping angular range is 8~16 °；Gas filtration room
（22）It is interior filled with cupric oxide solid；Gas filtration room（22）Inside and outside wall between be provided with adding thermal resistance；Gas hothouse
（23）It is provided with gas recovery delivery outlet；Gas hothouse（23）It is interior filled with solid calcium chloride；
Described gas reservoir（3）Inwall be provided with for controlling gas reservoir（3）Operationally internal temperature is 2 DEG C
Circulating cooling water pipe；
Described electroforming solution memory（4）Magnetic stirring apparatus work when rotating speed be 400~600r/min.
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| CN201510241096.5A Active CN104846406B (en) | 2015-05-12 | 2015-05-12 | supercritical composite electroforming system recycling device and working method thereof |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN106801235A (en) | 2017-06-06 |
| CN106811773B (en) | 2018-06-08 |
| CN106801235B (en) | 2018-06-08 |
| CN104846406A (en) | 2015-08-19 |
| CN106868577A (en) | 2017-06-20 |
| CN106868577B (en) | 2018-06-08 |
| CN104846406B (en) | 2017-03-08 |
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