CN106811773B - Supercritical composite electroforming system recycling device - Google Patents
Supercritical composite electroforming system recycling device Download PDFInfo
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- CN106811773B CN106811773B CN201710068972.8A CN201710068972A CN106811773B CN 106811773 B CN106811773 B CN 106811773B CN 201710068972 A CN201710068972 A CN 201710068972A CN 106811773 B CN106811773 B CN 106811773B
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- 238000005323 electroforming Methods 0.000 title claims abstract description 93
- 239000002131 composite material Substances 0.000 title claims abstract description 85
- 238000004064 recycling Methods 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 133
- 238000001514 detection method Methods 0.000 claims abstract description 54
- 239000002245 particle Substances 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- 238000000926 separation method Methods 0.000 claims abstract description 42
- 239000007787 solid Substances 0.000 claims abstract description 40
- 239000011246 composite particle Substances 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 23
- 238000011084 recovery Methods 0.000 claims abstract description 6
- 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 15
- 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
- 239000008246 gaseous mixture Substances 0.000 claims description 4
- 239000013589 supplement 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
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 229910000431 copper oxide Inorganic materials 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 238000001035 drying Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 8
- 238000003860 storage Methods 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract 6
- 239000007789 gas Substances 0.000 description 107
- 239000012530 fluid Substances 0.000 description 12
- 239000010432 diamond Substances 0.000 description 11
- 229910003460 diamond Inorganic materials 0.000 description 11
- 230000008569 process Effects 0.000 description 7
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000002923 metal particle Substances 0.000 description 5
- 238000007747 plating Methods 0.000 description 5
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 4
- 239000002956 ash Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 230000001351 cycling effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000003252 repetitive effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004070 electrodeposition Methods 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 239000004615 ingredient 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
- 239000000126 substance Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 210000005056 cell body Anatomy 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 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
- 238000012360 testing method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 230000009471 action Effects 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
- 230000004888 barrier function Effects 0.000 description 1
- 238000004140 cleaning Methods 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
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 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
- 230000005484 gravity Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 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
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research 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
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 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
- C25D1/00—Electroforming
-
- 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
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 vacuum pump, a vacuum,Gas storage, electroforming liquid storage, magnetic pump, electroforming liquid detection and blending assembly, composite particle recoverer, high-pressure pump and 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; the composite particle recoverer is used for recovering useful solid particles in the composite electroforming liquid; 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. is 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 fields, and in particular to a kind of overcritical composite electroformed system recycling 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 is current or even following will all play the part of important angle
Color.
Supercritical fluid（Supercritical Fluid）Refer to that pure substance is in critical point（Critical pressure and critical
Temperature）More than when, showed one kind between liquid and gaseous fluid.In recent years, composite electroformed technology is faced with super
Boundary's fluid technique is combined, and is a research hotspot for preparing High performance nanometer composite material.At present, it is electric under supercritical environment
Deposition prepares the process of nanocomposite and micro-workpiece and device has finding.If Authorization Notice No. is CN
The Chinese patent literature of 101092716B discloses a kind of subtle electroforming technique of supercritical fluid and its device, with SCF-
CO2Carry out the molding of micro-structure part for plating environment, metal plating layer surface depositing homogeneous as obtained by this method, without product
Knurl, and cast layer tissue is fine and closely woven smooth；The Chinese patent literature that for another example publication No. is CN 102146573A proposes a kind of overcritical
The method that fluid electrotyping forming prepares nanocomposite, mainly electro-deposition prepares metal under mechanical agitation subsidiary conditions
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；Moreover, CO2Global Greenhouse Effect can be aggravated by being directly discharged into air；And chemical plating fluid is to environment dirt
Dye influences significantly, to be directly discharged into the Nature, be 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 be remaining a part of, furthermore prepare the especially nano level cost of compound particle very
Height, thus the compound particle recycling cast in liquid is relatively inexpensive.
Invention content
The purpose of the present invention is：For supercritical CO2Composite electroformed system can recycle CO when providing a kind of use2Gas
Particle is fixed required for body, electroforming solution and electroforming as a means of recycling, so as to effectively improve the service efficiency of electroforming solution, reduction pair
The pollution of environment, the overcritical composite electroformed system recycle device and its method of work for reducing composite electroformed financial cost.
The technical scheme is that：The overcritical composite electroformed system recycle device of the present invention, including reaction kettle,
Reaction kettle has leakage fluid dram, exhaust outlet and air inlet；It is structurally characterized in that：Control valve group, pneumatic filter, gas is further included to deposit
Reservoir, electroforming solution memory, magnetic drive pump, electroforming solution detection allotment component, composite particles recover, high-pressure pump, CO2Gas cylinder and pressure
Power table；
It is defeated that above-mentioned control valve group includes gas liquid mixture discharge control valve, electroforming solution discharge control valve, reaction kettle gas
Enter control valve and gas supply control valve；
Pneumatic filter includes the gas-liquid separation chamber for setting gradually and mutually ventilating from top to bottom, the gentle soma in gas filtration room
Dry room；Gas-liquid separation chamber discharges control valve by the gas liquid mixture of control valve group and is connected with the exhaust outlet of reaction kettle；
Gas reservoir is equipped with recycling gas input port, tonifying Qi input port and air supply opening；The recycling gas input of gas reservoir
Mouth is connected with the gas dry room of pneumatic filter；The tonifying Qi input port of gas reservoir passes through high-pressure pump and gas supply control valve
With CO2Gas cylinder is connected；The air inlet phase that the air supply opening of gas reservoir passes through reaction kettle gas input control valve and reaction kettle
Connection；
Electroforming solution memory is equipped with inlet, liquid outlet and magnetic stirring apparatus；Magnetic stirring apparatus is arranged on electroforming solution storage
The bottom of device；The inlet of electroforming solution memory discharges control valve by electroforming solution and is connected with the leakage fluid dram of reaction kettle；
Magnetic drive pump is equipped with inlet, liquid outlet and detachable absorption filter element；The inlet of magnetic drive pump is stored with electroforming solution
The liquid outlet of device is connected；
Electroforming solution detection allotment component includes ion detection slot, ion gauge and composite electroformed liquid surge-tank；Ion is examined
It surveys slot and is equipped with inlet, liquid outlet, detection liquid outlet and waste discharge mouth；The liquid outlet phase of the inlet of ion detection slot and magnetic drive pump
Connection；Ion gauge is connected by the detection liquid outlet of ion detection slot with ion detection slot；The waste discharge of ion detection slot
Mouth is used to discharge waste liquid；The liquid outlet of ion detection slot is connected with composite electroformed liquid surge-tank；
Composite particles recover is used for the useful solid particle in the composite electroformed liquid for recycling reaction kettle releasing；Composite particles
Recover 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 reservoir2CO is supplemented when insufficient into gas reservoir2Gas；Pressure
Power table is used to detecting air pressure in reaction kettle, pressure gauge be arranged on reaction kettle gas input control valve and reaction kettle air inlet it
Between；
The lower end of the gas-liquid separation chamber of above-mentioned pneumatic filter is equipped with gaseous mixture input port；In gas-liquid separation room be equipped with to
Under inclined one group of baffle, baffle tilts down angular range as 8~16 °；Copper oxide solid is filled in gas filtration room；Gas
Adding thermal resistance is provided between the inside and outside wall of body filter chamber；Gas dry room is equipped with gas recovery delivery outlet；In gas dry room
Filled with solid calcium chloride；
The inner wall of above-mentioned gas reservoir is equipped with that internal temperature is 2 DEG C and follows at work for controlling gas reservoir
Ring cooling water pipe；
Rotating speed during the magnetic stirring apparatus work of above-mentioned electroforming solution memory is 400~600r/min.
Further embodiment 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 outside package double-layer filter cloth.
Further embodiment also has：The unit that burns of above-mentioned composite particles recover is used for passing through the removable of magnetic drive pump
The solid particle for unloading the recycling of formula absorption filter element carries out burning disposal；
Sedimentation separation unit includes composite particles centrifugal settler；Sedimentation separation unit is used to produce the burning for burning unit
Object carries out centrifugal sedimentation separation so that solid particle and heavy metal particles point in incineration ashes needed for composite electroformed liquid configuration
From；
Unit is cleaned and dried for being cleaned and dried to the solid particle needed for the composite electroformed liquid isolated configuration；
Detection unit is used to make to whether the solid particle needed for the composite electroformed liquid configuration after cleaning-drying meets cycle
It is detected with standard.
The method of work of above-mentioned overcritical composite electroformed system recycle device, includes the following steps：
1. gas recycles：Open the gas liquid mixture discharge control valve of control valve group so that reactor constant temperature is depressurized to one
A atmospheric pressure, the mixed gas inside reaction kettle pass through gas-liquid separation chamber, gas filtration room and the gas dry of pneumatic filter
It is collected in gas reservoir and recycles after the purification processes of room；
2. solid particle recycles：
The first step：Electroforming solution discharge control valve is opened, the composite electroformed liquid in reaction kettle is collected in electroforming solution memory
In, start the magnetic stirring apparatus of electroforming solution memory, the insoluble solid particle in composite electroformed liquid is made effectively to disperse to suspend；
Second step：Magnetic drive pump extracts the composite electroformed liquid in electroforming solution memory, and composite electroformed liquid can by magnetic drive pump
It flows in ion detection slot, is entered step 3. after the filtering of detachable absorption filter element；Solid particle in composite electroformed liquid is by magnetic force
Pump detachable absorption filter element be collected into it is a certain amount of after transfer to composite particles recover handle；
Third walks：Solid particle in the composite electroformed liquid collected by the detachable absorption filter element of magnetic drive pump is successively through multiple
The burning unit for closing particle recover carries out burning disposal, sedimentation separation unit carries out centrifugal sedimentation separation, is cleaned and dried unit
Cleaning-drying and detection unit purity detecting, obtain recyclable recycling composite electroformed liquid configuration needed for solid
Grain；Detection solid particle not up to standard puts into sedimentation separation cell processing again；
3. electroforming solution removes impurity：The electroforming solution of solid particle is eliminated after the detachable absorption filter element filtering of magnetic drive pump
After flowing into ion detection slot, the ingredient and concentration of various ions in electroforming solution are detected by ion gauge, removes it as required
Middle trace impurity ion, the ion that supplement electroforming solution needs, obtains satisfactory electroforming solution；
4. allocate composite electroformed liquid：By step 2. in obtain composite electroformed liquid configuration needed for solid particle and step
3. the electroforming solution obtained in is deployed into the compound electric for meeting electroforming requirement according to set proportion in composite electroformed liquid surge-tank
Liquid is cast for recycling.
Further embodiment is：Above-mentioned step 1. in, gas filtration room work when temperature control at 200 degrees Celsius；
Temperature when gas dry room works is room temperature.
Further embodiment is：In the third step of above-mentioned step 2., during the burning cell operation of composite particles recover
At 500 DEG C, the burning time is 5~10min for 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 embodiment 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）The overcritical composite electroformed system recycle device of the present invention, by setting
Pneumatic filter is put, can effectively recycle the CO in overcritical electroforming system2Gas uses for repetitive cycling, avoids CO2Gas
Global Greenhouse Effect can be aggravated by being directly discharged into air；Effectively reaction kettle can be avoided to arrange by the setting of steam filter simultaneously
Electroforming solution enters pipeline with gas discharge duct is caused to block during gas, substantially increases the service life of pipeline and valve.（2）This
The overcritical composite electroformed system recycle device of invention, by the design of structure, when use, which can effectively recycle, to be used
Composite electroformed liquid and wherein useful solid particle for repetitive cycling use, 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）The overcritical composite electroformed system of the present invention is returned
It receives using device, is made when in use by recycling used composite electroformed liquid and wherein useful solid particle repetitive cycling
With, processing cost can be not only reduced, and processing-waste and waste residue pollution on the environment can be effectively reduced, it is environmentally protective.
Description of the drawings
Fig. 1 is the structural diagram of the present invention, its reaction kettle with overcritical composite electroformed device is also shown in figure
Air-liquid connection relation；
Fig. 2 is the structure diagram of pneumatic filter in Fig. 1；
Fig. 3 is the structure diagram of the composite particles recover in Fig. 1.
Reference numeral in above-mentioned attached drawing is as follows：
Reaction kettle 100,
Control valve group 1, gas liquid mixture discharge control valve 1-1, electroforming solution discharge control valve 1-2, the input of reaction kettle gas
Control valve 1-3, gas supply control valve 1-4；
Pneumatic filter 2, gas-liquid separation chamber 21, baffle 21-1, gas filtration room 22, gas dry room 23,
Gas reservoir 3
Electroforming solution memory 4,
Magnetic drive pump 5,
Electroforming solution detection allotment component 6, ion detection slot 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 will be further described in detail below with reference to the accompanying drawings and specific embodiments.
（Embodiment 1）
See Fig. 1 to Fig. 3, the overcritical composite electroformed system recycle device of the present embodiment, applied to overcritical compound
Eletroforming device, the core devices of overcritical composite electroformed device are reaction kettle 100, and reaction kettle 100 has leakage fluid dram, exhaust
Mouth 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 form.
It is defeated that control valve group 1 includes gas liquid mixture discharge control valve 1-1, electroforming solution discharge control valve 1-2, reaction kettle gas
Enter control valve 1-3 and gas supply control valve 1-4.
It is gentle that pneumatic filter 2 includes the gas-liquid separation chamber 21 that sets gradually and ventilate from top to bottom, gas filtration room 22
Body hothouse 23.The lower end of gas-liquid separation chamber 21 is equipped with gaseous mixture input port；The arrangement that connects successively is equipped in gas-liquid separation chamber 21
One group of baffle 21-1, baffle 21-1 tilts down angular range as 8~16 °；Consolidate in gas filtration room 22 filled with copper oxide
Body, and there are certain holes；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 dry room 23 is equipped with gas recovery delivery outlet；Filled with solid calcium chloride in gas dry room 23, and
There are certain holes；Temperature when gas dry room 23 works is room temperature；The gaseous mixture input port of gas-liquid separation chamber 21 passes through control
The gas liquid mixture discharge control valve 1-1 of valve group 1 processed is connected with the exhaust outlet of reaction kettle 100.
Gas reservoir 3 has recycling gas input port, tonifying Qi input port and air supply opening；The recycling gas of gas reservoir 3 is defeated
Entrance is connected with the gas recovery delivery outlet of the gas dry room 23 of pneumatic filter 2；The tonifying Qi input port of gas reservoir 3
Pass through 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 reaction kettle gas
Input control valve 1-3 is connected with the air inlet of reaction kettle 100.The inner wall of gas reservoir 3 is equipped with circulating cooling water pipe；For
Controlling gas reservoir 3, internal temperature is 2 DEG C or so at work.
Electroforming solution memory 4 is equipped 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 reaction kettle 100.
Magnetic drive pump 5 is equipped 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
Outside package 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 slot 61, ion gauge 62 and composite electroformed liquid surge-tank 63.
Ion detection slot 61 is equipped with inlet, liquid outlet, detection liquid outlet and waste discharge mouth；The inlet and magnetic drive pump of ion detection slot 61
5 liquid outlet is connected；Ion gauge 62 is connected by the detection liquid outlet of ion detection slot 61 with ion detection slot 61；
The waste discharge mouth of ion detection slot 61 is used to discharge waste liquid；The liquid outlet of ion detection slot 61 is connected with composite electroformed liquid surge-tank 63
It connects.
Composite particles recover 7 is used for the useful solid particle in the composite electroformed liquid for recycling the releasing of reaction kettle 100.It is compound
Particle recover 7 is mainly made of burning unit 71, sedimentation separation unit 72, cleaning-drying unit 73 and detection unit 74.
Unit 71 is burned to be used to carry out at burning the solid particle that the detachable absorption filter element by magnetic drive pump 5 recycles
Reason plays the role of being reduced loss of weight, incineration ashes is include heavy metal particles to remove the organic matter and moisture in solid particle
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 for 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 is sunk to the bottom is handled using conventional anodes mud processing mode, and heavy metal therein is carried out
It refines.
Unit 73 is cleaned and dried for being cleaned and dried to the solid particle needed for the composite electroformed liquid isolated configuration；
Detection unit 74 is detected the solid particle needed for the composite electroformed liquid configuration after cleaning-drying, if Testing index meets electricity
Casting requirement, 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 handled.
High-pressure pump 8 and CO2Gas cylinder 9 is used for as CO in gas reservoir 32When insufficient CO is supplemented into gas reservoir 32Gas
Body.
Pressure gauge 10 is arranged between reaction kettle gas input control valve 1-3 and the air inlet of reaction kettle 100；Pressure gauge 10
For detecting the air pressure in reaction kettle 100.
The overcritical composite electroformed system recycle device of the present embodiment is when in use to overcritical composite electroformed system
Recycling process, illustrated for being the composite electroformed liquid of Ni-based diamond in reaction kettle 100：
In reaction kettle 100 electroforming after hours, due to the heat-insulating property of reaction kettle 100, the temperature of overcritical electroforming system
Degree maintains operating temperature；Gas liquid mixture discharge control valve 1-1 is slowly opened, the mixed gas in reaction kettle 100 flows to gas
Body filter 2,22 temperature of gas filtration room of pneumatic filter 2 are controlled at 200 degrees Celsius, and the temperature of gas dry room 23 is normal
Temperature by hydrogen and water vapour micro in mixed gas removing behind gas filtration room 22 and gas dry room 23, reaches and carries
Pure effect；As gas liquid mixture discharge control valve 1-1 openings increase, the liquid electroforming solution in reaction kettle 100 can be with
Mixed gas, which sprays, enters gas-liquid separation chamber 21, and the one group of baffle 21-1 set in 21 gas-liquid separation chamber 21 of gas-liquid separation chamber is effective
Ground liquid barrier, meanwhile, baffle 21-1 has downward angle of inclination, is conducive to remain in the electroforming solution on baffle 21-1 certainly
Reaction kettle 100 is slid back under body gravity step by step；Mixed gas after vapor-liquid separation passes through 22 gentle soma of gas filtration room
Behind dry room 23, it is collected in through in overcooled gas reservoir 3,3 internal temperature control of gas reservoir is at 2 DEG C or so；Work as gas
CO in body memory 32It, can be by CO when insufficient2Gas cylinder 9 supplements.
Electroforming solution discharge control valve 1-2 is opened, the composite electroformed liquid in reaction kettle 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 disperses to suspend；Magnetic drive pump 5 extracts the composite electroformed liquid in electroforming solution memory 4, and composite electroformed liquid passes through
It is flowed in ion detection slot 61 after the detachable absorption filter element filtering of magnetic drive pump 5；Diamond particles in composite electroformed liquid and
The earth of positive pole effectively obstructs by the detachable absorption filter element of magnetic drive pump 5, and diamond particles and earth of positive pole mixture are collected
The burning unit 71 that composite particles recover 7 is put into after reaching a certain amount of carries out burning disposal, burns the control of 71 temperature of unit and exists
500 DEG C or so, the time is 5~10min；The organic matter and moisture effectively removed in mixture is burned, plays decrement loss of weight
Effect；Incineration ashes are crossed water in sedimentation separation unit 72 to clean, are put into composite particles centrifugal settler, centrifugal settler
Rotating speed it is slower, control in 100~150r/min；Due to passing through burning disposal, the solid particle in mixture is only comprising a huge sum of money
Metal particles and diamond particles, under the action of sedimentation liquid and centrifugal force, diamond particles can be suspended in solution due to light-weight
Upper strata, and heavy metal particles are in lower floor since quality is big, and with certain magnetism, are easily adsorbed by bottom electromagnet；
It takes upper strata aaerosol solution and diamond particles is obtained by filtration, cleaned drying unit 73 is cleaned and dried to obtain diamond particles powder
End；Detection unit 74 is detected the obtained purity of diamond particles powder, if meeting electroforming requirement, is sent into compound electric
Casting liquid surge-tank 63 recycles；If not up to electroforming requirement, continued input sedimentation separation unit 72 and carry out repeating sieve
Select removal process.The remaining waste residue of centrifugal settler bottom can carry out heavy metal therein by conventional anodes mud processing mode
Refine recycling.
Ion gauge 62 is pumped into each ion in the composite electroformed liquid in ion detection slot 61 after being filtered to magnetic drive pump 5
Ingredient and content are detected；The micro metal impurities ion detected in composite electroformed liquid is gone using electrochemical method
It removes；Nickel ion with nickel sulfate, nickel chloride or nickel hydroxide can be supplemented, control pH value so that composite electroformed liquid reaches
To the Parameter Conditions needed for electroforming；Deployed composite electroformed liquid is imported in composite electroformed liquid surge-tank 63, and addition includes recycling
Diamond particles including 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, method of work mainly include following step
Suddenly：
1. gas recycles：Open the gas liquid mixture discharge control valve 1-1 of control valve group 1 so that 100 constant temperature of reaction kettle drops
It is depressed into an atmospheric pressure, gas-liquid separation chamber 21 of the mixed gas inside reaction kettle 100 by pneumatic filter 2, gas filtration
It is collected in gas reservoir 3 and recycles after 23 purification processes of room 22 and gas dry room；
Wherein, the operating pressure of reaction kettle is 8~20MPa, and operating temperature is 35~70 DEG C；The inside of gas reservoir 3
Temperature is controlled at 2 DEG C or so；
Gas liquid mixture discharge control valve 1-1 should be opened slowly；The temperature of gas filtration room 22 is controlled at 200 DEG C or so,
For replacing reaction except hydrogen；
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 Al2O3
Deng particle diameter is nanoscale.
2. solid particle recycles：
The first step：Electroforming solution discharge control valve 1-2 is opened, the composite electroformed liquid in reaction kettle 100 is collected in electroforming solution
In memory 4, start the magnetic stirring apparatus of electroforming solution memory 4, the insoluble solid particle in composite electroformed liquid is made effectively to divide
It dissipates and suspends；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 by magnetic drive pump 5
It flows in ion detection slot 61, is entered step 3. after detachable absorption filter element filtering；Solid particle in composite electroformed liquid by
The detachable absorption filter element of magnetic drive pump 5 be collected into it is a certain amount of after composite particles recover 7 is transferred to handle；
Third walks：Solid particle in the composite electroformed liquid collected by the detachable absorption filter element of magnetic drive pump 5 passes through successively
The burning unit 71 of composite particles recover 7 carries out burning disposal, sedimentation separation unit 72 carries out centrifugal sedimentation separation, cleaning is dry
The cleaning-drying of dry unit 73 and the purity detecting of detection unit 74 obtain the composite electroformed liquid configuration institute of recyclable recycling
The solid particle needed；
Burning temperature control when unit 71 works, at 500 DEG C, it is 5~10 minutes to burn the time；The sedimentation separation unit
The rotating speed of 72 composite particles centrifugal settler is controlled in 100~150r/min.
3. electroforming solution removes impurity：The electroforming of solid particle is eliminated after the detachable absorption filter element filtering of magnetic drive pump 5
After liquid stream enters ion detection slot 61, the ingredient 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 handles again；
The concentration value of ion gauge 62 can be accurate to 0.0001mol/L；Trace impurity ion is removed with electrochemical process.
4. allocate composite electroformed liquid：By step 2. in obtain composite electroformed liquid configuration needed for solid particle and step
3. the electroforming solution obtained in is deployed into according to set proportion in composite electroformed liquid surge-tank 63 meets the compound of electroforming requirement
Electroforming solution is for recycling.
Above example is the explanation rather than limitation of the present invention to the specific embodiment of the present invention, related technology
The technical staff in field without departing from the spirit and scope of the present invention, can also make various transformation and variation and obtain
To corresponding equivalent technical solution, therefore all equivalent technical solutions should be included into the patent protection model of the present invention
It encloses.
Claims (1)
1. a kind of overcritical composite electroformed system recycle device, including reaction kettle（100）, reaction kettle（100）With drain
Mouth, exhaust outlet and air inlet；It is characterized in that：Further include control valve group（1）, pneumatic filter（2）, gas reservoir（3）, electricity
Cast 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）；
The control valve group（1）Control valve is discharged including gas liquid mixture（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 and mutually ventilating from top to bottom（21）, gas filtration room（22）
With gas dry room（23）；Gas-liquid separation chamber（21）Pass through 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）Equipped with recycling gas input port, tonifying Qi input port and air supply opening；Gas reservoir（3）Recycling gas it is defeated
Entrance and pneumatic filter（2）Gas dry room（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 it is defeated by reaction kettle gas
Enter control valve（1-3）With reaction kettle（100）Air inlet be connected；
Electroforming solution memory（4）Equipped with inlet, liquid outlet and magnetic stirring apparatus；Magnetic stirring apparatus is arranged on electroforming solution memory
（4）Bottom；Electroforming solution memory（4）Inlet control valve is discharged by electroforming solution（1-2）With reaction kettle（100）Drain
Mouth is connected；
Magnetic drive pump（5）Equipped 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 slot（61）, ion gauge（62）With composite electroformed liquid surge-tank
（63）；Ion detection slot（61）Equipped with inlet, liquid outlet, detection liquid outlet and waste discharge mouth；Ion detection slot（61）Feed liquor
Mouth and magnetic drive pump（5）Liquid outlet be connected；Ion gauge（62）Pass through ion detection slot（61）Detection liquid outlet with from
Sub- detect tank（61）It is connected；Ion detection slot（61）Waste discharge mouth for discharging waste liquid；Ion detection slot（61）Liquid outlet
With composite electroformed liquid surge-tank（63）It is connected；
Composite particles recover（7）For recycling reaction kettle（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 insufficient（3）Interior supplement
CO2Gas；Pressure gauge（10）For detecting reaction kettle（100）Interior air pressure, pressure gauge（10）It is arranged on the input of reaction kettle gas
Control valve（1-3）With reaction kettle（100）Air inlet between；
The pneumatic filter（2）Gas-liquid separation chamber（21）Lower end be equipped with gaseous mixture input port；Gas-liquid separation chamber（21）
It is interior equipped with tilt down one group of baffle（21-1）, baffle（21-1）It is 8~16 ° to tilt down angular range；Gas filtration room
（22）It is interior to be filled with copper oxide solid；Gas filtration room（22）Inside and outside wall between be provided with adding thermal resistance；Gas dry room
（23）Equipped with gas recovery delivery outlet；Gas dry room（23）It is interior to be filled with solid calcium chloride；
The gas reservoir（3）Inner wall be equipped with for controlling gas reservoir（3）Internal temperature is 2 DEG C at work
Circulating cooling water pipe；
The electroforming solution memory（4）Magnetic stirring apparatus work when rotating speed be 400~600r/min.
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| CN201710068972.8A Active CN106811773B (en) | 2015-05-12 | 2015-05-12 | Supercritical composite electroforming system recycling device |
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- 2015-05-12 CN CN201710068969.6A patent/CN106801235B/en active Active
- 2015-05-12 CN CN201710068972.8A patent/CN106811773B/en active Active
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Also Published As
| Publication number | Publication date |
|---|---|
| CN106801235B (en) | 2018-06-08 |
| CN104846406A (en) | 2015-08-19 |
| CN106868577A (en) | 2017-06-20 |
| CN106801235A (en) | 2017-06-06 |
| CN104846406B (en) | 2017-03-08 |
| CN106811773A (en) | 2017-06-09 |
| CN106868577B (en) | 2018-06-08 |
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