CN107311218A - A kind of method of stable dispersion metal oxide nanoparticles in aqueous phase - Google Patents
A kind of method of stable dispersion metal oxide nanoparticles in aqueous phase Download PDFInfo
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- CN107311218A CN107311218A CN201710440091.4A CN201710440091A CN107311218A CN 107311218 A CN107311218 A CN 107311218A CN 201710440091 A CN201710440091 A CN 201710440091A CN 107311218 A CN107311218 A CN 107311218A
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- metal oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention belongs to nano material chemical industry, field of food application, and in particular to a kind of method of stable dispersion metal oxide nanoparticles in aqueous phase.The present invention to form mutually exclusive electric double layer and obvious steric effect between nano material by CNF addition, so that metal oxide nanoparticles can be stably dispersed in water.Mixed liquor is uniformly dispersed eventually through the mode of ball milling and centrifugation.The present invention has preparation method easy to operate, with low cost and green non-pollution, its metal oxide nanoparticles dispersion liquid good dispersion prepared, stability are high, follow-up use and storage for a long time beneficial to dispersion liquid, the service efficiency of metal oxide nanoparticles is improved, and further widens its application field.
Description
Technical field
The invention belongs to nano material chemical industry, field of food application, and in particular in a kind of aqueous phase stable dispersion gold
Belong to the method for oxide nano particles.
Background technology
Nano material due to characteristics such as nanometer size effect, skin effect, quantum size effects, with special mechanics,
Electricity, magnetic, optical property and chemism.Metal oxide nanoparticles are the nano materials that a class has extensive use,
There is wide application value and prospect in fields such as chemical industry, electronics, food, biology, medical science.
As titanium dioxide nanoparticle has a most valuable optical property, very high chemical stability, heat endurance, nothing
Toxicity, Superhydrophilic, non-migratory, are widely used in automotive field, anti-ultraviolet material, weaving, photocatalysis catalyst, sun-proof
Frost, coating, paper industry etc.；Nano zine oxide can be used for ultraviolet light masking material in fields such as weaving, coating, antiseptic, glimmering
Luminescent material, catalysis material etc.；Nanometer tungsten oxide also has in terms of discoloration, sensing, photocatalysis and is widely applied and grinds very much
Study carefully；Vanadium oxide nanoparticle is applied in chemical industry synthesis and desulfurization again as new catalyst；Nano-nickel oxide is same in catalytic field
And electronic applications have great application prospect.
In the final application of metal oxide nanoparticles, application of the good dispersity of particle closer to reality
State, therefore its is well dispersed and stable dispersion liquid has extensive use.But be due to nano particle specific surface area it is larger,
Surface can be high, simultaneously because intermolecular force between particle, nano particle is easily reunited.Therefore good dispersion property is prepared
And stable metal oxide nanoparticles dispersion liquid, it can effectively solve the problem that it easily reunites in application and draws hydraulic performance decline, receive
The problems such as meter Xiao Ying plays insufficient.
When the metal oxide nanoparticles of current chemical industry and field of food are applied, typically using organic solvent, You Jihuo
Inorganic dispersion aids, surfactant carry out surface modification to metal oxide nanoparticles, carry out dispersing metal oxides and receive
Rice grain.But it is difficult to there is cleaning, and cost is high, the deficiency such as, stability irritant to human body is poor.
Nano-cellulose (CNF) and its derivative in recent years, because its draw ratio is high, specific surface area is big, mechanical strength
Height, is once used to strengthen composite as green packing material.In addition with applying in terms of electric thin field
Research report (such as polyaniline, CNT, graphene are the conducting film of matrix).
The content of the invention
There is problem or deficiency for above-mentioned, for the scattered cleaning of solution metal oxide nanoparticles is difficult, cost is high, divide
Dissipate stability difference and to human body it is irritant the problem of, the invention provides stable dispersion metal oxide nano in a kind of aqueous phase
The method of particle.
Concrete technical scheme is as follows：
Step 1：Nano-cellulose is weighed, deionized water is added, stirs and evenly mixs；Centrifuge tube is added to be built on centrifuge,
2~5min is centrifuged under conditions of 1000~3000 turns/min, removes after sediment, configures nano-cellulose mass percent
Content is 0.2%~1% dispersion liquid, standby；
Step 2：Nano-cellulose aqueous dispersions prepared by weighing metal oxide nanoparticles and step 1 are positioned over ball
In grinding jar, wherein ball milling ball complement product occupies 1/4~1/3, CNF of ball milling tank volume and the proportion of metal oxide nanoparticles
≤1:5, CNF whole mixed liquor mass ratio >=0.2wt%, then carry out be milled to it is well mixed；
Step 3：The metal oxide dispersion that step 2 is obtained is added in centrifuge tube, 5000~10000 turns/min from
2~5min of the heart, then removes sediment, obtains well dispersed and stable metal oxide dispersion.
Nano-cellulose source is wood pulp, cotton, sisal hemp or bacterium in above-mentioned steps 1.
A diameter of 4~10nm of nano-cellulose in above-mentioned steps 1, length is 1000~3000nm.
Metal oxide nanoparticles are titanium dioxide, tungstic acid, nickel oxide, vanadium oxide or oxidation in above-mentioned steps 2
Zinc nanoparticles.
The size of metal oxide nanoparticles is 5~100nm in above-mentioned steps 2.
The present invention to form mutually exclusive electric double layer between nano material by CNF addition and obvious steric hindrance is imitated
Should, so that metal oxide nanoparticles can be stably dispersed in water.Nano-cellulose itself carries-COO-Na+Base
Group, when nanofiber dispersion is in water, due to the ionization of carboxyl, makes the repulsive interaction of formation electric double layer between fiber, makes
Obtaining CNF can stably be dispersed in water, and this helps dispersion effect to provide the foundation for CNF's.The surface of CNF fibers has amphiphilic
Property, it can form hydrophobic interaction with hydrophobic material, so CNF can be together with dewatering nano material be adsorbed onto.By
There is larger draw ratio in CNF, and be made up of in microstructure the crystalline region and amorphous area of cellulose, cause to exist on fiber and permitted
The weakness of many mechanics so that easily common tangle occurs fiber itself for bending and other nano materials.Eventually through ball milling and centrifugation
Mode mixed liquor is uniformly dispersed.
The present invention is due to using nanofiber usually dispersing metal oxides nano particle, and its dispersion effect is well and stably
Property it is high, technological operation is simple, and easy scale, environmental protection is nontoxic, has in the application aspect of chemical industry and food great
Value and significance.
In summary, the present invention has preparation method easy to operate, with low cost and green non-pollution, its metal prepared
Oxide nano particles dispersion liquid good dispersion, stability are high, follow-up use and storage for a long time beneficial to dispersion liquid, improve
The service efficiency of metal oxide nanoparticles, and further widen its application field.
Brief description of the drawings
Fig. 1 be non-bonus point powder, addition SDS and embodiment ball milling after gained nanoparticulate dispersion place in kind after 6h
State vs scheme；
Fig. 2 is the state vs' figure in kind of gained nanoparticulate dispersion before and after the centrifugation of embodiment；
The SEM figures of film are made for gained nanoparticulate dispersion lifting before and after the centrifugation of embodiment by Fig. 3.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
Step 1：A diameter of 4~10nm is weighed, length is 1000~3000nm nano-cellulose 0.3g, deionized water
50g, is put into the beaker that capacity is 100ml.Magnetic stir bar is added, closing beaker mouthful is positioned on magnetic stirrer and started
Stirring.Stir speed (S.S.) 800 turns/min, time 10min.It is subsequently placed on centrifuge, is centrifuged under conditions of 3000 turns/min
2min, then removes sediment, configures the dispersion liquid that nanofiber cellulose content is 0.3wt%, standby；
Step 2：Weigh particle diameter 5~100nm titania nanoparticles 1g, and 50ml the Nanowire for preparing of step 1
The plain aqueous dispersions of dimension, are added in ball grinder.With vibration at high speed ball mill ball milling 10 minutes；
Step 3：Step 2 gained titania nanoparticles dispersion liquid is added in centrifuge tube, in 8000 turns/min conditions
Lower centrifugation 3min, obtains well dispersed and stable titania nanoparticles aqueous dispersions.
Step 4：By substrate ionized water and absolute alcohol successively ultrasound 15min, it is repeated 2 times, drying for standby.Then will lining
Bottom is fixed on pulling machine, and is soaked with 3000um/s speed in the titania nanoparticles dispersion liquid before and after centrifugation
Stain is lifted, and is repeated 1 times, natural air drying after film forming.It is positioned in Muffle furnace and is calcined with the sample after will air-drying.It is specific to burn
Tied and be referred to as：500 DEG C are raised to from room temperature in 30min, Temperature fall after 30min is kept, obtains titania nanoparticles film.
Fig. 3 shows the SEM figures of the obtained film of gained nanoparticulate dispersion lifting before and after centrifugation.
The titanium dioxide metal oxide nanoparticles dispersion phase that the present embodiment is prepared is compared to be not added with dispersant
And the dispersion liquid that SDS dispersants are obtained is added, dispersiveness and stability are more preferably (as shown in Figure 1)；And be compared to without
The scattered metal oxide nanoparticles of the nano-cellulose of centrifugal treating have more excellent dispersed and stability (Fig. 2 and figure
3).As fully visible, the side of use nano-cellulose stable dispersion metal oxide nanoparticles in aqueous phase of the present invention
Method can obtain good dispersion and metal oxide nanoparticles aqueous dispersion liquid of the long-time stable without sedimentation.
Claims (5)
1. the method for stable dispersion metal oxide nanoparticles, is comprised the following steps that in a kind of aqueous phase：
Step 1：Nano-cellulose CNF is weighed, ionized water is added, stirs and evenly mixs；Add centrifuge tube to be placed on centrifuge, 1000
2~5min is centrifuged under conditions of~3000 turns/min, is removed after sediment, configuring nano-cellulose mass percentage content is
0.2%~1% dispersion liquid, it is standby；
Step 2：Nano-cellulose aqueous dispersions prepared by weighing metal oxide nanoparticles and step 1 are positioned over ball grinder
In, wherein ball milling ball complement product occupies 1/4~1/3, CNF of ball milling tank volume and proportion≤1 of metal oxide nanoparticles:
5, CNF whole mixed liquor mass ratio >=0.2wt%, then carry out be milled to it is well mixed；
Step 3：The metal oxide dispersion that step 2 is obtained is added in centrifuge tube, 5000~10000 turns/min centrifugations 2
~5min, then removes sediment, obtains well dispersed and stable metal oxide dispersion.
2. the method for stable dispersion metal oxide nanoparticles in aqueous phase as claimed in claim 1, it is characterised in that：The step
Nano-cellulose source is wood pulp, cotton, sisal hemp or bacterium in rapid 1.
3. the method for stable dispersion metal oxide nanoparticles in aqueous phase as claimed in claim 1, it is characterised in that：The step
A diameter of 4~10nm of nano-cellulose in rapid 1, length is 1000~3000nm.
4. the method for stable dispersion metal oxide nanoparticles in aqueous phase as claimed in claim 1, it is characterised in that：The step
Metal oxide nanoparticles are titanium dioxide, tungstic acid, nickel oxide, vanadium oxide or Zinc oxide nanoparticle in rapid 2.
5. the method for stable dispersion metal oxide nanoparticles in aqueous phase as claimed in claim 1, it is characterised in that：The step
The size of metal oxide nanoparticles is 5~100nm in rapid 2.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710440091.4A CN107311218A (en) | 2017-06-12 | 2017-06-12 | A kind of method of stable dispersion metal oxide nanoparticles in aqueous phase |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710440091.4A CN107311218A (en) | 2017-06-12 | 2017-06-12 | A kind of method of stable dispersion metal oxide nanoparticles in aqueous phase |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1863498A (en) * | 2003-09-18 | 2006-11-15 | Fmc有限公司 | Method for dispersing metal oxides |
| CN101613600A (en) * | 2008-06-25 | 2009-12-30 | 法国原子能委员会 | The dispersion of luminescent rare earth oxide particles and the method for marking substrates |
| CN103890054A (en) * | 2011-10-26 | 2014-06-25 | 斯托拉恩索公司 | Process for producing a dispersion comprising nanoparticles and a dispersion produced according to the process |
-
2017
- 2017-06-12 CN CN201710440091.4A patent/CN107311218A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1863498A (en) * | 2003-09-18 | 2006-11-15 | Fmc有限公司 | Method for dispersing metal oxides |
| CN101613600A (en) * | 2008-06-25 | 2009-12-30 | 法国原子能委员会 | The dispersion of luminescent rare earth oxide particles and the method for marking substrates |
| CN103890054A (en) * | 2011-10-26 | 2014-06-25 | 斯托拉恩索公司 | Process for producing a dispersion comprising nanoparticles and a dispersion produced according to the process |
Non-Patent Citations (1)
| Title |
|---|
| 刘荣厚等: "《生物质生物转换技术》", 31 December 2015, 上海交通大学出版社 * |
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