CN107363269B - A kind of preparation method of the Nano silver solution based on tea powder - Google Patents
A kind of preparation method of the Nano silver solution based on tea powder Download PDFInfo
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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Abstract
The present invention provides a kind of preparation method of Nano silver solution based on tea powder, comprising the following steps: step 1: taking tea powder, in being dissolved in the water under room temperature, obtains tea powder solution；Step 2: taking silver salt, in being dissolved in the water under room temperature, obtain silver salt solution；Step 3: silver salt solution described in step 2 being added in tea powder solution described in step 1, mixed solution is obtained, is mixed at room temperature, obtains nano silver mixed liquor；Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering, ethanol washing and filtering, water dispersion obtain Nano silver solution.The present invention uses tea powder as reducing agent, while tea powder is also used as stabilizer, and for preparation process without adding other such as stabilizer substances, preparation process preparation process is simple and mild, green, safe and non-toxic, guarantees the safety of operator.
Description
Technical field
The present invention relates to technical field of material, and in particular to a kind of preparation side of the Nano silver solution based on tea powder
Method.
Background technique
Nano silver is a kind of new function material, has a variety of properties such as nanometer size effect, precious metal surface effect, extensively
It is general to be applied in the fields such as sensor, biological antibacterial, bionic catalyst.Nano silver possesses good bacteriostasis property, has simultaneously
The performance of bionic enzyme.Currently, the process of synthesizing nano-silver is complicated, and need to be added the substances such as dispersing agent, stabilizer, protective agent,
The reunion for preventing nano silver particles, the Chinese patent if publication No. is CN 103212720A disclose a kind of nano silver dispersion
And preparation method thereof and a kind of preparation method of nano silver antibacterial coating, need to be added the substances such as thickener and dispersing agent, most
The nano silver dispersion complicated component obtained eventually, it is at high cost.
Summary of the invention
The object of the present invention is to provide a kind of preparation process simply, the system of the Nano silver solution based on tea powder of safety and environmental protection
Preparation Method.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of preparation method of the Nano silver solution based on tea powder, comprising the following steps:
Step 1: taking tea powder, in being dissolved in the water under room temperature, obtain tea powder solution；
Step 2: taking silver salt, in being dissolved in the water under room temperature, obtain silver salt solution；
Step 3: silver salt solution described in step 2 being added in tea powder solution described in step 1, mixed solution is obtained, in room temperature
Lower mixing, obtains nano silver mixed liquor；
Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering reuses ethyl alcohol and is repeatedly washed and mistake
Filter, then dispersed with pure water, obtain Nano silver solution.
Further, the tea powder the preparation method comprises the following steps: take tealeaves, be mechanically pulverized, cross 300 meshes, then extract, extract
Solvent is water, and extraction solid-liquid ratio is 1:1~7, and extraction temperature is 40~70 DEG C, and extraction time is 1~6 hour, then will extraction
Liquid is centrifuged to obtain supernatant, and finally supernatant is spray-dried up to tea powder.
Further, the tealeaves is black tea, green tea, Longjing tea, oolong tea, dark green tea, yellow tea, white tea or jasmine tea.
Further, the silver salt is silver nitrate or silver acetate.
Further, the revolving speed of stirring described in step 3 is 40~600 revs/min, and the time of stirring is 20 seconds~150 points
Clock.
Further, the concentration of the tea powder solution is the mg/mL of 0.05 mg/mL~1.5.
Further, the concentration of the silver salt solution is 1moL/L.
Further, the concentration of silver salt is 0.1 mmoL/L~50mmoL/L in the mixed solution.
Further, the nano silver average grain diameter in the Nano silver solution is 1nm~60nm.
The invention has the benefit that
A kind of preparation method of Nano silver solution based on tea powder provided by the invention, using tea powder as reducing agent, together
When tea powder be also used as stabilizer, preparation process is without adding other such as stabilizer substance, and preparation process preparation process is simple and temperature
With green, it is safe and non-toxic, guarantee the safety of operator；Nano silver solution prepared by the present invention have good biocidal property and
Bionic catalysis performance.
Detailed description of the invention
Fig. 1 is a kind of ultravioletvisible absorption light of the preparation method embodiment 1 of the Nano silver solution based on tea powder of the present invention
Spectrogram.
Fig. 2 is a kind of particle size distribution figure of the preparation method embodiment 1 of the Nano silver solution based on tea powder of the present invention.
Fig. 3 is a kind of ultravioletvisible absorption light of the preparation method embodiment 2 of the Nano silver solution based on tea powder of the present invention
Spectrogram.
Fig. 4 is a kind of transmission electron microscope picture of the preparation method embodiment 2 of the Nano silver solution based on tea powder of the present invention.
Fig. 5 is a kind of transmission electron microscope picture of the preparation method embodiment 3 of the Nano silver solution based on tea powder of the present invention.
Fig. 6 is a kind of particle size distribution figure of the preparation method embodiment 4 of the Nano silver solution based on tea powder of the present invention.
Fig. 7 is a kind of transmission electron microscope picture of the preparation method embodiment 5 of the Nano silver solution based on tea powder of the present invention.
Fig. 8 is a kind of Nano silver solution prepared by the preparation method embodiment 6 of the Nano silver solution based on tea powder of the present invention
To the fungistatic effect figure of Escherichia coli.
Fig. 9 is a kind of Nano silver solution prepared by the preparation method embodiment 6 of the Nano silver solution based on tea powder of the present invention
To the fungistatic effect figure of staphylococcus aureus.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and specific embodiments:
Embodiment 1
A kind of preparation method of the Nano silver solution based on tea powder, comprising the following steps:
Step 1: taking white tea tea powder 0.3g, in being dissolved in 1000mL water under room temperature, obtain tea powder solution, tea powder solution
Concentration be 0.3 mg/mL；
Step 2: taking silver nitrate 8.4935g, in being dissolved in 50mL water under room temperature, obtain silver salt solution, silver salt solution
Concentration be 1moL/L；
Step 3: silver salt solution described in 80 μ L steps 2 being added in tea powder solution described in 30mL step 1, must be mixed molten
Liquid, the concentration of silver nitrate is 0.4 mmoL/L in mixed solution, is mixed at room temperature, obtains nano silver mixed liquor；Stirring turns
Speed is 80 revs/min, and mixing time is 80 minutes；
Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering reuses ethyl alcohol and is repeatedly washed and mistake
Filter, then dispersed with pure water, obtain Nano silver solution.
It is scanned using Nano silver solution of the ultraviolet-visible absorption spectroscopy instrument to preparation, the result is shown in Figure 1 exists as the result is shown
There is nano silver characteristic absorption peak at 420 nm；It is tested using Nano silver solution of the particle size analyzer to preparation, as a result sees Fig. 2, tied
Fruit shows that mean particle size is 12nm.
Embodiment 2
A kind of preparation method of the Nano silver solution based on tea powder, comprising the following steps:
Step 1: taking black tea tea powder 0.15g, in being dissolved in 100mL water under room temperature, obtain tea powder solution, tea powder solution
Concentration be 1.5 mg/mL；
Step 2: taking silver nitrate 8.4935g, in being dissolved in 50mL water under room temperature, obtain silver salt solution, silver salt solution
Concentration be 1moL/L；
Step 3: silver salt solution described in 100 μ L steps 2 being added in tea powder solution described in 20mL step 1, must be mixed molten
Liquid, the concentration of silver nitrate is 0.5 mmoL/L in mixed solution, is mixed at room temperature, obtains nano silver mixed liquor；Stirring turns
Speed is 80 revs/min, and mixing time is 10 minutes；
Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering reuses ethyl alcohol and is repeatedly washed and mistake
Filter, then dispersed with pure water, obtain Nano silver solution.
Wherein, the tea powder the preparation method comprises the following steps: take black tea leaf, be mechanically pulverized, cross 300 meshes, then extract, extract
Solvent is water, and extraction solid-liquid ratio is 1:1, and extraction temperature is 40 DEG C, and extraction time is 1 hour, is then centrifuged extract liquor
Supernatant is finally spray-dried up to black tea tea powder by clear liquid.
It is scanned using Nano silver solution of the ultraviolet-visible absorption spectroscopy instrument to preparation, as a result sees Fig. 3, exist as the result is shown
There is nano silver characteristic absorption peak at 420 nm；It is characterized using nano silver of the transmission electron microscope to preparation, as a result sees figure
4, the results showed that grain diameter is 3~14nm.
Embodiment 3
A kind of preparation method of the Nano silver solution based on tea powder, comprising the following steps:
Step 1: taking green tea tea powder 0.1g, in being dissolved in 1000mL water under room temperature, obtain tea powder solution, tea powder solution
Concentration be 0.1 mg/mL；
Step 2: taking silver nitrate 8.4935g, in being dissolved in 50mL water under room temperature, obtain silver salt solution, silver salt solution
Concentration be 1moL/L；
Step 3: silver salt solution described in 50 μ L steps 2 being added in tea powder solution described in 20mL step 1, must be mixed molten
Liquid, the concentration of silver nitrate is 0.25 mmoL/L in mixed solution, is mixed at room temperature, obtains nano silver mixed liquor；Stirring turns
Speed is 60 revs/min, and mixing time is 60 minutes；
Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering reuses ethyl alcohol and is repeatedly washed and mistake
Filter, then dispersed with pure water, obtain Nano silver solution；
The tea powder the preparation method comprises the following steps: take green tea, be mechanically pulverized, cross 300 meshes, then extract, extractant
For water, extraction solid-liquid ratio is 1:3, and extraction temperature is 70 DEG C, and extraction time is 6 hours, and extract liquor is then centrifuged to obtain supernatant,
Finally supernatant is spray-dried up to green tea tea powder；
It is characterized using Nano silver solution of the transmission electron microscope to preparation, as a result sees Fig. 5, the results showed that particle
Diameter is 10~20nm.
Embodiment 4
A kind of preparation method of the Nano silver solution based on tea powder, comprising the following steps:
Step 1: taking oolong tea tea powder 0.2g, in being dissolved in 1000mL water under room temperature, obtain tea powder solution, tea powder is molten
The concentration of liquid is 0.2 mg/mL；
Step 2: taking silver nitrate 8.4935g, in being dissolved in 50mL water under room temperature, obtain silver salt solution, silver salt solution
Concentration be 1moL/L；
Step 3: silver salt solution described in 100 μ L steps 2 being added in tea powder solution described in 20mL step 1, must be mixed molten
Liquid, the concentration of silver nitrate is 0.5 mmoL/L in mixed solution, is mixed at room temperature, obtains nano silver mixed liquor；Stirring turns
Speed is 40 revs/min, and mixing time is 20 minutes；
Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering reuses ethyl alcohol and is repeatedly washed and mistake
Filter, then dispersed with pure water, obtain Nano silver solution.
It is tested using Nano silver solution of the particle size analyzer to preparation, as a result sees Fig. 2, the results showed that mean particle size is
19nm。
Embodiment 5
A kind of preparation method of the Nano silver solution based on tea powder, comprising the following steps:
Step 1: taking green tea tea powder 0.1g, in being dissolved in 1000mL water under room temperature, obtain tea powder solution, tea powder solution
Concentration be 0.1 mg/mL；
Step 2: taking silver nitrate 8.4935g, in being dissolved in 50mL water under room temperature, obtain silver salt solution, silver salt solution
Concentration be 1moL/L；
Step 3: silver salt solution described in 100 μ L steps 2 being added in tea powder solution described in 20mL step 1, must be mixed molten
Liquid, the concentration of silver nitrate is 0.5 mmoL/L in mixed solution, is mixed at room temperature, obtains nano silver mixed liquor；Stirring turns
Speed is 40 revs/min, and mixing time is 60 minutes；
Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering reuses ethyl alcohol and is repeatedly washed and mistake
Filter, then dispersed with pure water, obtain Nano silver solution.
It is characterized using Nano silver solution of the transmission electron microscope to preparation, as a result sees Fig. 7, the results showed that particle
Diameter is 20nm.
Embodiment 6
A kind of preparation method of the Nano silver solution based on tea powder, comprising the following steps:
Step 1: taking green tea tea powder 0.1g, in being dissolved in 1000mL water under room temperature, obtain tea powder solution, tea powder solution
Concentration be 0.1 mg/mL；
Step 2: taking silver nitrate 8.4935g, in being dissolved in 50mL water under room temperature, obtain silver salt solution, silver salt solution
Concentration be 1moL/L；
Step 3: silver salt solution described in 100 μ L steps 2 being added in tea powder solution described in 20mL step 1, must be mixed molten
Liquid, the concentration of silver nitrate is 0.5 mmoL/L in mixed solution, is mixed at room temperature, obtains nano silver mixed liquor；Stirring turns
Speed is 40 revs/min, is sampled when mixing time is 20 minutes, 40 minutes, 60 minutes；
Using the Nano silver solution of scraps of paper inhibition zone method assessment preparation to the fungistatic effect of Escherichia coli, Fig. 8 is as a result seen,
In 0 be blank control group, 1 be stir 20 minutes when Nano silver solution fungistatic effect, 2 for stir 40 minutes when Nano silver solution
Fungistatic effect, 3 be stir 60 minutes when Nano silver solution fungistatic effect.
Using the Nano silver solution of scraps of paper inhibition zone method assessment preparation to the fungistatic effect of staphylococcus aureus, as a result see
Fig. 9, wherein 0 is blank control group, 1 is the fungistatic effect of Nano silver solution when stirring 20 minutes, and 2 be nanometer when stirring 40 minutes
The fungistatic effect of silver-colored solution, 3 be the fungistatic effect of Nano silver solution when stirring 60 minutes.
Embodiment 7
A kind of preparation method of the Nano silver solution based on tea powder, comprising the following steps:
Step 1: taking Longjing tea tea powder 0.5g, in being dissolved in 1000mL water under room temperature, obtain tea powder solution, tea powder is molten
The concentration of liquid is 0.05 mg/mL；
Step 2: taking silver acetate 8.3456g, in being dissolved in 50mL water under room temperature, obtain silver salt solution, silver salt solution
Concentration be 1moL/L；
Step 3: silver salt solution described in 20 μ L steps 2 being added in tea powder solution described in 200mL step 1, must be mixed molten
Liquid, the concentration of silver acetate is 0.1 mmoL/L in mixed solution, is mixed at room temperature, obtains nano silver mixed liquor；Stirring turns
Speed is 200 revs/min, and mixing time is 5 minutes；
Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering reuses ethyl alcohol and is repeatedly washed and mistake
Filter, then dispersed with pure water, obtain Nano silver solution；
Wherein, the tea powder the preparation method comprises the following steps: take Longjing tea tealeaves, be mechanically pulverized, cross 300 meshes, then extract, extract
Taking solvent is water, and extraction solid-liquid ratio is 1:7, and extraction temperature is 55 DEG C, and extraction time is 4 hours, is then centrifuged extract liquor
Supernatant is finally spray-dried up to Longjing tea tea powder by supernatant.
The embodiment of the above, only presently preferred embodiments of the present invention, not limits the scope of the present invention, therefore
All equivalent change or modifications done according to technical solution described in the invention patent range should be included in the present patent application patent model
In enclosing.
Claims (6)
1. a kind of preparation method of the Nano silver solution based on tea powder, which comprises the following steps:
Step 1: taking tea powder, in being dissolved in the water under room temperature, obtain tea powder solution, the concentration of the tea powder solution is 0.05
The mg/mL of mg/mL~1.5；The tea powder the preparation method comprises the following steps: take tealeaves, be mechanically pulverized, cross 300 meshes, then extract, extract
Solvent is water, and extraction solid-liquid ratio is 1:1~7, and extraction temperature is 40~70 DEG C, and extraction time is 1~6 hour, then will extraction
Liquid is centrifuged to obtain supernatant, and finally supernatant is spray-dried up to tea powder；
Step 2: taking silver salt, in being dissolved in the water under room temperature, obtain silver salt solution；The concentration of the silver salt solution is 1moL/
L；
Step 3: silver salt solution described in step 2 being added in tea powder solution described in step 1, mixed solution is obtained, mixes at room temperature
Stirring is closed, nano silver mixed liquor is obtained；
Step 4: by nano silver mixed liquor described in step 3 by being centrifuged, filtering reuses ethyl alcohol and is repeatedly washed and filtered,
Dispersed again with pure water, obtains Nano silver solution.
2. a kind of preparation method of Nano silver solution based on tea powder according to claim 1, which is characterized in that the tea
Leaf is black tea, green tea, dark green tea, yellow tea, white tea or jasmine tea.
3. a kind of preparation method of Nano silver solution based on tea powder according to claim 1, which is characterized in that the silver
Salt is silver nitrate or silver acetate.
4. a kind of preparation method of Nano silver solution based on tea powder according to claim 1, which is characterized in that step 3
The revolving speed of the stirring is 40~600 revs/min, and the time of stirring is 20 seconds~150 minutes.
5. a kind of preparation method of Nano silver solution based on tea powder according to claim 1, which is characterized in that described mixed
The concentration for closing silver salt in solution is 0.1 mmoL/L~50mmoL/L.
6. a kind of preparation method of Nano silver solution based on tea powder according to claim 1, which is characterized in that described to receive
Nano silver average grain diameter in the silver-colored solution of rice is 1nm~60nm.
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| CN110810445B (en) * | 2019-11-19 | 2021-06-01 | 西北民族大学 | Method for biologically synthesizing nano-silver bacteriostatic agent by utilizing Tibetan medicine willow tea extract |
| CN113084182A (en) * | 2021-03-04 | 2021-07-09 | 福建农林大学 | Method for preparing nano-silver by using tea leaching solution as raw material |
Citations (5)
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|---|---|---|---|---|
| US5292359A (en) * | 1993-07-16 | 1994-03-08 | Industrial Technology Research Institute | Process for preparing silver-palladium powders |
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN103302306A (en) * | 2013-06-19 | 2013-09-18 | 东南大学 | Method for reducing and preparing functionalized nano-silver based on polyphenol |
| CN105478792A (en) * | 2015-12-05 | 2016-04-13 | 浙江大学 | Environment-friendly preparing method for modified chitosan-nano-silver sol |
| CN107186223A (en) * | 2017-05-22 | 2017-09-22 | 上海理工大学 | A kind of method that utilization China pink tea leaching liquor prepares silver nano-grain |
-
2017
- 2017-09-23 CN CN201710870395.4A patent/CN107363269B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5292359A (en) * | 1993-07-16 | 1994-03-08 | Industrial Technology Research Institute | Process for preparing silver-palladium powders |
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN103302306A (en) * | 2013-06-19 | 2013-09-18 | 东南大学 | Method for reducing and preparing functionalized nano-silver based on polyphenol |
| CN105478792A (en) * | 2015-12-05 | 2016-04-13 | 浙江大学 | Environment-friendly preparing method for modified chitosan-nano-silver sol |
| CN107186223A (en) * | 2017-05-22 | 2017-09-22 | 上海理工大学 | A kind of method that utilization China pink tea leaching liquor prepares silver nano-grain |
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