CN104588644B - The method of the nano carbon particle of microwave irradiation synthesis load Au - Google Patents
The method of the nano carbon particle of microwave irradiation synthesis load Au Download PDFInfo
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- CN104588644B CN104588644B CN201510027111.6A CN201510027111A CN104588644B CN 104588644 B CN104588644 B CN 104588644B CN 201510027111 A CN201510027111 A CN 201510027111A CN 104588644 B CN104588644 B CN 104588644B
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Abstract
The invention discloses the method for the nano carbon particle of a kind of microwave irradiation synthesis load Au, comprise the following steps: get graphite and put into H is housed
5pW
10v
2o
40there-necked flask in, put up reflux, and stir, then reflux 24h under 140 DEG C of fluidized states; There-necked flask is cooled to normal temperature, phegma is imported in bag filter, then this bag filter is permeated in deionized water; After infiltration by the solution adjust ph in bag filter to 6.5; Above-mentioned solution is loaded centrifuge tube to carry out centrifugal, gets supernatant liquor 5ml afterwards, is diluted to 50ml by deionized water; Put into diluting the solution obtained the bottle that outer wall has cooling water, and often change the cooling water of outer wall, to keep room temperature, simultaneously by microwave, complete reduction process, by the HAuCl of 0.5ml, 0.1M before microwave
43H
2o solution joins in above-mentioned solution; Obtain suspension after reaction terminates, suspension is dried, obtains the nano carbon particle of solid particle load Au.More economic, the convenient and environmental protection of the present invention.
Description
Technical field
The present invention relates to the preparation method of nano-sized carbon, refer to the preparation method of the nano carbon particle of a kind of load Au especially.
Background technology
Different nano-carbon materials has different functions, and as Nano graphite carbon granule has powerful adsorption capacity, easy and histocyte adsorbs.This type nano granular has good cell compatibility, enhancement effect, has very large potential value in cytology field.As brand-new material, nano-carbon material also plays an important role in military project national defence; The surface-functionalized nano carbon particle with gold or platinum coating can be used as photo-reduction agent catalysis CO
2be converted into hydrocarbon; Fluorescence nano carbon granule not only has good biocompatibility and is easy to the advantage such as surface-functionalized, also has can realize conversion fluorescence and launch and the characteristic of stable luminescence, so have important using value at biomedicine field.Nano-carbon material is varied, has different features and application separately.
At present, the preparation method of nano carbon particle can be divided into two classes: method and from bottom to top method from top to bottom.Namely method peels off the physical method preparing nano carbon particle from larger carbon structure from top to bottom, mainly comprises: arc discharge method, laser ablation method, electrochemical process, acid return cooking method.Namely method is prepared the chemical method of nano carbon particle by molecular precursor from bottom to top, mainly comprises: support synthetic method, organic carbon method.There is certain deficiency in these synthetic methods, the pattern of nano carbon particle, output and difficult quality reach accurate control separately, can not reach large-scale simple synthesis.Also discussion is lacked for its growth mechanism, particularly because the restriction of synthetic method makes it still be in the starting stage in the research of application aspect.
Summary of the invention
In view of this, the object of the invention is to the method for the nano carbon particle proposing a kind of microwave irradiation synthesis load Au, more economic, the convenient and environmental protection when preparing the nano carbon particle of load Au.
Based on the method for the nano carbon particle of above-mentioned purpose a kind of microwave irradiation synthesis load Au provided by the invention, comprise the following steps:
(1) get graphite to put into H is housed
5pW
10v
2o
40there-necked flask in, put up reflux, and at room temperature stir 24h, then reflux 24h under 140 DEG C of fluidized states;
(2) described there-necked flask is cooled to normal temperature, phegma is imported in 500 type bag filters, more described bag filter is permeated in deionized water;
(3) after infiltration, by the solution adjust ph in described bag filter to 6.5;
(4) described solution being loaded centrifuge tube carries out centrifugal;
(5) centrifugal complete after, get supernatant liquor 5ml, be diluted to 50ml by deionized water;
(6) step (5) is diluted the solution obtained and put into the bottle that outer wall has cooling water, and often change the cooling water of outer wall, to keep room temperature, simultaneously by micro-wave oven 500W microwave, complete reduction process;
(7) radiation is front by the HAuCl of 0.5ml, 0.1M
43H
2o solution, joins in above-mentioned solution;
(8) reaction obtains suspension after terminating, and is dried by described suspension, obtains the nano carbon particle of solid particle load Au.
Preferably, described step has got 1g graphite in (1), and the H of 5M, 150ml is housed in described there-necked flask
5pW
10v
2o
40.
Preferably, the time of penetration in described step (2) is 3 days, and per half a day need change water once.
Preferably, the NaOH of 0.25M is used to regulate pH in described step (3).
Preferably, in described step (4) with the centrifugation 1h of 1500r/min.
Preferably, the microwave irradiation time in described step (6) is 360 minutes.
Preferably, the bake out temperature in described step (8) is 40 DEG C, and drying time is 3 days.
As can be seen from above, the method for the nano carbon particle of microwave irradiation synthesis load Au provided by the invention, beneficial effect is:
The advantages such as the present invention has can continuous seepage, low in the pollution of the environment, more economic, the convenient and environmental protection when preparing the nano carbon particle of load Au.
Accompanying drawing explanation
Fig. 1 is that the nano carbon particle sample UV of embodiment of the present invention load Au schemes;
Fig. 2 is the nano carbon particle sample particle diameter resolution chart of embodiment of the present invention load Au;
Fig. 3 is the SEM figure of embodiment of the present invention raw graphite;
Fig. 4 is that the nano carbon particle sample TEM of embodiment of the present invention load Au schemes.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
Arbitrary feature disclosed in this description, unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object.That is, unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.
A method for the nano carbon particle of microwave irradiation synthesis load Au, preparation method is as follows: get 1g graphite, put into and 5M, 150mlH are housed
5pW
10v
2o
40there-necked flask in, put up reflux.Stirred at ambient temperature 24h, then under 140 DEG C of fluidized states, backflow 24h.Treat that there-necked flask is cooled to normal temperature, imported by phegma in the bag filter of 500 models, this bag filter permeates 3 days in deionized water, and period per half a day changes water once.After infiltration, by the NaOH adjust ph of the solution 0.25M in bag filter to 6.5.Above-mentioned solution is loaded centrifuge tube, centrifugal 1 hour of 1500r/min.Centrifugal complete after, get supernatant liquor 5ml, be diluted to 50ml by deionized water.Above-mentioned solution is put into the bottle that outer wall has cooling water, and often changes the cooling water of outer wall, to keep room temperature, simultaneously by micro-wave oven 500W microwave 360min, complete reduction process, by the HAuCl of 0.5ml, 0.1M before radiation
43H
2o solution, joins in above-mentioned solution.Obtain suspension after reaction terminates, dried 3 days at 40 DEG C by suspension, the solid particle obtained after oven dry is the nano carbon particle of load Au.
Solid particle samples obtained above is carried out the analysis (see Fig. 1) of ultraviolet sign by ultraviolet-uisible spectrophotometer (UV) (T6 Beijing Pu Xi all purpose instrument Co., Ltd), wavelength is 210-800nm.
As shown in Figure 1, there is the characteristic peak of obvious Au at 537nm place.In figure, curve a is the nano carbon particle curve before load Au, from this curve, is carbon particle curve; Curve f is HAuCl
43H
2o original solution UV schemes; Curve b is that load Au60minUV schemes, curve c is that 180minUV schemes, curve d is that 240minUV schemes, curve e is 360minUV figure.Known load time 60min just has Au to separate out.Further demonstrate that product is exactly the nano carbon particle of load Au.
Solid particle samples obtained above is undertaken analyzing (see Fig. 2) by nano-particle size analysis instrument (NANOPHOXParticleSizeAnalysis), test specification: 1-10000nm, concentration range: ppm-70vol.%, light source: He-Ne Lasers, wavelength 632.8nm, laser power: 10mw, temperature: 15-40 DEG C, humidity 20-70% frozen-free.
As shown in Figure 2, the nano carbon particle particle diameter of load Au is about 1.2nm, can obtain thus, has successfully prepared the nano carbon particle of load Au.
As shown in Figure 3 and Figure 4, Fig. 4 is the TEM figure testing the solid particle obtained, Au particulate load on carbon particles as seen from Figure 4, Fig. 3 is the SEM figure of raw graphite, graphite presents sheet, and dense distribution granular nanometer carbon granule in figure, compared with Fig. 3, can know that the lamellar structure of graphite is destroyed, nano level carbon granule is prepared.
The present invention is not limited to aforesaid detailed description of the invention.The present invention expands to any new feature of disclosing in this manual or any combination newly, and the step of the arbitrary new method disclosed or process or any combination newly.
Claims (7)
1. a method for the nano carbon particle of microwave irradiation synthesis load Au, is characterized in that, comprises the following steps:
(1) get graphite to put into H is housed
5pW
10v
2o
40there-necked flask in, put up reflux, and at room temperature stir 24h, then reflux 24h under 140 DEG C of fluidized states;
(2) described there-necked flask is cooled to normal temperature, phegma is imported in 500 type bag filters, more described bag filter is permeated in deionized water;
(3) after infiltration, by the solution adjust ph in described bag filter to 6.5;
(4) described solution being loaded centrifuge tube carries out centrifugal;
(5) centrifugal complete after, get supernatant liquor 5ml, be diluted to 50ml by deionized water;
(6) step (5) is diluted the solution obtained and put into the bottle that outer wall has cooling water, and often change the cooling water of outer wall, to keep room temperature, simultaneously by micro-wave oven 500W microwave, complete reduction process;
(7) radiation is front by the HAuCl of 0.5ml, 0.1M
43H
2o solution, joins in above-mentioned solution;
(8) reaction obtains suspension after terminating, and is dried by described suspension, obtains the nano carbon particle of solid particle load Au.
2. the method for the nano carbon particle of microwave irradiation synthesis load Au according to claim 1, is characterized in that, described step has got 1g graphite in (1), and the H of 5M, 150ml is housed in described there-necked flask
5pW
10v
2o
40.
3. the method for the nano carbon particle of microwave irradiation synthesis load Au according to claim 1, is characterized in that, the time of penetration in described step (2) is 3 days.
4. the method for the nano carbon particle of microwave irradiation synthesis load Au according to claim 1, is characterized in that, uses the NaOH of 0.25M to regulate pH in described step (3).
5. the method for the nano carbon particle of microwave irradiation synthesis load Au according to claim 1, is characterized in that, with the centrifugation 1h of 1500r/min in described step (4).
6. the method for the nano carbon particle of microwave irradiation synthesis load Au according to claim 1, is characterized in that, the microwave irradiation time in described step (6) is 360 minutes.
7. the method for the nano carbon particle of microwave irradiation synthesis load Au according to claim 1, is characterized in that, the bake out temperature in described step (8) is 40 DEG C, and drying time is 3 days.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1235873A (en) * | 1998-05-19 | 1999-11-24 | 中国石油化工总公司 | Silicon dioxide carried heteropoly acid catalyst, its preparation and use |
| CN1424149A (en) * | 2002-12-27 | 2003-06-18 | 浙江大学 | Method for coating mono-metal particles on carbon nano tube surface |
| CN103586480A (en) * | 2012-08-14 | 2014-02-19 | 南京大学 | One-step microwave preparation method for bimetal/carbon layered composite sphere |
| CN103977841A (en) * | 2014-06-04 | 2014-08-13 | 黑龙江大学 | Method for preparing nitride/carbon nano tube-graphene ternary complex |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101349265B1 (en) * | 2012-05-02 | 2014-01-22 | 성균관대학교산학협력단 | Nanoparticle having core/shell structure, and preparing method of the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1235873A (en) * | 1998-05-19 | 1999-11-24 | 中国石油化工总公司 | Silicon dioxide carried heteropoly acid catalyst, its preparation and use |
| CN1424149A (en) * | 2002-12-27 | 2003-06-18 | 浙江大学 | Method for coating mono-metal particles on carbon nano tube surface |
| CN103586480A (en) * | 2012-08-14 | 2014-02-19 | 南京大学 | One-step microwave preparation method for bimetal/carbon layered composite sphere |
| CN103977841A (en) * | 2014-06-04 | 2014-08-13 | 黑龙江大学 | Method for preparing nitride/carbon nano tube-graphene ternary complex |
Non-Patent Citations (2)
| Title |
|---|
| Microwave-radiated synthesis of gold nanoparticles/carbon nanotubes composites and its application to voltammetric detection of trace mercury(II);He Xu et al;《Electrochemistry Communications》;20081231(第10期);第1839–1843页 * |
| 贵金属及其合金/碳纳米管复合材料的制备与表征;甘自保;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20120215(第2期);第16-43页 * |
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Inventor after: Li Xia Inventor before: Jin Chongjun Inventor before: Wang Shan Inventor before: Wang Keyuan Inventor before: Mao Xianjun Inventor before: Ye Chener Inventor before: Li Ting |
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Effective date of registration: 20171129 Address after: 537200 Guigang City, Guiping City People's government compound in the Guangxi Zhuang Autonomous Region Patentee after: GUIPING PRODUCTIVITY PROMOTION CENTER Address before: 1656, room 1558, 315000 Jiangnan Road, hi tech Zone, Zhejiang, Ningbo Patentee before: Ningbo Ka Er new material Science and Technology Ltd. |