CN105600793A - Method for preparing silicon oxide nanofiber - Google Patents
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- CN105600793A CN105600793A CN201511008887.XA CN201511008887A CN105600793A CN 105600793 A CN105600793 A CN 105600793A CN 201511008887 A CN201511008887 A CN 201511008887A CN 105600793 A CN105600793 A CN 105600793A
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- C—CHEMISTRY; METALLURGY
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention discloses a method for preparing silicon oxide nanofiber. The method comprises the following steps of mixing silica sol with a nitrate solution, performing ultrasonic dispersion on the solution, adding ethylenediamine after the dissolution of the nitrate solution, and stirring uniformly to obtain a mixed solution; putting the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene liner, standing the reaction kettle in a high-temperature baking oven after the closing of the reaction kettle, and performing a hydrothermal reaction; taking out the reaction kettle and cooling the reaction kettle to room temperature after the completion of the reaction, collecting precipitates in the reaction kettle, and washing the precipitates to obtain a silicon oxide nanofiber crude product; adding the silicon oxide nanofiber crude product into a hydrochloric acid solution, stirring in a thermostatic water bath, removing impurity components from the silicon oxide nanofiber crude product, and performing centrifugal separation to obtain a silicon oxide nanofiber finished product. The method disclosed by the invention has the advantages that not only can the high energy consumption in a nanofiber preparation process through a traditional chemical vapor deposition and thermal evaporation technology be avoided, but also the production is easily expanded by utilization of a hydrothermal synthesis technology.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of bently, have compared with high-flexibility and flame retardancy matterThe preparation method of monox nanometer fiber.
Background technology
In Oil & Gas Storage and oil field development automation and intelligentification process, the exploitation of Fibre Optical Sensor becomes the work of current dynamic monitoringMake focus. But mechanical fiber optic performance is not good. Core is high index of refraction silica glass fiber, and mechanical strength only has 0.2GPa left and right, has frangible feature. Due to transportation problem and fitting operation personnel's artificial careless mistake, most of optical fiber is in peaceThe dress initial stage just cannot normally be used. Thereby limit greatly this technology in oilfield enterprise's large-scale promotion. Ensureing that machinery is strongWhen degree, developing a kind of silicon oxide fibre material with high-flexibility becomes problem in the urgent need to address.
For a long time, scientist is devoted to find always and has ideal machine intensity and flexible tencel material concurrently with meetingThe particular/special requirement in the fields such as work, electronics, military affairs. For this reason, scientific research personnel to multiple natural fiber material (as spider silk, silkDeng) and artificial synthetic fiber material (as high polymer fiber, alloy fiber etc.) carried out the research of a large amount of fracture mechanism.But, passed through the effort of many decades, the fibrous material that research and development can have a high-strength high-tractility be simultaneously still one hugeChallenge. This mainly stems from the essential contradictory relation between material self Young's modulus and mechanical strength properties. Conventionally Young mould,Measure low material and there is stronger plastic deformation ability, but a little less than this also means that binding ability between this material atom, therebyCause the reduction of mechanical strength. After CNT is found, 1-dimention nano fiber is because of its distinctive microstructure and spread out by thisThe high-mechanical property that raw small-size effect show is significantly different from macroscopic fibres material, wide in range Young's modulus modulation scopeAnd the considerable elastic deformation limit (4%-7%), become the popular candidate (S. of high-strength high-tractility fiber of future generationHao etc., Science, 2013,339,1191-1194.). Up to the present, there is multiple high intensity nano fibre to be groundSend, for example: nano silver wire, copper nano-wire, Ge nanoline, sulfide nanometer linear and high molecular polymerization nanofiber etc.
Along with to amorphous solid, especially the exploration of amorphous silica glass material breaking strain mechanism deeply, is more and more groundStudy carefully and recognize that silica molecular structure has stronger local flexibility, particularly Si-O-Si key and O-Si-O key respectively can be certainlyBy rotation～9-12 ° and 5 °. On nanoscale, it is spontaneous that the unordered network structure of this unique long-range can order about defect sitesForm lar nanometric cavities, reduce breaking bonds to keep the relevance between inner atom, energy in reduction system. These lar nanometric cavities justBubble in picture viscous fluid, can dilute atomic density, and induction produces local viscous flow region, effectively improves amorphous silicaThe ductility of material regional area, shows the pliability that is similar to metal alloy. Therefore, when the yardstick of amorphous silica is limitBuilt in Nano grade, will show mechanical effect (G.Brambilla etc., the Nano significantly different from macroscopical silica fragilityLett., 2009,9,831-835). In addition, by being combined with 1-dimention nano fibre structure, can be effectively by defective bit pairThe impact of mechanical strength is limited in very little scope, and then acquisition possesses high mechanical properties simultaneously, and (uniaxial tension intensity can reach 8More than GPa) and the monox nanometer fibrous material of high ductibility (elongation > 100%).
Early stage molecular dynamics simulation tentatively explained this scheme feasibility (Y.C.Chen etc., Phys.Rev.Lett.,2007,99,155506). Directly atomic scale experimental study further confirms to manufacture in nano silicon oxide is received material oxygen sky subsequentlyCave and ion defects can significantly strengthen uniaxial tension ductility (K.Zheng etc., Nat in ensureing higher mechanical strengthComm., 2010,1,1-8). Although there is partial report to show that superhigh intensity silica white nano-wire can pass through top-down processingTechnology and high temperature gas phase method are realized (L.M.Tong etc., NanoLett., 2005,5,259-262). But owing to closingBecome temperature higher, often cause in nano wire product defective bit more, pliability is not good. Up to the present, still lacking canAt the effective ways compared with preparing on a large scale high-flexibility monox nanometer fiber under low energy consumption.
Summary of the invention
Based on above-mentioned technical problem, the invention provides a kind of preparation method of monox nanometer fiber.
The technology used in the present invention solution is:
A preparation method for monox nanometer fiber, comprises the following steps:
A mixes Ludox and ultrasonic dispersion with nitrate solution, after nitrate solution dissolves, add ethylenediamine, stir,Obtain mixed solution;
The mixed solution that b obtains step a is moved in teflon-lined stainless steel cauldron, dries after airtight at high temperatureIn case, leave standstill, carry out hydro-thermal reaction;
After c has reacted, take out reactor and be cooled to room temperature, collecting the sediment obtaining in reactor, then sediment is washedAfter washing, obtain monox nanometer fiber crude product;
The monox nanometer fiber crude product that d obtains step c joins in hydrochloric acid solution, under water bath with thermostatic control, stirs, and removesImpurity composition in monox nanometer fiber crude product, then through centrifugation, obtain monox nanometer fibrous finished product.
In step a: described Ludox is preferably alkaline silica sol, Ludox mass fraction is preferably 30%～40%. Ludox toolBody is preferably bimodal porous silica or SBA-15 molecular sieve.
In step a: described nitrate is preferably ferric nitrate or silver nitrate.
In step a: in described nitrate solution, in nitrate and Ludox, the ratio of the amount of substance of silicon is preferably 1～2.
In step a: in described ethylenediamine and mixed solution, the ratio of the volume of solvent is preferably 1.6～1.7.
In step b: the hydro-thermal reaction time is preferably 3～4 days; Hydrothermal temperature is preferably 170～200 degrees Celsius.
In steps d: described concentration of hydrochloric acid solution is preferably 1～3 mol/L.
In steps d: described bath temperature is preferably 80 degrees Celsius; The water-bath time is preferably 1 hour.
In steps d: described centrifugation rate is preferably 4000～5000 revs/min.
Useful technique effect of the present invention is:
The monox nanometer fiber preparation method convenient and efficient that the present invention proposes, with low cost, by both having adopted Hydrothermal Synthesis technologyCan avoid traditional chemical vapor deposition and thermal evaporation technique to prepare the high energy consumption in nanofiber process, be easy to again expanding production, haveHelp the conversion of product from laboratory preparation to commercial Application.
The productive rate of the monox nanometer fiber product that the present invention produces is higher than 95%, and purity is high, size uniform, and product reappearance is goodGood. The mechanical performance of product is good, can bend and fracture and structural damage do not occur by deep camber, shows good pliability.In addition, also show good anti-flammability, stretch-proof performance by the fibrous film of this monox nanometer, at high thermal-flame pointFire after ten minutes, do not occur curling crackedly, can keep complete pattern. The monox nanometer fiber that the present invention obtains can be wideThe general necks such as flame-retarding fire-extinguishing, high-strength anti-corrosion layer, anti-shearing thickening liquid (liquid bullet resistant material) and Fibre Optical Sensor that are applied toIn territory.
The monox nanometer fiber that adopts preparation method of the present invention to obtain has considerable draw ratio (> 100), bigger serface, withAnd differ from the pliability of macroscopical glass fibre. This structure can form the network structure interweaving in length and breadth, enlarges markedly with external substanceContact-making surface, can play very strong " pinning " effect to the material in surrounding environment. For example, the silica that the present invention produces is receivedRice fiber can produce peculiar anti-shearing thickening phenomenon in the solution such as ethanol, polyethylene glycol, increases fluid viscosity. Can also showWork improves compactness, the mechanical stability of the rear expansion carbon layer of burning, strengthens carbon-coating and makes it not with the adhesion of equipment matrix surfaceEasily come off, thereby effectively stop heat transmission, extend fire endurance. In addition formed by this high-intensity high-tenacity nanofiber,Spatial network skeleton space average-size all below 100nm, airborne oxygen, the freedom of nitrogen equimolecular in its holeMobile quilt greatly weakens, and significantly reduces thermal convection current. Meanwhile, small-bore can cause heat reflection/scattering interface in unit volume to increase,Thermal radiation absorption ability strengthens, and effectively reduces thermal conductivity factor. The effusion of this material to heat transmission, thermal decomposition material and airDiffusion mixes can play effective retarding action.
Brief description of the drawings
Fig. 1 is the SEM photo of the monox nanometer fibrous material prepared of the present invention;
Fig. 2 is monox nanometer fiber product element power spectrum;
Fig. 3 is monox nanometer fiber product XRD spectra;
Fig. 4 is that monox nanometer fiber TEM characterizes; Wherein (a) monox nanometer fiber TEM characterizes; (b, c) nanofiberDeep camber bending form; (d) amorphous state monox nanometer fibre structure; (e) single-crystal silica nanofiber lattice structure;(f) amorphous state and the contrast of single-crystal silica nanofiber diameter.
Detailed description of the invention
For existing nano-fiber material synthesis technique complexity, energy consumption cost is higher, on a large scale preparation and product purity,The not good shortcomings such as easy fracture that cause of productive rate and pliability, the invention provides a kind of easy, low cost, low based on Hydrothermal SynthesisThe preparation method of energy consumption, the difficulty that can be used for large-scale production high-intensity high-tenacity is fired monox nanometer fibrous material. The present invention one sideIt is not good that face has improved existing silica type fiber product flexility, and the mechanical performance of bending easy fracture has solved existing on the other handDeposit 1000 degrees Celsius of monox nanometer fiber preparation method synthesis temperatures higher (>), be difficult for the technological problems of expanding production. BelowBy specific embodiment, the invention will be further described.
Embodiment 1
Take the SiO that 3.75 gram mass marks are 30%2Ludox (alkalescence), adds 37.5 ml distilled waters. Stir and surpassAfter sound is uniformly dispersed, then take 15.14 grams of Fe (NO3)3.9H2O (nine water ferric nitrates) joins in silica aqueous solution, stirsMix and dissolve completely to ferric nitrate for 15 minutes.
Subsequently, above-mentioned solution is slowly dropped in the flask that fills 60 milliliters of ethylenediamine liquid, when dripping process, carry outMagnetic agitation (500 revs/min). Treat that solution dropwises, this emulsion stirred 15 hours, system is fully mixed,Obtain mixed solution.
Above-mentioned mixed solution is moved in the polytetrafluoroethyllining lining stainless steel cauldron of 150 milliliters, Celsius 180 after airtightIn degree baking oven, leave standstill 4 days, carry out hydro-thermal reaction.
After having reacted, take out reactor and be cooled to room temperature. Use respectively sediment in absolute ethyl alcohol and distilled water washing reaction stillEach three times, remove the mixture that obtains bottle green iron containing compounds and silicon nanowires after solvent impurity. And then product is immersed to 200In the hydrochloric acid solution of milliliter 1 mol/L, under 80 degrees Celsius of water-baths, stir 1 hour, remove the iron component in product.
Finally centrifugal above-mentioned mixed acid solution (4000 revs/min of centrifugation rates) isolated to monox nanometer fiber, use distilled waterAfter washing 3 times, pack in the reservoir vessel that is full of inert gas.
Fig. 1 is the SEM photo of monox nanometer fibrous material. SEM (SEM) characterizes and shows a large amount of size uniformsThe loose porous flocculence network structure of fibre structure formation crosslinked together, wherein the diameter dimension of single nanofiber is28.2 ± 8.0 nanometers, length exceedes 2 microns.
Fig. 2 is monox nanometer fiber product element power spectrum. X ray energy dispersive spectrum (EDX) shows that nanofiber forms intoBe divided into silicon and oxygen, the spot scan of element power spectrum shows that silica element is than for 1:1.4～1:2.2, proves that silica prepared by the present invention receivesIn rice fiber, exist the oxygen defect position of some.
Fig. 3 is monox nanometer fiber product XRD spectra. X-ray diffraction (XRD) characterize spectrogram show product crystal structure withKnown oxygen SiClx is consistent, and the broadening of wherein levying diffraction maximum has illustrated that nanofiber product small-size effect is remarkable, has confirmed the present inventionThe chemical composition of the nanofiber of preparation is silica.
Fig. 4 is that monox nanometer fiber TEM characterizes. Transmission electron microscope (TEM) analysis shows monox nanometer fiber surfaceSmooth, and can carry out deep camber bending and not rupture. High power TEM and electronic diffraction spectrum analysis further show instituteObtain monox nanometer fiber and be mainly undefined structure (amorphous), but also doped with a small amount of nanometer monocrystalline fiber. Monocrystalline oxidationIn silicon nanowires, spacing is that the lattice fringe of 0.487 nanometer and 0.739 nanometer corresponds respectively to silica (200) and (020)Plane. In addition, from TEM, also can be observed nanometer monocrystalline fibre diameter (13～24 nanometer) and be conventionally less than amorphous nano fibreDimension diameter (22～36 nanometer).
Embodiment 2
Take 3.75 gram of 30% alkaline SiO2Ludox, adds 37.5 ml distilled waters. After stirring ultrasonic being uniformly dispersed,Take again 6.36 grams of AgNO3(silver nitrate) joins in silica aqueous solution, stirs and dissolves completely to silver nitrate for 20 minutes.
Subsequently, above-mentioned solution is slowly dropped in the flask that fills 60 milliliters of ethylenediamine liquid, when dripping process, carry outMagnetic agitation (500 revs/min). Treat that solution dropwises, this emulsion stirred 12 hours, system is fully mixed,Obtain mixed solution.
Above-mentioned mixed solution is moved in the polytetrafluoroethyllining lining stainless steel cauldron of 150 milliliters, Celsius 170 after airtightIn degree baking oven, leave standstill 4 days.
After having reacted, take out reactor and be cooled to room temperature. Use respectively sediment in absolute ethyl alcohol and distilled water washing reaction stillEach three times, remove the mixture that obtains Ag-containing compound and silicon nanowires after solvent impurity. And then product is immersed to 200 milliliter 1In the hydrochloric acid solution of mol/L, under 80 degrees Celsius of water-baths, stir 1 hour, remove the silver components in product. Finally will mixAcid solution centrifugal (5000 revs/min of centrifugation rates) is isolated monox nanometer fiber, is full of with packing into after distilled water washing 3 timesIn the reservoir vessel of inert gas.
XRD analysis result shows that product is silica.
Typical case SEM, Fig. 1 in TEM result and embodiment 1, Fig. 4 result is similar.
Embodiment 3
Take 15 gram of 30% alkaline SiO2Ludox, adds 150 ml distilled waters. After stirring ultrasonic being uniformly dispersed, then claimGet 30 grams of Fe (NO3)3.9H2O (nine water ferric nitrates) joins in silica aqueous solution, stir 30 minutes complete to silver nitrateDissolve.
Subsequently, above-mentioned solution is slowly dropped in the flask that fills 240 milliliters of ethylenediamine liquid, when dripping process, carry outMagnetic agitation (500 revs/min). Treat that solution dropwises, this emulsion stirred 15 hours, system is fully mixed,Obtain mixed solution.
It is in the 1Cr18Ni9Ti specification HTHP stainless steel cauldron of 1 liter that above-mentioned mixed solution is moved into volume, in still, pressesPower maintains 2MPa, reacts 3 days under 170 degree celsius temperature.
After having reacted, take out reactor and be cooled to room temperature. After sediment suction filtration enrichment in still, use respectively absolute ethyl alcohol andEach three times of sediment in distilled water washing reaction still. And then product is immersed in the hydrochloric acid solution of 200 milliliter of 3 mol/L,Under 80 degrees Celsius of water-baths, stir 1 hour, remove the iron component in product.
Finally centrifugal mixed acid solution in above-mentioned steps (5000 revs/min of centrifugation rates) isolated to monox nanometer fiber, useDistilled water packs in the reservoir vessel that is full of inert gas after washing 3 times.
Typical case XRD, SEM, tem analysis result is similar to embodiment 1, proves that the present invention amplifies rear reappearance in proportion good.
The burning of monox nanometer fiber membrane and bend tension test, specific as follows:
Gained monox nanometer fiber sample in embodiment 1 is dispersed in 50% ethanol water ultrasonic 30 minutes by a, will disperseLiquid by vavuum pump suction filtration to polyvinylidene fluoride micro-filtration membrane (aperture is 0.65 micron, and thickness is 125 microns) surface.
B according to the suction filtration time that need to maintain of required tunica fibrosa thickness within the scope of 30～90 minutes.
After c suction filtration completes, the polyvinylidene fluoride micro-filtration membrane that is coated with nano fibrous membrane is transferred on ptfe substrate, putsEnter under vacuum drying chamber room temperature and be dried 30～50 minutes.
After d is dry, by careful tunica fibrosa taking off from micro-filtration membrane surface, obtain monox nanometer fiber membrane.
Under best test condition gained monox nanometer fiber membrane of the present invention stretch and bending process in can holding structure completeProperty, without obviously losing Fragmentation Phenomena, prove that it has good stretch-proof and bending property, also show that prepared silica receivesRice fibrous material has good mechanical robustness, pliability. In addition, monox nanometer fiber membrane is processed under thermal-flameRoasting ten minutes, there is not combustion phenomena, exterior appearance, without obvious curling behavior, can maintain complete shape and appearance simultaneously, showsThis monox nanometer fiber has good flame retardancy.
Claims (10)
1. a preparation method for monox nanometer fiber, is characterized in that comprising the following steps:
A mixes Ludox and ultrasonic dispersion with nitrate solution, after nitrate solution dissolves, add ethylenediamine, stir,To mixed solution;
The mixed solution that b obtains step a is moved in teflon-lined stainless steel cauldron, airtight after in high temperature ovenLeave standstill, carry out hydro-thermal reaction;
After c has reacted, take out reactor and be cooled to room temperature, collecting the sediment obtaining in reactor, then by after sediment washing,Obtain monox nanometer fiber crude product;
The monox nanometer fiber crude product that d obtains step c joins in hydrochloric acid solution, stirs, except deoxidation under water bath with thermostatic controlImpurity composition in silicon nanofiber crude product, then through centrifugation, obtain monox nanometer fibrous finished product.
2. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in step a: described siliconColloidal sol is alkaline silica sol, and Ludox mass fraction is 30%～40%.
3. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in step a: described siliconColloidal sol is bimodal porous silica or SBA-15 molecular sieve.
4. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in step a: described nitreHydrochlorate is ferric nitrate or silver nitrate.
5. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in step a: described nitreIn acid salt solution, in nitrate and Ludox, the ratio of the amount of substance of silicon is 1～2.
6. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in step a: described secondIn diamines and mixed solution, the ratio of the volume of solvent is 1.6～1.7.
7. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in step b: hydro-thermal is anti-Between seasonable, it is 3～4 days; Hydrothermal temperature is 170～200 degrees Celsius.
8. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in steps d: described saltAcid solutions is 1～3 mol/L.
9. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in steps d: described waterBath temperature is 80 degrees Celsius; The water-bath time is 1 hour.
10. the preparation method of a kind of monox nanometer fiber according to claim 1, is characterized in that, in steps d: described inCentrifugation rate is 4000～5000 revs/min.
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| US10233380B1 (en) * | 2017-09-11 | 2019-03-19 | Saudi Arabian Oil Company | Well treatment fluid having an acidic nanoparticle based dispersion and a polyamine |
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| US10577526B2 (en) | 2017-09-11 | 2020-03-03 | Saudi Arabian Oil Company | Loss circulation material composition having an acidic nanoparticle based dispersion and polyamine |
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| US11279865B2 (en) | 2017-09-11 | 2022-03-22 | Saudi Arabian Oil Company | Well treatment fluid having an acidic nanoparticle based dispersion, an epoxy resin, and a polyamine |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107537493A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | Co-based fischer-tropsch catalyst and its application method |
| CN107537493B (en) * | 2016-06-29 | 2020-12-01 | 中国石油化工股份有限公司 | Cobalt-based Fischer-Tropsch catalyst and application method thereof |
| US10233380B1 (en) * | 2017-09-11 | 2019-03-19 | Saudi Arabian Oil Company | Well treatment fluid having an acidic nanoparticle based dispersion and a polyamine |
| US10316238B2 (en) | 2017-09-11 | 2019-06-11 | Saudi Arabian Oil Company | Nanosilica dispersion for thermally insulating packer fluid |
| US10577526B2 (en) | 2017-09-11 | 2020-03-03 | Saudi Arabian Oil Company | Loss circulation material composition having an acidic nanoparticle based dispersion and polyamine |
| US10683452B2 (en) | 2017-09-11 | 2020-06-16 | Saudi Arabian Oil Company | Nanosilica dispersion for thermally insulating packer fluid |
| US10731069B2 (en) | 2017-09-11 | 2020-08-04 | Saudi Arabian Oil Company | Well treatment fluid having an acidic nanoparticle based dispersion and a polyamine |
| US11034881B2 (en) | 2017-09-11 | 2021-06-15 | Saudi Arabian Oil Company | Nanosilica dispersion for thermally insulating packer fluid |
| US11279865B2 (en) | 2017-09-11 | 2022-03-22 | Saudi Arabian Oil Company | Well treatment fluid having an acidic nanoparticle based dispersion, an epoxy resin, and a polyamine |
| US11370955B2 (en) | 2017-09-11 | 2022-06-28 | Saudi Arabian Oil Company | Nanosilica dispersion for thermally insulating packer fluid |
| CN109881305A (en) * | 2019-04-03 | 2019-06-14 | 中国恩菲工程技术有限公司 | A kind of gas phase spinning process and device continuously preparing silicon nanofiber |
| CN109881305B (en) * | 2019-04-03 | 2023-08-22 | 中国恩菲工程技术有限公司 | Gas phase spinning method and device for continuously preparing silicon nanofiber |
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