CN104004388A - Method for low-temperature storage of two-dimension nano-powder dispersion solution - Google Patents
Method for low-temperature storage of two-dimension nano-powder dispersion solution Download PDFInfo
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- CN104004388A CN104004388A CN201410186880.6A CN201410186880A CN104004388A CN 104004388 A CN104004388 A CN 104004388A CN 201410186880 A CN201410186880 A CN 201410186880A CN 104004388 A CN104004388 A CN 104004388A
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Abstract
A provided method for low-temperature storage of a two-dimension nano-powder dispersion solution comprises: firstly adding a two-dimension nano-material into a mixed solution to prepare a dispersion solution with a predetermined concentration, mixing for a period; then performing centrifugation processing on the above dispersion solution, standing for a period, transferring the supernatant into a container; then transferring the prepared two-dimension nano-powder dispersion solution to a low-temperature apparatus for storage, and controlling the storage temperature to be lower than zero DEG C and higher than the freezing point of the dispersion solution; and finally directly transferring the dispersion solution out from the low-temperature apparatus for usage. The provided low-temperature storage method relatively well maintains the sheet layer thickness and the structure of the powder, enables the performances of the two-dimension nano-powder to be not influenced, solves the easily-appeared agglomeration and re-stacking problems of the two-dimension nano-powder dispersion solution at normal temperature, improves the storage effect of the two-dimension nano-powder dispersion solution, and helps to substantially improve the application performance of two-dimension nano-materials.
Description
Technical field:
The invention belongs to technical field of nano material, relate in particular to a kind of method of two-dimensional nano powder dispersion low-temperature storage.
Technical field
Nano material can be divided into zero dimension, a peacekeeping two-dimensional nano material according to space dimensionality.Wherein two-dimensional nano material refers to only the material of unidimensional scale at Nano grade in space three-dimensional yardstick.In numerous nano materials, Two-dimensional Inorganic stratified material is extensively paid attention to, and is on the one hand that structure and the performance of two-dimensional nano material is very unique, and two-dimensional nano lamella has wide application prospect on the other hand.
Two-dimensional nano material mainly comprises Graphene, molybdenumdisulphide, boron nitride, tungsten disulfide, titanium disulfide, curing zirconium, two selenizing niobiums, two antimony selenides, three telluriumization two bismuths etc.Such as Graphene has excellent electric property, high heat conductance, high-ratio surface, good mechanical property, stable chemical property, superpower anticorrosion etc., have broad application prospects at aspects such as nano electron device, sensor, energy storage.The excellent properties such as electrical insulating property that the crystalline structure tool of hexagonal boron nitride is good, thermal conductivity, chemical stability, two-dimensional nano boron nitride has broad application prospects in fields such as ion-exchange, absorption, conduction, separation simultaneously, becomes the focus of domestic and international research.The two-dimentional sulfide such as nano tungsten disulfide and molybdenumdisulphide has special performance in many-sides such as optics, electricity, catalysis and machineries, is widely used in the fields such as solid lubricant, catalyzer, electrode materials, gas storage material, semiconductor material and electronic probe.
Individual layer and few layer two-dimensional nano material have unique performance, but are easy to occur stacking again or reunite because the van der Waals interaction between lamella makes it, make the excellent properties of two-dimensional nano material be difficult to show.Most of two-dimensional nano materials have the characteristic of poor hydrophilic and oleophilic, are therefore difficult to be distributed in water and organic solvent, form stable suspension.This problem causes two-dimensional nano lamella just to occur at short notice serious reunion and the situation such as stacking again, has limited its application in a lot of fields, is therefore the needs of expanding its widespread use by the stable preservation of two-dimensional nano dispersion of materials liquid.
The stability that improves at present two-dimensional nano dispersion of materials liquid can only adopt high boiling solvent by employing, adds tensio-active agent or directly carry out the methods such as surface modification.At present conventional high boiling solvent is as N-Methyl pyrrolidone, dimethyl formamide etc., conventionally has stronger toxicity, cost is high, boiling point is high and needs high temperature drying to remove while using.Add tensio-active agent and be conducive to improve the stability of dispersion liquid, remove link but also bring subsequent applications to increase, easily affect the premium properties of two-dimensional nano material.Meanwhile, solvophilic functional group need to be introduced in surface directly method of modifying on two-dimensional nano material structure, has improved preparation cost on the one hand, on the other hand due to structural damage, has had a strong impact on material property.If the Graphene of the functionalized processing of strong oxidizer is due to the destruction that the introducing of oxygen groups has caused phenyl ring conjugated structure, reduce the good performance of material.
The research of employing subzero treatment two-dimensional nano material at present mainly concentrates on and prepares dry powder field, as the Chinese patent of application number CN201010179339.4 has proposed a kind of method that adopts cryodesiccated method to prepare dry graphene powder, the method need to be positioned over freezing the dispersion liquid of Graphene powder in freeze drier and process, due to solvent distillation, and make solvent and powder obtain good separation.The method can keep Graphene dispersiveness and microscopic appearance preferably, effectively reduces the reunion of Graphene.But the method need to be prepared into dry powder, and invest that high, step is many and efficiency is lower.The Chinese patent of application number CN201310131520.1 has proposed a kind of method that freezing and filtering is prepared graphene powder fast, by by freezing graphene dispersing solution formation ice cube, after thawing, forming cotton-shaped powder suction filtration separates again, what the method had reduced Graphene to a certain extent piles superimposition agglomeration traits again, preserve but need to be prepared into equally dry powder, and dispersion effect is poor compared with freeze-drying method.
By regulating the method for two-dimensional nano dispersion of materials liquid storing temp, realize the control to dispersion liquid viscosity, can obviously reduce like this heap superimposition of two-dimensional nano material and reunite, can not exert an influence to material property, secondly can realize in long-term stably stored simultaneously.Low-temperature storage method has improved the preservation effect of two-dimensional nano powder, can significantly improve the Application Areas of two-dimensional nano material, is conducive to the commercial application of two-dimensional nano material.
Summary of the invention:
In view of this, the object of the present invention is to provide a kind of method of two-dimensional nano powder dispersion low-temperature storage, method technique provided by the invention is simple, easy and simple to handle, with low cost.
For achieving the above object, the present invention has adopted a kind of method of two-dimensional nano powder dispersion low-temperature storage, first the method is transferred to the two-dimensional nano powder dispersion preparing cryogenic unit and is preserved, storing temp need to, lower than zero centigrade and higher than the zero pour of dispersion liquid, directly migrate out cryogenic unit by dispersion liquid when use.
In sum, the method for a kind of two-dimensional nano powder dispersion of the present invention low-temperature storage, the method concrete steps are as follows:
Step 1: two-dimensional nano material piece is added in mixing solutions, be mixed with the dispersion liquid of predetermined concentration, and do combination treatment for some time.
Step 2: above-mentioned dispersion liquid is carried out to centrifugal treating, handle rear standing for some time, then supernatant liquor is moved on in container.
Step 3: the above-mentioned container that dispersion liquid is housed is transferred to common low-temperature storing apparatus, and storing temp need to be lower than zero centigrade and higher than the zero pour of dispersion medium.
Step 4: in the time that needs use, two-dimensional nano powder dispersion is shifted out to direct use.
Wherein, the two-dimensional nano dispersion of materials liquid concentration described in step 1 is not limit, and preferred concentration is 0.05-50mg/ml;
Wherein, the mixing solutions described in step 1 is the mixture of organic solvent and water, and organic solvent is not limit.Preferred organic solvent is the dispersion liquid of a kind of and water in Virahol, acetone, ethanol.
Wherein, the two-dimensional nano dispersion of materials liquid and preparation method thereof described in step 1 is not limit, and can adopt the preparation methods such as ultrasonic cavitation method, spheroidal graphite method, paddling process and jet flow cavitation method etc.Preferred method is that jet flow cavitation legal system is for two-dimensional nano material (note: jet flow cavitation treatment process and method are shown in patent of invention " a kind of jet flow cavitation technique is prepared the device and method of Graphene ", the patent No.: 201110190763.3; " method of the two-dimensional nano boron nitride prepared of a kind of jet flow cavitation technique ", the patent No.: 201110347905.2; " a kind of method of preparing two-dimensional nano molybdenum disulfide by jet cavitation technology ", the patent No.: 201110347902.9).
Wherein, the time of the combination treatment described in step 1 is 10 minutes-100 minutes.
Wherein, the centrifugal acceleration described in step 2 is 25-3000g, and centrifugation time is about 20-200 minute, and described time of repose is 0.5-20 hour.Dispersion liquid can be peeled off incomplete large lamella by centrifugal removal in advance.
Wherein, storing temp need to be lower than zero centigrade and higher than dispersion liquid zero pour described in step 3, makes two-dimensional nano dispersion of materials liquid keep at low temperatures liquid.Preferred storing temp is-10 DEG C to-60 DEG C.
Wherein, the low-temperature storing apparatus described in step 3 is not limit, and preferably tests refrigerator and freezer.
Compared with prior art, the present invention adopts thermoregulator method to realize the control to dispersion medium viscosity, thereby has improved the stability of two-dimensional nano dispersion of materials liquid.Present method is simple, easy and simple to handle and with low cost without the former dispersion medium of change, technique.Experiment shows, adopts the present invention that the graphene dispersing solution of the Virahol of 50% volume ratio and water is placed in-18 DEG C of freezer compartment of refrigerator and is placed 1 month, and Graphene sedimentation ratio is less than 10%.
Brief description of the drawings
Fig. 1 placed in case study on implementation 1 after 2 weeks, the cuvette comparison diagram of solution and initial soln after stored under refrigeration solution and normal temperature storage.
Fig. 2 is FB(flow block) of the present invention.
Embodiment:
See Fig. 1,2, in order to further illustrate the present invention, below in conjunction with embodiment, the preparation method of two-dimensional nano material provided by the invention be have been described in detail.In following examples, raw materials used being from the market buied.
Embodiment 1:
Step 1: Graphite Powder 99 adds in the mixing solutions of 50% volume ratio Virahol and water and is mixed with 1m
gthe dispersion liquid of the concentration of/ml, supersound process 20 hours.
Step 2: above-mentioned dispersion liquid, with centrifugal 45 minutes of 500 revs/min of speed, is then moved on to supernatant liquor in plastic containers.
Step 3: above-mentioned dispersion liquid is transferred to general refrigerator refrigeration chamber, store 2 weeks at-18 DEG C of temperature.
Step 4: in the time that needs use, graphene powder dispersion liquid is shifted out to direct use.
Embodiment 2:
Step 1: hexagonal boron nitride powder is added in the ethanol of 50% volume ratio and the mixing solutions of water and is mixed with 3m
gthe dispersion liquid of/ml concentration.Adopt under jet flow cavitation method 20MPa and process 3h.(note " method of the two-dimensional nano boron nitride prepared of a kind of jet flow cavitation technique ", the patent No.: 201110347905.2; )
Step 2: will peel off rear dispersion liquid with centrifugal 45 minutes of 500 revs/min of speed, and then supernatant liquor be moved on in plastic containers.
Step 3: above-mentioned dispersion liquid is transferred to general refrigerator refrigeration chamber, store 2 months at-18 DEG C of temperature.
Step 4: in the time that needs use, freezing boron nitride powder dispersion liquid is shifted out to direct use.
Embodiment 3:
Step 1: molybdenum disulphide powder is added in the acetone of 70% volume ratio and the mixing solutions of water, be mixed with 5m
gthe dispersion liquid of/ml concentration.Adopt under jet flow cavitation method 20MPa and process 3h.
Step 2: dispersion liquid after treatment, with centrifugal 45 minutes of 500 revs/min of speed, is then moved on to supernatant liquor in plastic containers.
Step 3: centrifugal rear dispersion liquid is transferred in cryogenic refrigerator, stored 1 month at-20 DEG C of temperature.
Step 4: in the time that needs use, molybdenumdisulphide powder dispersion is shifted out to direct use.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise of not departing from the present invention; can make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. a method for two-dimensional nano powder dispersion low-temperature storage, is characterized in that: the method concrete steps are as follows:
Step 1: two-dimensional nano material piece is added in mixing solutions, be mixed with the dispersion liquid of predetermined concentration, and do combination treatment for some time;
Step 2: above-mentioned dispersion liquid is carried out to centrifugal treating, handle rear standing for some time, then supernatant liquor is moved on in container;
Step 3: the above-mentioned container that dispersion liquid is housed is transferred to low-temperature storing apparatus, and storing temp need to be lower than zero centigrade and higher than the zero pour of dispersion medium;
Step 4: in the time that needs use, two-dimensional nano powder dispersion is shifted out to direct use.
2. the method for a kind of two-dimensional nano powder dispersion low-temperature storage according to claim 1, is characterized in that: the two-dimensional nano dispersion of materials liquid concentration described in step 1 is not limit, and preferred concentration is 0.05-50mg/ml.
3. the method for a kind of two-dimensional nano powder dispersion low-temperature storage according to claim 1, is characterized in that: the mixing solutions described in step 1 is the mixture of organic solvent and water, and organic solvent is not limit; Preferred organic solvent is the dispersion liquid of a kind of and water in Virahol, acetone, ethanol.
4. the method for a kind of two-dimensional nano powder dispersion low-temperature storage according to claim 1, it is characterized in that: the two-dimensional nano dispersion of materials liquid and preparation method thereof described in step 1 has ultrasonic cavitation method, spheroidal graphite method, paddling process and jet flow cavitation legal system standby, preferred method is that jet flow cavitation legal system is for two-dimensional nano material.
5. the method for a kind of two-dimensional nano powder dispersion low-temperature storage according to claim 1, is characterized in that: the time of the combination treatment described in step 1 is 10 minutes-100 minutes.
6. the method for a kind of two-dimensional nano powder dispersion low-temperature storage according to claim 1, is characterized in that: the centrifugal acceleration described in step 2 is 25-3000g, and centrifugation time is about 20-200 minute; Described time of repose is 0.5-20 hour, and dispersion liquid is peeled off incomplete large lamella by centrifugal removal in advance.
7. the method for a kind of two-dimensional nano powder dispersion low-temperature storage according to claim 1, it is characterized in that: described in step 3, storing temp need to be lower than zero centigrade and higher than dispersion liquid zero pour, make two-dimensional nano dispersion of materials liquid keep at low temperatures liquid; Preferred storing temp is-10 DEG C to-60 DEG C.
8. the method for a kind of two-dimensional nano powder dispersion low-temperature storage according to claim 1, is characterized in that: the low-temperature storing apparatus described in step 3 is not limit, and preferably tests refrigerator and freezer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271185A (en) * | 2014-06-25 | 2016-01-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional lamellar structure stable dispersion liquid and gel, and preparation method and application thereof |
| CN106277059A (en) * | 2016-08-22 | 2017-01-04 | 齐齐哈尔大学 | A kind of method preparing tungsten disulfide/Graphene heterojunction structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1750811A (en) * | 2001-10-19 | 2006-03-22 | 巴克斯特国际公司 | Stable composition comprising particles in a frozen aqueous matrix |
| CN101965315A (en) * | 2008-03-10 | 2011-02-02 | 塔塔化学有限公司 | Process for the preparation of nano zinc oxide particles |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1750811A (en) * | 2001-10-19 | 2006-03-22 | 巴克斯特国际公司 | Stable composition comprising particles in a frozen aqueous matrix |
| CN101965315A (en) * | 2008-03-10 | 2011-02-02 | 塔塔化学有限公司 | Process for the preparation of nano zinc oxide particles |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271185A (en) * | 2014-06-25 | 2016-01-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional lamellar structure stable dispersion liquid and gel, and preparation method and application thereof |
| CN106277059A (en) * | 2016-08-22 | 2017-01-04 | 齐齐哈尔大学 | A kind of method preparing tungsten disulfide/Graphene heterojunction structure |
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