CN108584882A - A kind of nano material preparation system and the technique using the system production nano material - Google Patents
A kind of nano material preparation system and the technique using the system production nano material Download PDFInfo
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- CN108584882A CN108584882A CN201810868112.7A CN201810868112A CN108584882A CN 108584882 A CN108584882 A CN 108584882A CN 201810868112 A CN201810868112 A CN 201810868112A CN 108584882 A CN108584882 A CN 108584882A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/20—Methods for preparing sulfides or polysulfides, in general
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0894—Processes carried out in the presence of a plasma
Abstract
The invention discloses a kind of nano material preparation system and the techniques for utilizing the system production nano material.The system includes that liquid precursor is quantified the atomising device of atomization, the plasma reactor for generating nano powder material, by nano-powder collection device that nano powder material is detached with gas phase, the exhaust gas processing device handled to the gas phase detached and intelligence control system.The technique, including following procedure：（1）Precursor solution configures；（2）Plasma exciatiaon；（3）Presoma is atomized；（4）Atomized drop normal direction injects plasma；（5）Collect nano powder material；（6）Gas-liquid separation；（7）Vent gas treatment.The preparation system and technique of the present invention, can be applied to the precursor species of various suitable atomizations, has the characteristics that applied widely；Also, the system can serialization prepare and collect nano material, production efficiency is high, and technological process is simple, process control, high degree of automation.
Description
Technical field
It is the present invention relates to technical field of nanometer material preparation more particularly to a kind of nano material preparation system and using this
The technique of system production nano material.
Background technology
Nano material refers to its material of size less than 100nm at least in one direction, can be divided into zero by its dimension
Dimension nano material, monodimension nanometer material and two-dimension nano materials.Nano material have significant skin effect, small-size effect,
Macroscopic quantum channel effect, Dielectric confinement effect etc., it is apparent with macroscopic material that this series of effects so that nano material is shown
Different specific physical chemical property.These special natures make nano material in the energy, environment, function new material, medical treatment, letter
There is extensive and important application in the fields such as breath technology.However, since its size is small, specific surface area is huge, the system of nano material
It is standby relatively difficult.Currently, can extensive, continuous, batch production nano material method and apparatus system it is less, this annoyings
Numerous nano material experts, seriously restricts the development of nanotechnology.
Different according to the property of nano material itself, synthesis or the method for preparing nano material are very more and considerably complicated.
Traditional preparation method of nano material includes mainly chemical method and Physical, and the use of chemical method is more universal among these, it is again
Liquid chemical precipitation method and gas phase chemical deposition can be divided into（CVD）Deng.Plasma activated chemical vapour deposition (PCVD) is gas phase
Very important branch in chemical deposition, it is using plasma as the heating source or chemistry for preparing nano material presoma
The excitaton source of reaction makes presoma gasification, cracking or reaction, and condenses deposition on base material, especially suitable for nano-sized membrane
Preparation.However, presoma used in plasma chemical vapor deposition is usually gaseous material or can be through plasma
The substance of gasification, this severely limits its use scopes.Moreover, PCVD methods are usually batch production, and it is less efficient, it is uncomfortable
Preparation and collection for powder body material.
Invention content
It is an object of the present invention to for the above-mentioned deficiency of the prior art, a kind of nanometer simple in structure, high income is proposed
Material preparation system and the technique for utilizing the system production nano material.
A kind of nano material preparation system of the present invention includes that liquid precursor is quantified the atomising device of atomization, is generated
The plasma reactor of nano powder material, the nano-powder collection device for detaching nano powder material with gas phase, to point
From the exhaust gas processing device that is handled of gas phase and to regulate and control presoma prepare during nano material each response parameter and
The intelligence control system of procedure parameter.
Preferably, the plasma reactor includes plasma producing apparatus, plasm reaction cavity and condensation part.
Preferably, the plasma producing apparatus is direct-current plasma generator, microwave plasma-generator or
Inductively coupled plasma generator.
Preferably, the plasm reaction cavity includes the cylinder of two coaxial sockets.
Preferably, it is anti-to be injected into a manner of normal direction coaxially arranged plasma by carrier gas by the liquid precursor of atomization for it
It answers in chamber.
Preferably, the atomising device is high-pressure fog or ultrasonic spray apparatus.
Preferably, nano-powder collection device 4 includes gas-liquid separation device 50, receiving flask 41, gas-solid separating device 45, gas
Solid separation device 45 is cyclone separator 40, wet separator or cloth bag collector.
Preferably, the gas-liquid separation device type of cooling is water cooling, air cooling or coolant liquid cooling.
Preferably, the exhaust gas processing device includes the processing pond for being filled with absorbing liquid；The absorbing liquid is acid absorbs
Liquid or alkaline absorption solution.
The technique using above-mentioned system production nano material of the present invention, including following procedure：（1）Precursor solution
Configuration；（2）Plasma exciatiaon；（3）Presoma is atomized；（4）Atomized drop normal direction injects plasma；（5）Powder is collected to receive
Rice material；（6）Gas-liquid separation；（7）Vent gas treatment.
A kind of nano material preparation system provided by the present invention and the technique for utilizing the system production nano material, can answer
For the precursor species of various suitable atomizations, have the characteristics that applied widely；Also, the system can serialization preparation and receipts
Collect various zero dimensions, one-dimensional or two-dimensional inorganic nano material, metal nano material, nano-metal-oxide or sulfide, carbon to receive
Rice material and hybrid nano-material, production efficiency is high, and technological process is simple, process control, high degree of automation, is a kind of novel
Nano powder material technology of preparing and system.
Description of the drawings
Fig. 1 is the nano material preparation system schematic diagram of the present invention；
Fig. 2 is the process flow chart of the present invention.
1- plasma reactors；10- plasma producing apparatus；11- plasma electrical sources；12- plasma guns；
13- plasma gun intake valves；14- plasma working gas；15- cools down medium；16- plasma guns front end；17- etc. from
Daughter；20- presoma atomising devices；21- peristaltic pumps；22- presomas；23- atomizers；24- spray chambers；25- gas-carrier pipeline electricity
Magnet valve；26- carrier gas；27- spray chambers front end；30- plasm reaction cavities；31- plasm reaction cavity outer chambers；32- etc. from
Daughter reaction chamber inner chamber body；321- inlets；34- plasma-assisted gas air inlets；341- plasma-assisted gas；
35- plasma-assisted gas pipeline electromagnetic valves；36- plasm reaction cavity inner chamber body tail ends；The condensation parts 3-；37- coolings are situated between
Matter solenoid valve；38- condenser pipes；39- plasm reaction cavities tail portion；4- nano-powder collection devices；40-cyclone separators；
41- receiving flasks；42-cyclone separator lower ends；43- cyclone separators upper end；The air inlet of 44- cyclone separators；45- gas-solids
Separator；50- gas-liquid separation devices；51- condenser pipes；52- cools down medium solenoid valve；The front end of 53- gas-liquid separation devices；
The bottom of 54- gas-liquid separation devices；The bottom leakage fluid dram of 55- gas-liquid separation devices；The tail portion of 56-gas-liquid separation devices；57-
Liquid-phase collection bottle；60- exhaust gas processing devices；61- air inlet pipe；62- air inlet pipe bottom end；63- exhaust outlets；64- exhaust outlets bottom end；
65- processing ponds；70- intelligence control systems；71,72,73,74,75- thermocouples；81,82,83,84,85,86-connecting flange.
Specific implementation mode
Following is a specific embodiment of the present invention in conjunction with the accompanying drawings, technical scheme of the present invention will be further described,
However, the present invention is not limited to these examples.
As shown in Figure 1, the nano material preparation system of the present invention includes：Include before liquid precursor is quantified atomization
It drives body atomising device 20, the plasma reactor 1 for generating nano powder material, received what nano powder material was detached with gas phase
Rice flour body collection device 4, the exhaust gas processing device 60 handled to the gas phase of separation and prepare nanometer to regulate and control presoma
Each response parameter and the intelligence control system of procedure parameter 70 in materials process.
Plasma reactor 1 may include plasma producing apparatus 10, plasm reaction cavity 30 and condensation part 3.
One plasma producing apparatus 10, the presoma being made of plasma electrical source 11 and plasma gun 12 is atomized
Device 20, one is coaxial horizontally disposed by cylindrical plasma reaction chamber outer chamber 31 and plasm reaction cavity inner chamber body 32
Plasma reaction chamber 30, a cyclone separator 40, a gas-liquid separation device 50, an exhaust gas processing device 60 and an intelligence control
System 70 processed；Plasma electrical source 11 provides 12 electric energy of plasma gun, will be fed into the plasma in plasma gun 12
Working gas 14 excites, and is formed by two circles, coaxially arranged plasm reaction cavity outer chamber 31 and inner chamber body 32
In plasm reaction cavity 30 formed plasma 17, thereafter, presoma 22 be quantitatively sent into through peristaltic pump 21 in atomizer 23 into
Row atomization, the drop after atomization enters formation high concentration presoma atomized drop in spray chamber 24, then passes through mist by carrier gas 26
Change the inlet 321 that room 24 is connected with plasma reaction inner chamber body 32 and presoma atomized drop normal direction is injected into plasma
In 17, it is made to react rapidly, wherein controlling the flow of carrier gas 26 by gas-carrier pipeline solenoid valve 25, the product after reaction exists
Nano powder material is condensed into condensation part 3 etc. in vitro precursor reactant chamber tail portion 39, nano powder material is by plasma work gas
Body 14, plasma-assisted gas 341 and carrier gas 26 are sent to jointly in cyclone separator 40, plasma gun intake valve
The inlet of 13 control plasma working gas 14, nano powder material is collected in receiving flask 41, and gas phase portion enters
In gas-liquid separation device 50, after mounted on the condensation of the condenser pipe 51 of the front end of gas-liquid separation device 50 53, wherein low-boiling
Part be cooled into liquid and collect in liquid-phase collection bottle 57, remaining gas phase portion be then sent in exhaust gas processing device 60 with
Remove pollution toxic gas.Power, the plasma working gas that intelligence control system 70 passes through control plasma electrical source 11
14 switches and flow and acquisition 71 data of thermocouple, regulate and control the diameter and temperature of plasma 17, and by acquiring peristaltic pump 21
Rotary speed data and control gas-carrier pipeline electromagnetic valve switch, setting presoma 22 enter the flow velocity of atomizer 23, it are made quantitatively to be atomized,
And it is controlled into the speed in plasma 17, to reach suitable reaction condition and reaction rate；It was prepared by acquisition
The cooling medium solenoid valve 37 of the data of each key area thermocouple 72,73,74,75 and each cooling medium pipeline of control in journey,
52, intelligence adjusts setting nano powder material condensation zones and gas-liquid separation temperature.
Plasma producing apparatus 10 can be made of plasma electrical source 11 and plasma gun 12.Plasma electrical source
11 can be dc plasma power, microwave plasma power supply or inductive coupling plasma power supply.
Plasma gun front end 16 can be extend into inside plasm reaction cavity inner chamber body 32, and coaxially be arranged,
12 tail end 18 of plasma gun is connected with the pipeline of the air inlet pipeline of plasma working gas 14 and the cooling medium 15 of gun body,
And the air inlet pipeline of plasma working gas 14 is connected with solenoid valve, its beginning and flow velocity size can be controlled, with adjusting etc.
The diameter and temperature of gas ions 17.Cooling medium 15 is used for cooling gun body component in order to avoid being damaged influence service life.
Presoma atomising device 20 can be made of peristaltic pump 21, atomizer 23 and spray chamber 24.Peristaltic pump 21 is by forerunner
Body 22 is quantitatively sent in atomizer 23 and is atomized, and the fine droplet after atomization enters spray chamber 24, spray chamber front end 27 with
The piping connection of carrier gas 26, the other end are connect by flange 81 with inlet 321, and the presoma after atomization is by carrier gas 26 with normal direction
Mode, which is injected into plasma, is reacted.According to the number of inlet 321, presoma atomising device 20 is corresponding mating
Connection.
Plasma reaction chamber 30 may include the cylinder of two coaxial sockets.In the present embodiment, plasma reaction
Chamber 30 is coaxial by two different size of cylindrical plasma reaction chamber outer chambers 31 and plasm reaction cavity inner chamber body 32
It being nested, outer chamber 31 and inner chamber body 32 can be made of heat safe metal alloy, corundum, quartz or refractory brick material,
Preferred outer chamber 31 is built by refractory brick, to improve its insulating efficiency.Position of the inner chamber body 32 close to plasma gun front end 16
It sets and is provided with multiple symmetrical inlets 321 along cavity radial direction, and extend to 31 outside of outer chamber and presoma mist
Makeup sets 20 and is connected.Plasm reaction cavity 30 and plasma gun 12 connect one end and divide between inner chamber body 32 and outer chamber 31
Multiple auxiliary gas air inlets 34 are furnished with, the switch of gas 341 and flow is assisted to be controlled by plasma-assisted gas pipeline electromagnetic valve 35
System plays the role of cooling inner chamber body 32 and its high temperature is avoided to damage, while purging nano powder material, is sent to cyclonic separation
Device 40.Near inlet 321 and 32 tail end of inner chamber body, 36 exit is equipped with thermocouple, to detect plasma reaction temperature
And plasma exit temperature.Condenser pipe 38, the condensed pipe of cooling medium stream are installed in plasma reaction chamber tail portion 39
38 play the role of reducing cavity temperature, and cavity inner temperature detects by thermocouple 73, the purpose of reducing reaction cavity temperature be for
Product condensation is to form nano powder material after promoting reaction, while providing follow-up gas-liquid separation efficiency.
Nano-powder collection device 4 includes gas-liquid separation device 50, receiving flask 41, gas-solid separating device 45, gas solid separation
Device 45 can be cyclone separator 40, wet separator or cloth bag collector.In the present embodiment, gas-solid separating device 45 is
Cyclone separator 40.
The air inlet 44 of cyclone separator 40 is coaxially connected through flange 82 with plasm reaction cavity 30, under cyclone separator
End 42 is connected with the receiving flask 41 of nano powder material by flange 84, and cyclone separator upper end 43 is logical with gas-liquid separation device 50
Cross the connection of flange 83.
The front end 53 of gas-liquid separation device 50 with cyclone separator 40 by flanged joint, and in gas-liquid separation device 50
A thermocouple 74 is arranged in front end 53, and the temperature of gas phase portion in gas-liquid separation device 50 is entered with detection, is installed additional by adjusting
In the cooling medium solenoid valve 52 of the condenser pipe 51 of gas-liquid separation device front end, and pass through gas phase after the detection condensation of thermocouple 75
Temperature controls cooling medium switch, realizes the condensation to low-boiling point material in gas phase, it is detached from gas phase, and is flowed into
In the liquid-phase collection bottle 57 being connected with 54 leakage fluid dram 55 of bottom of gas-liquid separation device 50, leakage fluid dram 55 passes through flange 85 and liquid phase
Receiving flask 57 connects, and realizes the separation of low-boiling point material and gas phase portion.
The air inlet pipe 61 of exhaust gas processing device 60 is connected with the tail portion 56 of gas-liquid separation device 50 by flange 86, air inlet pipe
61 bottom ends 62 are immersed in the tail gas absorption liquid liquid level in processing pond 65 hereinafter, 63 bottom end 64 of exhaust outlet is then located at ullage.Tail
Flash Gas Compression Skid System can connect in a similar manner, absorbing liquid can acid absorbing liquid, alkaline absorption solution or both combination,
Property depending on reaction product gas.
Intelligence control system 70 is equipped with human-computer interaction interface, by acquiring each key area electric thermo-couple temperature parameter, control
Working gas and fluid flow and beginning in each air-liquid pipeline are made, in conjunction with special algorithm, can intelligently adjust plasma electrical source work(
Rate, each gas and fluid flow and beginning realize prepared by the serialization of various nano materials.
As shown in Fig. 2, the technique using above system production nano powder material of the present invention includes precursor solution
Configuration, presoma atomization, atomized drop normal direction injection plasma, collects nano powder material, gas-liquid point at plasma exciatiaon
From and vent gas treatment.Precursor solution has been configured first, then adjusts plasma working gas and auxiliary gas flow amount, open etc.
Gas ions power supply, excitation working gas form stable plasma.Meanwhile precursor solution is quantified into atomization, atomized drop
It being injected into plasma and is reacted by carrier gas normal direction, the product after reaction condenses form nano powder material in the reactor chamber, then
It is sent to together in gas-solid separating device by working gas, auxiliary gas and carrier gas to collect nano powder material, gas phase portion
Divide and then further cooled down in gas-liquid separation device to remove low-boiling point material and solvent, rest part then enters tail gas absorption and fills
It sets to remove pollution toxic gas, innocuous gas discharge or recycling.
It is not directed to place above, is suitable for the prior art.
Although some specific embodiments of the present invention are described in detail by example, the skill of this field
Art personnel it should be understood that above example merely to illustrate, the range being not intended to be limiting of the invention, belonging to the present invention
Those skilled in the art can make various modifications or additions to described specific embodiment or use class
As mode substitute, but without departing from the direction or beyond the scope of the appended claims of the present invention.Ability
Domain it is to be understood by the skilled artisans that it is every according to the technical essence of the invention to made by embodiment of above it is any modification, etc.
With replacement, improvement etc., protection scope of the present invention should be included in.
Claims (10)
1. a kind of nano material preparation system, it is characterised in that：It include the presoma atomization dress that liquid precursor is quantified to atomization
It sets（20）, generate nano powder material plasma reactor（1）, the nano-powder that detaches nano powder material with gas phase
Collection device（4）, exhaust gas processing device that the gas phase of separation is handled（60）Nanometer material is prepared with to regulate and control presoma
The intelligence control system of each response parameter and procedure parameter during material（70）.
2. a kind of nano material preparation system as described in claim 1, it is characterised in that：The plasma reactor（1）
Including plasma producing apparatus（10）, plasm reaction cavity（30）The condensation part and（3）.
3. a kind of nano material preparation system as claimed in claim 2, it is characterised in that：The plasma producing apparatus
（10）It is direct-current plasma generator, microwave plasma-generator or inductively coupled plasma generator.
4. a kind of nano material preparation system as claimed in claim 2, it is characterised in that：The plasm reaction cavity（30）
Include the cylinder of two coaxial sockets.
5. a kind of nano material preparation system as claimed in claim 4, it is characterised in that：The liquid precursor of atomization is by carrier gas
It is injected into coaxially arranged plasm reaction cavity in a manner of normal direction（30）In.
6. a kind of nano material preparation system as described in claim 1, it is characterised in that：The presoma atomising device（20）
For high-pressure fog or ultrasonic spray apparatus.
7. a kind of nano material preparation system as described in claim 1, it is characterised in that：Nano-powder collection device（4）Packet
Include gas-liquid separation device（50）, receiving flask（41）, gas-solid separating device（45）, gas-solid separating device（45）For cyclone separator
（40）, wet separator or cloth bag collector.
8. a kind of nano material preparation system as claimed in claim 7, it is characterised in that：The gas-liquid separation device（50）It is cold
But mode is water cooling, air cooling or coolant liquid cooling.
9. a kind of nano material preparation system as described in claim 1, it is characterised in that：The exhaust gas processing device（60）Packet
Include the processing pond for being filled with absorbing liquid（65）；The absorbing liquid is acid absorbing liquid or alkaline absorption solution.
10. a kind of technique using the system production nano material as described in claim 1~9, it is characterised in that：Including following
Process：（1）Precursor solution configures；（2）Plasma exciatiaon；（3）Presoma is atomized；（4）Atomized drop normal direction injection etc. from
Daughter；（5）Collect nano powder material；（6）Gas-liquid separation；（7）Vent gas treatment.
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| CN201810868112.7A CN108584882A (en) | 2018-08-02 | 2018-08-02 | A kind of nano material preparation system and the technique using the system production nano material |
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| CN108584882A true CN108584882A (en) | 2018-09-28 |
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| CN109012527A (en) * | 2018-10-03 | 2018-12-18 | 张家港衡德新材料科技有限公司 | A kind of equipment producing nano material with liquid or gaseous precursor |
| CN110039062A (en) * | 2019-04-18 | 2019-07-23 | 北京科技大学 | A method of preparing spherical nickel base powder |
| CN113351146A (en) * | 2021-05-14 | 2021-09-07 | 南阳师范学院 | Special rotatory high temperature vulcanizer of rare earth sulfide synthesis |
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Application publication date: 20180928 |
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