CN103418159A - New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid - Google Patents
New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid Download PDFInfo
- Publication number
- CN103418159A CN103418159A CN2013101908137A CN201310190813A CN103418159A CN 103418159 A CN103418159 A CN 103418159A CN 2013101908137 A CN2013101908137 A CN 2013101908137A CN 201310190813 A CN201310190813 A CN 201310190813A CN 103418159 A CN103418159 A CN 103418159A
- Authority
- CN
- China
- Prior art keywords
- nano particle
- nano particles
- supercritical fluid
- reactor
- supercritical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000012530 fluid Substances 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 3
- NEOGGGHDLGYATP-UHFFFAOYSA-N 1,6-dimethylimidazo[4,5-b]pyridin-2-amine Chemical compound CC1=CN=C2N=C(N)N(C)C2=C1 NEOGGGHDLGYATP-UHFFFAOYSA-N 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- LLYXJBROWQDVMI-UHFFFAOYSA-N 2-chloro-4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1Cl LLYXJBROWQDVMI-UHFFFAOYSA-N 0.000 claims description 2
- MXOGJBKTZBIWOT-UHFFFAOYSA-N 2-phenoxycarbonylbenzoic acid Chemical compound OC(=O)C1=CC=CC=C1C(=O)OC1=CC=CC=C1 MXOGJBKTZBIWOT-UHFFFAOYSA-N 0.000 claims description 2
- QFOHBWFCKVYLES-UHFFFAOYSA-N Butylparaben Chemical compound CCCCOC(=O)C1=CC=C(O)C=C1 QFOHBWFCKVYLES-UHFFFAOYSA-N 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 238000001046 rapid expansion of supercritical solution Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract 1
- 239000012855 volatile organic compound Substances 0.000 abstract 1
- 238000001000 micrograph Methods 0.000 description 9
- 239000002048 multi walled nanotube Substances 0.000 description 8
- 238000012545 processing Methods 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 230000008021 deposition Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- -1 cost consumption Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
Images
Abstract
The invention provides a treatment method for preventing nano particles from re-agglomerating. The treatment method is characterized in that the RESS technology is adopted, and the suspending liquid containing both the nano particles and dissolved small organic molecules of supercritical fluid is directly sprayed to a container through spray microtubes and collected. Due to the instantaneous release of the supercritical fluid, the small organic molecules moving with the airflow are supersaturated to separate out solid particles, and the solid particles deposit and grow on the scattered nano particles to form a layer of film on each nano particle, so as to prevent the nano particles from re-agglomerating. The treatment method has the advantages that no volatile organic compound is needed, the operation is simple, the structures of the nano particles are not damaged, and industrialization is facilitated. The treatment method has a good effect and a high practical value in preventing nano particles from re-agglomerating.
Description
One, technical field
The invention provides a kind of moment discharged at supercritical fluid makes and separates out solia particle with the organic molecule of air motion because of supersaturation nano particle is wrapped up, thereby reach the processing method of reuniting again that prevents nano particle, belong to the technical field of nano particle.
Two, technical background
Nano particle with properties such as quantum size effect, small-size effect, skin effect and macro quanta tunnel effects, at aspects such as catalysis, optical filtering, light absorption, medicine, magnetizing mediums and new materials, huge scientific value and wide market prospects are arranged, caused worldwide great attention, various countries' researcher has carried out a large amount of research.
And the agglomeration traits again of nano particle is the crucial difficult problem of restriction nano particle application.In order to solve this difficult problem, people make a large amount of research work.As with organic matter washing, add dispersant etc. nano particle carried out to parcel, the absorption of physics, and then reach and stop reuniting again of nano particle.Carry out chemical modification by the surface to nano particle in addition, make the organic strand of nanoparticle surface polarization functional group or grafting, prevent reuniting again of nano particle.And these methods have defect in various degree at aspects such as the integrality of the removing of the consumption of washing agent, cost consumption, dispersant, nano particle, suitability for industrialized production, dissolvent residuals.The fast expanding supercritical fluid technique can improve the dispersion of nano particle effectively, but after rapid expanding, these nano particles are easy to reunite again.
In order to overcome above-mentioned the deficiencies in the prior art, the present invention adopts fast expanding supercritical fluid technique (RESS technology), by directly being sprayed onto in container and collecting through fine jet pipe containing the suspension of the supercritical fluid that is dissolved with organic molecule of nano particle.The abrupt release of supercritical fluid makes with the organic molecule of air motion and separates out solia particle because of supersaturation, in the nanoparticle surface deposition of being broken up, increases.Form thin film, thereby reach, prevent that it from reuniting again.The method do not need to use VOC, simple to operate, do not destroy the structure of nano particle and be easy to industrialization, preventing that nano particle from having very good effect and practical value aspect reuniting again.
Three, summary of the invention
In order to solve the agglomeration traits again of nano particle, the invention provides a kind of making and separate out solia particle with the organic molecule of air motion because of supersaturation nano particle is wrapped up when the abrupt release of supercritical fluid, thereby reach the processing method of reuniting again that prevents nano particle.
Concrete experimental procedure is:
A) taking a certain amount of nano particle and organic molecule puts in 1～500ml reactor.
B) connect reaction unit, check air-tightness, by the gas component in supercritical system, get rid of the air in reactor, then temperature is transferred to 0～600 ℃ of even higher temperature.
C) by being passed in reactor of shooting flow system, be pressurized to 0～30MPa even higher, mix 0～300min even longer.
D) supercritical system mixed is injected in container and collects fast through minute nozzle.
E), after cooling, take out sample.
In above-mentioned test method, nano particle can be carbon black, active carbon, carbon fiber, CNT, Graphene, aluminium oxide, any nano particle or the mix nanoparticles such as titanium dioxide, silica, imvite.
In above-mentioned test method, the system components of supercritical fluid is under carbon dioxide, methyl alcohol, ethanol, methane, ethane, propane or other normal temperature, to be one or more of gas or volatile liquid substance.
In above-mentioned test method, organic molecule is under phthalic acid phenyl ester, butyl p-hydroxybenzoate, DMIP or other normal temperature, to be one or more of material solid and that can be dissolved in supercritical system.
In above-mentioned test method, while in supercritical system, there is no gas component, with nitrogen, argon gas or other inert gas, discharge the air in reactor, and for pressurized operation.
In above-mentioned test method, the internal diameter of minute nozzle is 1～500 μ m.
The electron scanning micrograph that is not wrapped nano particle that the nano particle wrapped up by organic molecule of processing by RESS and RESS process contrasts, we find that fluorescence probe is by the nano particle parcel, and agglomeration does not have wrapped nano particle that obvious improvement has been arranged again.
That the present invention has is simple to operate, do not need to use VOC, do not destroy the structure of nano particle and be easy to industrialized advantage.The present invention is by directly being sprayed onto in container and collecting through fine jet pipe containing the suspension of the supercritical fluid that is dissolved with organic molecule of nano particle.The abrupt release of supercritical fluid makes to separate out solia particle with the organic molecule of air motion because of supersaturation, in the nanoparticle surface deposition of being broken up, increases.Form thin film, thereby reach, prevent that it from reuniting again.This kind of method preventing that nano particle from having very good effect and practical value aspect reuniting again.
Four, accompanying drawing explanation
Fig. 1 contains the electron scanning micrograph of the multi-walled carbon nano-tubes of DMIP while being the RESS processing.
Fig. 2 does not contain the electron scanning micrograph of the multi-walled carbon nano-tubes of DMIP while being the RESS processing.
Fig. 3 contains the electron scanning micrograph of the SWCN of DMIP while being the RESS processing.
Fig. 4 does not contain the electron scanning micrograph of the SWCN of DMIP while being the RESS processing.
Five, the specific embodiment
Below introduce embodiments of the invention.
Embodiment mono-:
Taking a certain amount of multi-walled carbon nano-tubes and DMIP puts in 1～500ml reactor.Connect reaction unit, check air-tightness, use CO
2Get rid of the air in reactor, then temperature is transferred to 0～600 ℃ of even higher temperature.By CO
2Be passed in reactor, be pressurized to 0～30MPa even higher, mix 0～300min even longer.The supercritical system that mixes is injected in container and collects fast through minute nozzle, cooling after, take out sample.
The deployment conditions of two kinds of multi-walled carbon nano-tubes is observed by electron scanning micrograph.Fig. 1, Fig. 2 are respectively that RESS does not contain the electron scanning micrograph that does not contain the multi-walled carbon nano-tubes of DMIP when the multi-walled carbon nano-tubes of DMIP and RESS process while processing.By contrast, we find that DMIP is by the multi-walled carbon nano-tubes parcel, and agglomeration does not have wrapped multi-walled carbon nano-tubes that obvious improvement has been arranged again.
Embodiment bis-:
Taking a certain amount of SWCN and DMIP puts in 1～500ml reactor.Connect reaction unit, check air-tightness, use CO
2Get rid of the air in reactor, then temperature is transferred to 0～600 ℃ of even higher temperature.By CO
2Be passed in reactor, be pressurized to 0～30MPa even higher, mix 0～300min even longer.The supercritical system that mixes is injected in container and collects fast through minute nozzle, cooling after, take out sample.
The deployment conditions of two kinds of SWCNs is observed by electron scanning micrograph.Fig. 1, Fig. 2 are respectively that RESS does not contain the electron scanning micrograph that does not contain the SWCN of DMIP when the SWCN of DMIP and RESS process while processing.By contrast, we find that DMIP is by the SWCN parcel, and agglomeration does not have wrapped SWCN that obvious improvement has been arranged again.
Claims (6)
1. the invention provides a kind of abrupt release at supercritical fluid and make to separate out solia particle with the organic molecule of air motion because of supersaturation nano particle is wrapped up, thereby reach the processing method of reuniting again that prevents nano particle, concrete experimental procedure is:
A) taking a certain amount of nano particle and organic molecule puts in 1～500ml reactor.
B) connect reaction unit, check air-tightness, by the gas component in supercritical system, get rid of the air in reactor, then temperature is transferred to 0～600 ℃ of even higher temperature.
C) by being passed in reactor of shooting flow system, be pressurized to 0～30MPa even higher, mix 0～300min even longer.
D) supercritical system mixed is injected in container and collects fast through minute nozzle.
E), after cooling, take out sample.
2. the described method of claim 1, wherein said nano particle can be carbon black, active carbon, carbon fiber, CNT, Graphene, aluminium oxide, any nano particle or the mix nanoparticles such as titanium dioxide, silica, imvite.
3. the described method of claim 1, the system components of wherein said supercritical fluid is under carbon dioxide, methyl alcohol, ethanol, methane, ethane, propane or other normal temperature, to be one or more of gas or volatile liquid substance.
4. the described method of claim 1, wherein said organic molecule is under phthalic acid phenyl ester, butyl p-hydroxybenzoate, DMIP or other normal temperature, to be one or more of material solid and that can be dissolved in supercritical system.
5. the described method of claim 1, while in wherein said supercritical system, there is no gas component, discharge the air in reactor with nitrogen, argon gas or other inert gas, and for pressurized operation.
6. the described method of claim 1, the internal diameter of wherein said described minute nozzle is 1～500 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101908137A CN103418159A (en) | 2013-05-09 | 2013-05-09 | New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101908137A CN103418159A (en) | 2013-05-09 | 2013-05-09 | New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103418159A true CN103418159A (en) | 2013-12-04 |
Family
ID=49643863
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101908137A Pending CN103418159A (en) | 2013-05-09 | 2013-05-09 | New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103418159A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722219A (en) * | 2014-09-03 | 2015-06-24 | 青岛科技大学 | Carbon nano tube dispersion method |
| CN106430113A (en) * | 2016-10-31 | 2017-02-22 | 重庆市南川区庆岩福利碱厂 | Production process capable of lowering sodium sulfide oxidation degree |
| CN107973292A (en) * | 2016-10-24 | 2018-05-01 | 林逸樵 | A kind of devices and methods therefor for producing graphene |
| CN113831762A (en) * | 2020-11-04 | 2021-12-24 | 东华理工大学 | Preparation method of coated titanium dioxide |
-
2013
- 2013-05-09 CN CN2013101908137A patent/CN103418159A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722219A (en) * | 2014-09-03 | 2015-06-24 | 青岛科技大学 | Carbon nano tube dispersion method |
| CN104722219B (en) * | 2014-09-03 | 2017-11-14 | 青岛科技大学 | A kind of carbon nano tube dispersion method |
| CN107973292A (en) * | 2016-10-24 | 2018-05-01 | 林逸樵 | A kind of devices and methods therefor for producing graphene |
| CN106430113A (en) * | 2016-10-31 | 2017-02-22 | 重庆市南川区庆岩福利碱厂 | Production process capable of lowering sodium sulfide oxidation degree |
| CN106430113B (en) * | 2016-10-31 | 2018-07-13 | 重庆市南川区庆岩福利碱厂 | A kind of manufacture craft reducing oxidizing sodium sulphide degree |
| CN113831762A (en) * | 2020-11-04 | 2021-12-24 | 东华理工大学 | Preparation method of coated titanium dioxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Fan et al. | Control of hole opening in single-wall carbon nanotubes and single-wall carbon nanohorns using oxygen | |
| Du et al. | Organic salt-assisted liquid-phase exfoliation of graphite to produce high-quality graphene | |
| CN105483939B (en) | A kind of preparation method of porous graphene nano fibrous membrane | |
| Chen et al. | Aligned macroporous TiO2/chitosan/reduced graphene oxide (rGO) composites for photocatalytic applications | |
| Chen et al. | Wetting-resistant photothermal nanocomposite membranes for direct solar membrane distillation | |
| Chang et al. | Fabrication of nanostructured hollow TiO2 nanofibers with enhanced photocatalytic activity by coaxial electrospinning | |
| CN103418159A (en) | New method for preventing nano particles from re-agglomerating during rapid expansion of supercritical fluid | |
| CN104072762A (en) | Preparation method of magnetic carbon nanotube with polydopamine-modified surface | |
| Zhang et al. | Magnetic recyclable TiO2/multi-walled carbon nanotube nanocomposite: Synthesis, characterization and enhanced photocatalytic activity | |
| Fortunati et al. | Spin coated cellulose nanocrystal/silver nanoparticle films | |
| Ge et al. | Visible light activation of superhydrophobic BiOBr/Ag loaded copper mesh for degradation and their use in oil/water separation | |
| CN103935982B (en) | The preparation method of graphene nanobelt | |
| Dinesh et al. | Use of amorphous carbon nanotube brushes as templates to fabricate GaN nanotube brushes and related materials | |
| Yang et al. | Polyacrylonitrile@ TiO2 nanofibrous membrane decorated by MOF for efficient filtration and green degradation of PM2. 5 | |
| Jiang et al. | Electrospinning of BCNNTs/PVA/PEDOT composite nanofibers films for research thermoelectric performance | |
| Xie et al. | Growth of high-density parallel arrays of ultralong carbon nanotubes with catalysts pinned by silica nanospheres | |
| Mokhena et al. | Nanomaterials: Types, synthesis and characterization | |
| Dali et al. | Electrospinning preparation and properties of NaGdF4: Eu3+ nanowires | |
| Akbarzadeh et al. | Influence of acid and thermal treatments on properties of carbon nanotubes | |
| Han et al. | Insight into the precursor nanofibers on the flexibility of La2O3-ZrO2 nanofibrous membranes | |
| CN102963878A (en) | Separation method for obtaining plenty of high-purity semiconductor single-walled carbon nanotubes | |
| CN103418330A (en) | Novel method for preventing reclustering of nano particles, and application of novel method in preparing nano particle/polymer-based composite material | |
| JP2016183082A (en) | Production method of carbon film, and carbon film | |
| KR102543599B1 (en) | Carbon film and manufacturing method thereof, and fibrous carbon nanostructure dispersion liquid and manufacturing method thereof | |
| CN102627969A (en) | Multi-walled carbon nanotube / AgBiS2 semiconductor nanoparticle hybrid material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131204 |