CN109226780A - A method of nano Au particle is prepared by template of red jujube polysaccharide - Google Patents
A method of nano Au particle is prepared by template of red jujube polysaccharide Download PDFInfo
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- CN109226780A CN109226780A CN201811086215.4A CN201811086215A CN109226780A CN 109226780 A CN109226780 A CN 109226780A CN 201811086215 A CN201811086215 A CN 201811086215A CN 109226780 A CN109226780 A CN 109226780A
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- particle
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- red jujube
- jujube polysaccharide
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- 239000002245 particle Substances 0.000 title claims abstract description 83
- 150000004676 glycans Chemical class 0.000 title claims abstract description 43
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 43
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 22
- 240000008866 Ziziphus nummularia Species 0.000 title 1
- 241001247821 Ziziphus Species 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 244000061458 Solanum melongena Species 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 230000000877 morphologic effect Effects 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000010931 gold Substances 0.000 description 58
- 239000000243 solution Substances 0.000 description 28
- YXOLAZRVSSWPPT-UHFFFAOYSA-N Morin Chemical compound OC1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 YXOLAZRVSSWPPT-UHFFFAOYSA-N 0.000 description 18
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 18
- 235000007708 morin Nutrition 0.000 description 18
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 17
- 229910052737 gold Inorganic materials 0.000 description 17
- 238000006555 catalytic reaction Methods 0.000 description 15
- 230000005540 biological transmission Effects 0.000 description 8
- 238000002835 absorbance Methods 0.000 description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 5
- 239000007853 buffer solution Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 240000000249 Morus alba Species 0.000 description 2
- 235000008708 Morus alba Nutrition 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- B01J35/393—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to a kind of methods for preparing nano Au particle as template using red jujube polysaccharide.Method includes the following steps: red jujube polysaccharide is dissolved in deionized water by (1), it is made into red jujube polysaccharide solution；(2) red jujube polysaccharide solution and chlorauric acid solution are mixed, puts it into metal bath, be stirred to react, slowly becomes aubergine from light yellow to solution, obtain nano Au particle.The above-mentioned method that nano Au particle is prepared as template using red jujube polysaccharide, use red jujube polysaccharide for template, it is low in cost, pollution-free, preparation condition is mild, easy to operate, reaction process is easily controllable, the morphological rules of obtained nano Au particle, uniform particle sizes, particle dispersion, specific surface area with higher and catalytic efficiency.
Description
Technical field
The present invention relates to nano metal material technical fields, prepare nanometer by template of red jujube polysaccharide more particularly to one kind
The method of gold particle.
Background technique
Noble metal nanometer material has become grinding for catalytic field due to its bigger serface, high surface energy in recent years
Study carefully hot spot.The metals such as gold, palladium, platinum, which are prepared into nanoparticle, can reduce their chemical inertness, improve their catalysis effect
Rate.The unique optics of gold nano-material, electrical properties have become a kind of good catalysis material.Nano Au particle system at present
Preparation Method has chemical gas-phase method, laser method, sol-gel method etc..But these method and processes are more complicated, and in preparation process
Need to be added reducing agent, the nanoparticle of preparation is easy to reunite, and influences its catalytic applications.Therefore, the simple green preparation of exploitation is received
The method of rice gold particle becomes focus concerned by people.The natural polysaccharide template of reducing property can by its own reproducibility,
Prepare morphological rules, more dispersed nano Au particle.
Summary of the invention
Based on this, it is necessary to which for current nano Au particle preparation process, complicated, particle, which is easy to reunite, leads to catalytic activity
Limited problem provides a kind of method for preparing nano Au particle as template using red jujube polysaccharide.
A method of nano Au particle is prepared by template of red jujube polysaccharide, comprising the following steps:
(1) red jujube polysaccharide is dissolved in deionized water, is made into red jujube polysaccharide solution；
(2) red jujube polysaccharide solution and chlorauric acid solution are mixed, puts it into metal bath, be stirred to react, to molten
Liquid slowly becomes aubergine from light yellow, obtains nano Au particle.
The above-mentioned method for preparing nano Au particle as template using red jujube polysaccharide, uses red jujube polysaccharide for template, low in cost,
Pollution-free, preparation condition is mild, easy to operate, reaction process is easily controllable, the morphological rules of obtained nano Au particle, grain
Diameter is uniform, particle disperses, specific surface area with higher and catalytic efficiency.
The concentration of the red jujube polysaccharide solution is 0.1~20mg/mL in one of the embodiments,.
The concentration of the chlorauric acid solution is 0.1~50mM in one of the embodiments,.
The molar ratio of the red jujube polysaccharide solution and chlorauric acid solution is 1:10~500 in one of the embodiments,.
The stirring rate being stirred to react is 200~600rpm in one of the embodiments,.
The reaction temperature being stirred to react is 10 DEG C~80 DEG C in one of the embodiments, and the reaction time is 2~8
Hour.
The partial size of the nano Au particle is 8~10nm in one of the embodiments,.
Detailed description of the invention
Fig. 1 is the TEM figure for the nano Au particle that the embodiment of the present invention 1 obtains；
Fig. 2 is the transmission electron microscope particle diameter distribution histogram for the nano Au particle that the embodiment of the present invention 1 obtains；
Fig. 3 be the embodiment of the present invention 1 obtain nano-scale gold particle muonic catalysis morin λ=403nm absorbance with react
Graph of relation between time；
Fig. 4 is ln (C of the nano-scale gold particle muonic catalysis morin in λ=403nm of the acquisition of the embodiment of the present invention 1t/C0) and it is anti-
Graph of relation between seasonable between (t)；
Fig. 5 is the TEM figure for the nano Au particle that the embodiment of the present invention 2 obtains；
Fig. 6 is the transmission electron microscope particle diameter distribution histogram for the nano Au particle that the embodiment of the present invention 2 obtains；
Fig. 7 is ln (C of the nano-scale gold particle muonic catalysis morin in λ=403nm of the acquisition of the embodiment of the present invention 2t/C0) and it is anti-
Graph of relation between seasonable between (t)；
Fig. 8 is the TEM figure for the nano Au particle that the embodiment of the present invention 3 obtains；
Fig. 9 is the transmission electron microscope particle diameter distribution histogram for the nano Au particle that the embodiment of the present invention 3 obtains；
Figure 10 is ln (C of the nano-scale gold particle muonic catalysis morin in λ=403nm of the acquisition of the embodiment of the present invention 3t/C0) and it is anti-
Graph of relation between seasonable between (t)；
Figure 11 is the TEM figure for the nano Au particle that the embodiment of the present invention 4 obtains；
Figure 12 is the transmission electron microscope particle diameter distribution histogram for the nano Au particle that the embodiment of the present invention 4 obtains；
Figure 13 is ln (C of the nano-scale gold particle muonic catalysis morin in λ=403nm of the acquisition of the embodiment of the present invention 4t/C0) and it is anti-
Graph of relation between seasonable between (t).
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited by the specific embodiments disclosed below.
Embodiment 1
Red jujube polysaccharide is dissolved in deionized water, the red jujube polysaccharide solution of 0.1mg/mL is configured to, is 0.1mg/ by concentration
Metal bath is put into after the chlorauric acid solution that the red jujube polysaccharide solution and concentration of mL the is 0.1mM ratio mixing of 1:10 in molar ratio
In, control stirring rate is 200rpm, and 2h is reacted under conditions of temperature is 10 DEG C, and mixed solution color becomes purple from light yellow
Red, i.e. acquisition nano Au particle.
The catalytic performance of gained nano Au particle is tested using ultraviolet specrophotometer.Take the morin of 150 μ L 0.5mM
Solution in cuvette, be added 1790 μ L pH=9 carbonate buffer solution, 50 μ L concentration manufactured in the present embodiment be 4.0 ×
10-3The nano Au particle of mM, then the hydrogenperoxide steam generator of 10 μ L 0.75M is added into cuvette, it does within every 5 minutes primary ultraviolet
Full wavelength scanner.
Take the morin solution of 100 μ L 0.5mM in cuvette, the carbonate buffer solution of 1860 μ L pH=9 of addition, 25
μ L concentration manufactured in the present embodiment is 4.0 × 10-3The nano Au particle of mM, then the peroxide of 15 μ L 0.5M is added into cuvette
Change hydrogen solution, measures absorbance versus time curve under 403nm with ultraviolet specrophotometer.
Transmission electron microscope is to the morphology characterization of nano Au particle as shown in Figure 1, the particle diameter distribution of nano Au particle is straight
Side's figure is as shown in Fig. 2, the average diameter of nano Au particle is 8.10nm, morphological rules, in spherical.
Nano-scale gold particle muonic catalysis morin is in the absorbance of λ=403nm and relation curve such as Fig. 3 institute between the reaction time
Show, shows that nano Au particle has preferable catalytic action to morin.Ln of the nano-scale gold particle muonic catalysis morin in λ=403nm
(Ct/C0) and the reaction time (t) between relation curve as shown in figure 4, showing nano-scale gold particle muonic catalysis morin λ=403nm's
Reaction is pseudo-first-order reaction.
Embodiment 2
Red jujube polysaccharide is dissolved in deionized water, the red jujube polysaccharide solution of 1mg/mL is configured to, is 1mg/mL's by concentration
It is put into metal bath, controls after the chlorauric acid solution that red jujube polysaccharide solution and concentration the are 5mM ratio mixing of 1:80 in molar ratio
Stirring rate is 350rpm, reacts 4h under conditions of temperature is 30 DEG C, mixed solution color becomes aubergine from light yellow, i.e.,
Obtain nano Au particle.
Take the morin solution of 100 μ L 0.5mM in cuvette, the carbonate buffer solution of 1860 μ L pH=9 of addition, 25
μ L concentration manufactured in the present embodiment is 4.0 × 10-3The nano Au particle of mM, then the peroxide of 15 μ L 0.5M is added into cuvette
Change hydrogen solution, surveys absorbance versus time curve under 403nm with ultraviolet specrophotometer.
Transmission electron microscope is to the morphology characterization of nano Au particle as shown in figure 5, the particle diameter distribution of nano Au particle is straight
Side's figure is as shown in fig. 6, the average diameter of nano Au particle is 8.27nm, morphological rules, in spherical.Nano-scale gold particle muonic catalysis mulberry color
Ln (C of the element in λ=403nmt/C0) and the reaction time (t) between relation curve as shown in fig. 7, showing nano-scale gold particle muonic catalysis
The reaction of morin λ=403nm is pseudo-first-order reaction.
Embodiment 3
Red jujube polysaccharide is dissolved in deionized water, the red jujube polysaccharide solution of 10mg/mL is configured to, is 10mg/mL by concentration
Red jujube polysaccharide solution and concentration be 25mM chlorauric acid solution in molar ratio 1:150 ratio mixing after be put into metal bath,
Control stirring rate is 500rpm, reacts 6h under conditions of temperature is 60 DEG C, mixed solution color becomes purplish red from light yellow
Color, i.e. acquisition nano Au particle.
Take the morin solution of 100 μ L 0.5mM in cuvette, the carbonate buffer solution of 1860 μ L pH=9 of addition, 25
μ L concentration manufactured in the present embodiment is 4.0 × 10-3The nano Au particle of mM, then the peroxide of 15 μ L 0.5M is added into cuvette
Change hydrogen solution, surveys absorbance versus time curve under 403nm with ultraviolet specrophotometer.
Transmission electron microscope is to the morphology characterization of nano Au particle as shown in figure 8, the particle diameter distribution of nano Au particle is straight
Side's figure is as shown in figure 9, the average diameter of nano Au particle is 8.82nm, morphological rules, in spherical.Nano-scale gold particle muonic catalysis mulberry color
Ln (C of the element in λ=403nmt/C0) and the reaction time (t) between relation curve it is as shown in Figure 10, show that nano Au particle is urged
The reaction for changing morin λ=403nm is pseudo-first-order reaction.
Embodiment 4
Red jujube polysaccharide is dissolved in deionized water, the red jujube polysaccharide solution of 20mg/mL is configured to, is 20mg/mL by concentration
Red jujube polysaccharide solution and concentration be 50mM chlorauric acid solution in molar ratio 1:200 ratio mixing after be put into metal bath,
Control stirring rate is 600rpm, reacts 8h under conditions of temperature is 80 DEG C, mixed solution color becomes purplish red from light yellow
Color, i.e. acquisition nano Au particle.
Take the morin solution of 100 μ L 0.5mM in cuvette, the carbonate buffer solution of 1860 μ L pH=9 of addition, 25
μ L concentration manufactured in the present embodiment is 4.0 × 10-3The nano Au particle of mM, then the peroxide of 15 μ L 0.5M is added into cuvette
Change hydrogen solution, surveys absorbance versus time curve under 403nm with ultraviolet specrophotometer.
Transmission electron microscope is the particle diameter distribution of nano Au particle to the morphology characterization of nano Au particle as shown in figure 11
Histogram is as shown in figure 12, and the average diameter of nano Au particle is 9.44nm, morphological rules, in spherical.Nano-scale gold particle muonic catalysis
Ln (C of the morin in λ=403nmt/C0) and the reaction time (t) between relation curve it is as shown in figure 13, show nano-scale gold particle
The reaction of muonic catalysis morin λ=403nm is pseudo-first-order reaction.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (7)
1. a kind of method for preparing nano Au particle as template using red jujube polysaccharide, which comprises the following steps:
(1) red jujube polysaccharide is dissolved in deionized water, is made into red jujube polysaccharide solution；
(2) red jujube polysaccharide solution and chlorauric acid solution are mixed, put it into metal bath, be stirred to react, to solution from
It is light yellow slowly to become aubergine, obtain nano Au particle.
2. the method according to claim 1 for preparing nano Au particle as template using red jujube polysaccharide, which is characterized in that described
The concentration of red jujube polysaccharide solution is 0.1~20mg/mL.
3. the method according to claim 1 for preparing nano Au particle as template using red jujube polysaccharide, which is characterized in that described
The concentration of chlorauric acid solution is 0.1~50mM.
4. the method according to claim 1 for preparing nano Au particle as template using red jujube polysaccharide, which is characterized in that described
The molar ratio of red jujube polysaccharide solution and chlorauric acid solution is 1:10~500.
5. the method according to claim 1 for preparing nano Au particle as template using red jujube polysaccharide, which is characterized in that described
The stirring rate being stirred to react is 200~600rpm.
6. the method according to claim 1 for preparing nano Au particle as template using red jujube polysaccharide, which is characterized in that described
The reaction temperature being stirred to react is 10 DEG C~80 DEG C, and the reaction time is 2~8 hours.
7. the method according to claim 1 for preparing nano Au particle as template using red jujube polysaccharide, which is characterized in that described
The partial size of nano Au particle is 8~10nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109894627A (en) * | 2019-02-19 | 2019-06-18 | 江南大学 | The synthetic method of noble metal nano particles |
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| WO2009044146A1 (en) * | 2007-10-02 | 2009-04-09 | University Of York | Metal nanoparticles |
| CN105057692A (en) * | 2015-08-06 | 2015-11-18 | 东北林业大学 | Green synthesis method of gold nanoparticles |
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2018
- 2018-09-18 CN CN201811086215.4A patent/CN109226780A/en not_active Withdrawn
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|---|---|---|---|---|
| WO2009044146A1 (en) * | 2007-10-02 | 2009-04-09 | University Of York | Metal nanoparticles |
| CN105057692A (en) * | 2015-08-06 | 2015-11-18 | 东北林业大学 | Green synthesis method of gold nanoparticles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109894627A (en) * | 2019-02-19 | 2019-06-18 | 江南大学 | The synthetic method of noble metal nano particles |
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Application publication date: 20190118 |