CN106735308A - A kind of preparation method of food-grade small particle nano silver colloidal sol - Google Patents

A kind of preparation method of food-grade small particle nano silver colloidal sol Download PDF

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Publication number
CN106735308A
CN106735308A CN201611245866.4A CN201611245866A CN106735308A CN 106735308 A CN106735308 A CN 106735308A CN 201611245866 A CN201611245866 A CN 201611245866A CN 106735308 A CN106735308 A CN 106735308A
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China
Prior art keywords
silver
colloidal sol
small particle
nano silver
food
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CN201611245866.4A
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Chinese (zh)
Inventor
陈敬锋
李勇
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Suzhou Micro Silver Nano New Material Co Ltd
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Suzhou Micro Silver Nano New Material Co Ltd
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Priority to CN201611245866.4A priority Critical patent/CN106735308A/en
Publication of CN106735308A publication Critical patent/CN106735308A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/30Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of preparation method of food-grade small particle nano silver colloidal sol, concrete technical scheme is as follows:Step one, silver nitrate and water are mixed by the requirement that silver content in solution is 20 10000pm, surfactant is added in silver nitrate solution, stirred 10 30 minutes after mixed solution is obtained, nano material is small due to particle diameter, soft-agglomerated and extremely difficult redisperse is easily formed because attracting each other in colloidal sol, selection adds surfactant for overcoming the deficiency in this step;Step 2, the mixed solution that step one is obtained carries out slaking reaction, specifically, the small particle nano silver colloidal sol that average grain diameter is 2 nanometers is can obtain after being irradiated 30 minutes to 24 hours with light with violet rays source.

Description

A kind of preparation method of food-grade small particle nano silver colloidal sol
Technical field
The invention belongs to nano metal colloidal sol technical field, more particularly to a kind of food-grade small particle nano silver colloidal sol Prepare.
Background technology
It is an important means for improving human health and environmental sanitation to suppress or kill harmful bacteria using antiseptic. The development of antiseptic and its product has turned into one of new focus of current scientific research field.Usually used antiseptic includes day Right antiseptic, organic antibacterial agent and inorganic antiseptic.Natural antibacterial agent kind is limited, and utilization rate is low;Organic antibacterial agent is except presence , also there is poor heat resistance, easily decompose and service life in toxic and side effect;And inorganic antiseptic have broad-spectrum antibacterial property, , all there is great advantage at security, persistence and the aspect such as environment-friendly and generally paid close attention to by people in high-fire resistance.
Metal ion is killed, the active descending order of suppression bacterium is:Hg、Ag、Cu、Cd、Cr、Ni、Pd、Co、 Zn、Fe.And the toxicity such as Hg, Cd, Pb and Cr therein is larger, act essentially as metal bactericide metal only have Ag, Cu and Zn.Wherein silver-colored sterilizing ability is most strong, and its sterilizing ability is thousands of times of zinc, thus current most study is silver-containing antibacterial Agent.Antibacterial Mechanism about silver is commonly considered as Action of Metal Ions and photocatalysis.The chemical constitution of silver determines silver-colored tool There is catalytic capability higher, the reduction potential of high oxidation state silver is high, it is sufficient to surrounding space is produced elemental oxygen, elemental oxygen is with strong Oxidisability can sterilize;Silver ion can be with sulfydryl of the strong adsorption on the protease in bacterial body(- SH)And it is anti-with sulfydryl Should, make the albumen enzymic coagulation loss of activity of bacterium, cause bacterial death;After bacterium is killed by silver ion, silver ion is again by thin Separate out is contacted with other bacteriums again in bacterium corpse, is proceeded as described above again and again.This is also that silver has persistently sterilization The reason for ability.
The particle size for reducing silver reaches nanoscale-Nano Silver, can give full play to its skin effect, greatly improves The photocatalysis performance of silver and the dissolution rate of silver ion, so that its antibacterial activity is greatly improved, with extremely excellent Sterilizing antagonistic property.According to Science Digest in 1978, a kind of antibiotic can about kill 6 kinds of pathogen, and Nano Silver can kill 650 various bacterias, and not produce drug resistance.As can be seen here, nano-silver colloid antibiosis and sterilization agent is researched and developed One barrier of green can be set up for protection human health, with significant economic benefit and social benefit.
The general particle diameter of nano-silver colloid prepared by conventional method is larger, and dispersiveness is poor, so bactericidal property is poor;More attach most importance to Want be due to use silver compound be raw material, general technique be difficult to elimination nano-silver colloid in harmful anion, make Its application in fields such as human body, paper, fibers is extremely limited.
The content of the invention
The present invention proposes a kind of preparation side of food-grade small particle nano silver colloidal sol to solve deficiency of the prior art Method, concrete technical scheme is as follows:Step one, by silver nitrate and water by silver content in solution for the requirement of 20-10000pm is mixed Close, surfactant added in silver nitrate solution, stirred 10-30 minutes after mixed solution is obtained, nano material is due to particle diameter It is small, soft-agglomerated and extremely difficult redisperse is easily formed because attracting each other in colloidal sol, selection adds surface to live in this step Property agent be used for overcome the deficiency.
Step 2, the mixed solution that step one is obtained carries out slaking reaction, and concrete mode is to use light with violet rays source Irradiation can obtain the small particle nano silver colloidal sol that particle diameter is 1-5 nanometers after 30 minutes to 24 hours.
Add after being mixed silver nitrate and water for the requirement of 20-10000pm by silver content in solution in the step one Enter diisooctyl succinate sodium sulfonate(AOT), the harmful anion in solution is displaced, the presence of harmful anion can increase to be received The toxic and side effect of rice silver sol, the harmful anion for eliminating or mitigating in colloidal sol is mainly putting by reaction intermediate intermediate ion Change, cemented out the harmful anion in reaction intermediate using harmless anion, realize the nontoxic pair of nano silver colloidal sol Action characteristic, is directly purified using the electrostatic repulsion between AOT suction-operateds and steric hindrance and like charges.
Surfactant in described step one is sodium stearyl sulfate or odium stearate.
The average grain diameter of silver is at 2 nanometers in the obtained nano silver colloidal sol.
The nano silver colloidal sol that a kind of preparation method of food-grade small particle nano silver colloidal sol is prepared, through it is aseptic in proportion Nanometer silver antimicrobial spray is can be made into after dilution.
Advantageous Effects of the invention:This product uses distinctive technique, using the surfactant of food-grade as adding Plus agent, prepare the ultra-thin water nano silver sol without harmful anion, average grain diameter only 2nm or so.Collosol stability Good, nontoxic, tasteless, sterilizing ability is strong, Mlc≤2PPm, can preserve for a long time without producing precipitation.Product has international first Enter, domestically leading level, have broad application prospects.Project Product production process realizes zero-emission, pollution-free;Product composition Containing only Nano Silver, water and small amount of food surfactant;Product has nontoxic, tasteless, polymolecularity and broad-spectrum antiseptic special Property, sterilizing rate reaches more than 99% within 24 hours, and the nano-silver colloid prepared with technical scheme has stabilization Polymolecularity energy, without precipitation within the shelf-life of 2 years.
Brief description of the drawings
Fig. 1 is the TEM figures of the nano silver colloidal sol that the present invention is prepared.
Fig. 2 is the grain size distribution of the nano silver colloidal sol that the present invention is prepared.
Fig. 3 is the nano silver colloidal sol antibacterial experiment result figure that the present invention is prepared.
Specific embodiment
Embodiment 1
First, silver nitrate and water are mixed by the requirement that silver content in solution is 20pm, ten is added in silver nitrate solution SOS or odium stearate, are stirred 10 minutes after mixed solution is obtained, and then, the mixed solution that will be obtained is cured Reaction, specifically, after being irradiated 30 minutes with light with violet rays source can obtain the small particle Nano Silver that particle diameter is 2 nanometers molten Glue.
Embodiment 2
First, silver nitrate and water are mixed by the requirement that silver content in solution is 100pm, ten is added in silver nitrate solution SOS or odium stearate, then toward adding diisooctyl succinate sodium sulfonate in solution(AOT), in displacing solution Harmful anion, stirs 15 minutes after mixed solution is obtained, and then, the mixed solution that will be obtained carries out slaking reaction, specifically, The small particle nano silver colloidal sol that particle diameter is 2 nanometers is can obtain after being irradiated 2 hours with light with violet rays source.
Embodiment 3
First, silver nitrate and water are mixed by the requirement that silver content in solution is 10000pm, is added in silver nitrate solution Sodium stearyl sulfate or odium stearate, then toward adding diisooctyl succinate sodium sulfonate in solution(AOT), in displacing solution Harmful anion, be obtained mixed solution after stir 20 minutes, then, the mixed solution that will be obtained carries out slaking reaction, specifically Ground, the small particle nano silver colloidal sol that particle diameter is 2 nanometers is can obtain after being irradiated 24 hours with light with violet rays source, and nanometer is obtained The TEM results of silver are as shown in figure 1, particle diameter distribution is as shown in Fig. 2 antibacterial experiment result is as shown in Figure 3.

Claims (5)

1. a kind of preparation method of food-grade small particle nano silver colloidal sol, comprises the following steps:
Step one, by silver nitrate and water by silver content in solution for the requirement of 20-10000pm is mixed, in silver nitrate solution Middle addition surfactant, stirs 10-30 minutes after mixed solution is obtained;
Step 2, the mixed solution that step one is obtained carries out slaking reaction, and concrete mode is irradiated with light with violet rays source The small particle nano silver colloidal sol that particle diameter is 1-5 nanometers is can obtain after 30 minutes to 24 hours.
2. the Nano Silver that a kind of preparation method of food-grade small particle nano silver colloidal sol according to claim 1 is prepared Colloidal sol, nanometer silver antimicrobial spray is can be made into after being diluted through sterile workshop and equipment deionized water.
3. the preparation method of food-grade small particle nano silver colloidal sol according to claim 1, it is characterised in that in step one Succinic acid di-isooctyl sulfonic acid is added after silver nitrate and water are mixed by silver content in solution for the requirement of 20-10000pm Sodium(AOT), displace the harmful anion in solution.
4. the preparation method of food-grade small particle nano silver colloidal sol according to claim 1, it is characterised in that in step one Surfactant be sodium stearyl sulfate or odium stearate.
5. the preparation method of food-grade small particle nano silver colloidal sol according to claim 1, it is characterised in that obtained to receive The average grain diameter of silver is at 2 nanometers in rice silver sol.
CN201611245866.4A 2016-12-29 2016-12-29 A kind of preparation method of food-grade small particle nano silver colloidal sol Pending CN106735308A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112920766A (en) * 2021-01-30 2021-06-08 高时(厦门)石业有限公司 Two-component antibacterial silicone sealant and preparation method thereof
CN114541169A (en) * 2022-02-18 2022-05-27 广东宝佳利新材料股份有限公司 Recyclable composite packaging bag

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100557314B1 (en) * 2004-11-08 2006-03-06 (주)바이오드림스 Nano-silicasilver and method for the preparation thereof
CN101791704A (en) * 2010-03-25 2010-08-04 江苏大学 Method for preparing nano silver
CN101999412A (en) * 2010-11-19 2011-04-06 佘振定 Nano-silver solution and preparation method thereof
CN102532376A (en) * 2010-12-28 2012-07-04 合肥杰事杰新材料股份有限公司 Method for preparing nano Ag/PVP (polyvinyl pyrolidone) composite material by utilizing ultraviolet irradiation
CN102935513A (en) * 2012-10-17 2013-02-20 武汉康银高科有限公司 Stable nanometer silver colloidal sol and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100557314B1 (en) * 2004-11-08 2006-03-06 (주)바이오드림스 Nano-silicasilver and method for the preparation thereof
CN101791704A (en) * 2010-03-25 2010-08-04 江苏大学 Method for preparing nano silver
CN101999412A (en) * 2010-11-19 2011-04-06 佘振定 Nano-silver solution and preparation method thereof
CN102532376A (en) * 2010-12-28 2012-07-04 合肥杰事杰新材料股份有限公司 Method for preparing nano Ag/PVP (polyvinyl pyrolidone) composite material by utilizing ultraviolet irradiation
CN102935513A (en) * 2012-10-17 2013-02-20 武汉康银高科有限公司 Stable nanometer silver colloidal sol and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112920766A (en) * 2021-01-30 2021-06-08 高时(厦门)石业有限公司 Two-component antibacterial silicone sealant and preparation method thereof
CN114541169A (en) * 2022-02-18 2022-05-27 广东宝佳利新材料股份有限公司 Recyclable composite packaging bag

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Application publication date: 20170531