CN103072966A - Apparatus for preparing water-soluble fullerene - Google Patents
Apparatus for preparing water-soluble fullerene Download PDFInfo
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- CN103072966A CN103072966A CN2012105507174A CN201210550717A CN103072966A CN 103072966 A CN103072966 A CN 103072966A CN 2012105507174 A CN2012105507174 A CN 2012105507174A CN 201210550717 A CN201210550717 A CN 201210550717A CN 103072966 A CN103072966 A CN 103072966A
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- ball mill
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- agitator
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Abstract
The invention discloses an apparatus for preparing water-soluble fullerene. The apparatus comprises a ball mill used for the strong mixing of fullerene powder and water-soluble molecules to form a mixture, a mixer used for dissolving the mixture in water and stirring to form a solution, a filtering device used for filtering the solution in the mixer, and a filling device for filling the filtered solution, and the ball mill, the mixer, the filtering device and the filling device are sequentially connected through a pipeline. The apparatus has the advantages of simple structure, low cost, strong practicality, production efficiency improvement and product quality improvement.
Description
Technical field
The present invention relates to mechanical field, relate in particular to a kind of equipment for preparing water-soluble fullerene.
Background technology
PEG), the water soluble molecules such as polyvinylpyrrolidone (PVP), cyclodextrin are wrapped to form the stability that water-soluble compound improves soccerballene with fullerene molecule.But also do not prepare preferably the equipment of water-soluble fullerene at present, cause the output of water-soluble fullerene can't reach the market requirement, preparation efficiency is low, and the quality product of preparation is not high yet.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of equipment for preparing water-soluble fullerene, be intended to solve the problem that does not also have in the prior art for the equipment of volume production water-soluble fullerene.
Technical scheme of the present invention is as follows:
A kind of equipment for preparing water-soluble fullerene, wherein, comprise for the ball mill that fullerene powder and water soluble molecules is carried out powerful mixing and form mixture, be used for described mixture is water-soluble and stir the agitator that forms solution, be used for the filtration unit that the solution to agitator filters, the filling apparatus that is used for carrying out filtering rear solution can that described ball mill, agitator, filtration unit and filling apparatus connect successively by pipeline.
The equipment of described preparation water-soluble fullerene wherein, arranges an on off control device in the described ball mill, described on off control device is controlled described ball mill start and stop once: turn round after 1 ~ 30 minute, stop 1 ~ 60 minute; And circulating start and outage totally 360 ~ 1080 minutes.
The equipment of described preparation water-soluble fullerene wherein, arranges a temperature-control device in the described ball mill, the temperature that described temperature-control device is controlled described ball mill remains on 20 ~ 30 ℃.
The equipment of described preparation water-soluble fullerene, wherein, the rotating speed the during running of described ball mill be 400 ~ 600 turn/hour.
The equipment of described preparation water-soluble fullerene, wherein, the controller that described agitator is provided with a lifting support and is connected with described lifting support, after agitator stops to stir, described controller sends to described lifting support and promotes instruction, described lifting support is controlled described agitator and is promoted to predetermined height after receiving and promoting instruction.
The equipment of described preparation water-soluble fullerene wherein, connects a sterilising plant between described filtration unit and the filling apparatus.
The equipment of described preparation water-soluble fullerene, wherein, described filtration unit is nanofiltration device.
The equipment of described preparation water-soluble fullerene, wherein, be provided with the first strainer and the second strainer that connect successively in the described nanofiltration device, the filtering membrane aperture in described the first strainer is 1 ~ 20 μ m, and the filtering membrane aperture of described the second strainer is 0.01 ~ 0.5 μ m.
Beneficial effect: the present invention by be provided for fullerene powder and water soluble molecules carry out powerful mixing form mixture ball mill, be used for described mixture is the water-soluble and agitator that stirs, be used for the filtration unit that the solution to agitator filters, the filling apparatus that is used for carrying out filtering rear solution can, so that the production capacity of water-soluble fullerene is brought up to 5 kilograms/single single working days, and realized the continuity of producing, the present invention is simple in structure, cost is low, practical, not only improve production efficiency, more improved quality product.
Description of drawings
Fig. 1 is the structural representation that the present invention prepares the equipment preferred embodiment of water-soluble fullerene.
Embodiment
The invention provides a kind of equipment for preparing water-soluble fullerene, clearer, clear and definite for making purpose of the present invention, technical scheme and effect, below the present invention is described in more detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
See also Fig. 1, Fig. 1 is the structural representation that the present invention prepares the equipment preferred embodiment of water-soluble fullerene, as shown in the figure, it comprises for the ball mill 100 that fullerene powder and water soluble molecules is carried out powerful mixing and form mixture, is used for described mixture is water-soluble and stirs the agitator 200 that forms solution, be used for the filtration unit 300 that the solution to agitator filters, the filling apparatus 400 that is used for carrying out filtering rear solution can.
Equipment among the present invention is for the preparation of water-soluble fullerene, water-soluble fullerene can be by fullerene powder (comprising C60 or C70) and PVP(polyvinylpyrrolidone) be prepared from, it should be noted that, adoptable soccerballene is except C60, C70 among the present invention, also comprise C76, C84 etc., and their mixture; And polymer also can adopt such as water-soluble chitosan, glucose, starch and derivative thereof, methylol/propyl cellulose, polyoxyethylene glycol etc. except optional PVP.
Described ball mill 100 is fullerene powder and water soluble molecules to be carried out powerful mixing prepare mixture, in the present invention, consider that long-time mechanical milling process can bring destruction to raw material, so preferably adopt the controlled ball mill of intermittent type and/or temperature, on off control device and/or temperature-control device namely are set in ball mill 100, described on off control device can be controlled described ball mill 100 start and stop and once comprise: turn round after 1 ~ 30 minute, stop 1 ~ 60 minute, in preparation process, circulating start and outage is totally 360 ~ 1080 minutes altogether, the reason that arranges like this is that the temperature with ball milling is controlled under the lower level, avoid long-time ball milling to produce high temperature to the structural damage of molecule own, the heat that can leave and in operation process, in ball mill 100 tank bodies, produce in ball mill 100 processes of shutting down.Further, described ball mill 100 start and stop once comprise: turn round after 5 minutes, stop 10 minutes, suitably reduce chopper frequency, make temperature be controlled at lower level, guarantee simultaneously preferably ball milling effect.
Except ball mill 100 is carried out the on off control, can also directly carry out temperature control to ball mill 100, namely adopt temperature-control device that the temperature in the ball mill 100 is controlled, make it remain on lower temperature, avoid that tank body, organism temperature in the ball mill 100 is too high to be impacted heat labile molecule.Preferably the temperature in the ball mill 100 is controlled at 10 ~ 50 ℃ among the present invention, further, is preferably 20 ~ 30 ℃, for example 25 degree make the raw molecule structure not be subject to high temperature and destroy.
In addition, in ball mill 100 operation process, can also reach and guarantee that namely the ball milling effect can reduce again the effect to the destruction of raw material as far as possible by controlling suitable rotating speed, find by practice, rotating speed during ball mill 100 running be preferably 400 ~ 600 turn/hour, for example 500 turn/hour, can reach better ball milling effect, simultaneous temperature can not rise too fast.
Mechanical milling process is to utilize the physical action add so that the fullerene powder in the ball mill is fully mixed with water soluble molecules, so that the less component of accounting example is dispersed between the component that accounts for large percentage, the present invention be exactly make the C60 cluster in mechanical milling process, be broken into less uniform particles to be dispersed in PVP intermolecular, realize the compound of the first step.
The mixture that ball milling is good is transported in the agitator 200 by artificial or transfer passage, in agitator 200, add enough water, make mixture soluble in water, carry out further compound, after stirring to a certain degree, soccerballene fully mixes with water soluble molecules, formed the solution of water-soluble fullerene, after stirring was finished, the solution in the agitator 200 need to be put in the filtration unit, and the present invention can arrange in the bottom of agitator 200 taphole, this taphole connects an end of a drainage tube, the other end of drainage tube connects filtration unit 300, and like this, the solution in the agitator 200 can directly flow into filtration unit 300 by drainage tube.In addition, also can arrange in described taphole and drainage tube junction one and be used for the valve system 220 whether control solution flows out, open valve system 220, the solution that can control in the agitator flow into drainage tube, and it does not flow out 220 controls of valve-off device.
For the solution of better controlling in the agitator 200 can flow into drainage tube by taphole, need to make the liquid level of agitator 200 be higher than filtration unit 300, so can a riser 210 be set at described agitator 200, described riser 210 also connects a controller, after described controller is used for agitator stirring end, send steering order to riser 210, after described riser 210 receives described steering order, promote described agitator 200 to predetermined height, this predetermined height is preferably the bottom that makes agitator 200 a little more than the top of filtration unit 300, and the solution of agitator 200 bottoms also can flow in the filtration unit like this.Among the present invention, the stirring action of agitator 200 can make fails compound C
60PVP realize further compound by the coating function that PVP forms behind the micella.The preferred mechanical stirring devices that adopt of agitator 200 wherein stir more abundant, and easy to control.
Filtration unit 300 among the present invention is preferably nanofiltration device, the aperture of the filtering membrane in the nanofiltration device is to determine according to the size of the impurity particle in the solution, adopt two-step approach to come impurity particle is carried out filtering separation among the present invention, be that the first step adopts wide-aperture membrane filtration to fall the macrobead insolubles, second step adopts the membrane filtration of small-bore to fall some remaining small-particle insolubles and bacteriums, namely in nanofiltration device, be provided with the first strainer and the second strainer that connect successively, wherein, 1 ~ 20 μ m is preferably adopted in the filtering membrane aperture of the first strainer, further, to adopt 10 μ m as good, 0.01 ~ 0.5 μ m is preferably adopted in the filtering membrane aperture of the second strainer, further, to adopt 0.2 ~ 0.3 μ m.Obtained the target product of transparent clarification by above-mentioned two steps filtration.
Side at described filtration unit 300 also is provided with a pressure-reduction outlet 310, is used for reducing the pressure of filtration unit 300 inside, and filtration procedure can be carried out smoothly.
Whether also carry out delivered solution by drainage tube between filtration unit and the filling apparatus, also can one second valve door gear 320 be set at this drainage tube, being used for the solution of controlled filter device flows out.
In addition, after having filtered, also product is carried out sterilising treatment, so between filtration unit 300 and filling apparatus 400, also be connected a sterilising plant, the optional high voltage sterilizing device of sterilising plant, after the sterilising treatment, can enter into filling apparatus 400 and carry out the can processing, be finished product with the product can after the sterilization.
In sum, the present invention by be provided for fullerene powder and water soluble molecules carry out powerful mixing form mixture ball mill, be used for described mixture is the water-soluble and agitator that stirs, be used for the filtration unit that the solution to agitator filters, the filling apparatus that is used for carrying out filtering rear solution can, so that the production capacity of water-soluble fullerene is brought up to 5 kilograms/single single working days, and realized the continuity of producing, the present invention is simple in structure, cost is low, practical, not only improve production efficiency, more improved quality product.
Should be understood that application of the present invention is not limited to above-mentioned giving an example, for those of ordinary skills, can be improved according to the above description or conversion that all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (8)
1. equipment for preparing water-soluble fullerene, it is characterized in that, comprise for the ball mill that fullerene powder and water soluble molecules is carried out powerful mixing and form mixture, be used for described mixture is water-soluble and stir the agitator that forms solution, be used for the filtration unit that the solution to agitator filters, the filling apparatus that is used for carrying out filtering rear solution can that described ball mill, agitator, filtration unit and filling apparatus connect successively by pipeline.
2. the equipment of preparation water-soluble fullerene according to claim 1 is characterized in that, an on off control device is set in the described ball mill, and described on off control device is controlled described ball mill start and stop once: turn round after 1 ~ 30 minute, stop 1 ~ 60 minute; And circulating start and outage totally 360 ~ 1080 minutes.
3. the equipment of preparation water-soluble fullerene according to claim 1 is characterized in that, a temperature-control device is set in the described ball mill, and the temperature that described temperature-control device is controlled described ball mill remains on 20 ~ 30 ℃.
4. the equipment of preparation water-soluble fullerene according to claim 1 is characterized in that, the rotating speed the during running of described ball mill be 400 ~ 600 turn/hour.
5. the equipment of preparation water-soluble fullerene according to claim 1, it is characterized in that, the controller that described agitator is provided with a lifting support and is connected with described lifting support, after agitator stops to stir, described controller sends to described lifting support and promotes instruction, described lifting support is controlled described agitator and is promoted to predetermined height after receiving and promoting instruction.
6. the equipment of preparation water-soluble fullerene according to claim 1 is characterized in that, connects a sterilising plant between described filtration unit and the filling apparatus.
7. the equipment of preparation water-soluble fullerene according to claim 1 is characterized in that, described filtration unit is nanofiltration device.
8. the equipment of preparation water-soluble fullerene according to claim 7, it is characterized in that, be provided with the first strainer and the second strainer that connect successively in the described nanofiltration device, filtering membrane aperture in described the first strainer is 1 ~ 20 μ m, and the filtering membrane aperture of described the second strainer is 0.01 ~ 0.5 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105507174A CN103072966A (en) | 2012-12-18 | 2012-12-18 | Apparatus for preparing water-soluble fullerene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105507174A CN103072966A (en) | 2012-12-18 | 2012-12-18 | Apparatus for preparing water-soluble fullerene |
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| CN103072966A true CN103072966A (en) | 2013-05-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2012105507174A Pending CN103072966A (en) | 2012-12-18 | 2012-12-18 | Apparatus for preparing water-soluble fullerene |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449993A (en) * | 2003-04-22 | 2003-10-22 | 上海大学 | Process for preparing fullerols |
| US20080279756A1 (en) * | 2007-05-08 | 2008-11-13 | Aruna Zhamu | Method of producing exfoliated graphite, flexible graphite, and nano-scaled graphene platelets |
| CN102674312A (en) * | 2012-04-17 | 2012-09-19 | 深圳市通产丽星股份有限公司 | Water soluble fullerene and preparation method thereof |
| CN102675655A (en) * | 2012-06-04 | 2012-09-19 | 郑州大学 | Water-soluble fullerene and preparation and application methods thereof |
-
2012
- 2012-12-18 CN CN2012105507174A patent/CN103072966A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449993A (en) * | 2003-04-22 | 2003-10-22 | 上海大学 | Process for preparing fullerols |
| US20080279756A1 (en) * | 2007-05-08 | 2008-11-13 | Aruna Zhamu | Method of producing exfoliated graphite, flexible graphite, and nano-scaled graphene platelets |
| CN102674312A (en) * | 2012-04-17 | 2012-09-19 | 深圳市通产丽星股份有限公司 | Water soluble fullerene and preparation method thereof |
| CN102675655A (en) * | 2012-06-04 | 2012-09-19 | 郑州大学 | Water-soluble fullerene and preparation and application methods thereof |
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Application publication date: 20130501 |