CN107518004A - A kind of preparation method of Nanometer Copper antibacterial granule - Google Patents

A kind of preparation method of Nanometer Copper antibacterial granule Download PDF

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Publication number
CN107518004A
CN107518004A CN201610452682.9A CN201610452682A CN107518004A CN 107518004 A CN107518004 A CN 107518004A CN 201610452682 A CN201610452682 A CN 201610452682A CN 107518004 A CN107518004 A CN 107518004A
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CN
China
Prior art keywords
preparation
nanometer copper
antibacterial granule
copper antibacterial
chitosan
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201610452682.9A
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Chinese (zh)
Inventor
范佳晨
赵云龙
徐丹
徐凯
徐再
赵维达
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Zhangjiagang Shanmu New Material Technology Development Co Ltd
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Zhangjiagang Shanmu New Material Technology Development Co Ltd
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Priority to CN201610452682.9A priority Critical patent/CN107518004A/en
Publication of CN107518004A publication Critical patent/CN107518004A/en
Withdrawn legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16Heavy metals; Compounds thereof
    • A01N59/20Copper
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

This application discloses a kind of preparation method of Nanometer Copper antibacterial granule, including step:(1), carboxymethyl chitosan and copper sulfate solution are dissolved in distilled water, and are stirred;(2) mixed solution, is warming up to 40~50 DEG C, N is added under stirring2H4·H2O, continue to be stirred;(3), centrifugation, supersound washing and drying, Nanometer Copper antibacterial granule is obtained.Nanometer Copper antibacterial granule of the present invention has good antibacterial, bactericidal action, Durability of antimicrobial effect length to Escherichia coli, staphylococcus aureus.

Description

A kind of preparation method of Nanometer Copper antibacterial granule
Technical field
The application is related to a kind of anti-biotic material, more particularly to a kind of preparation method of Nanometer Copper antibacterial granule.
Background technology
At present, the conventional inorganic antiseptic of in the market is silver system and zinc series antibacterial agent, though silver-series antibacterial agent is with higher Sterilizing ability, but because it has higher 0.798 volt of chemical potential (25 DEG C), chemical stability is poor, is irradiated in ultraviolet Lower or after being heated to certain temperature, silver ion is reduced to argent, and is immediately converts into silver oxide, makes that product is graying, blackening, This not only lowers its commercial value, also reduces its anti-microbial property.In addition, silver-series antibacterial agent price is higher, fungal resistance It is weaker.Though zinc series antibacterial agent is without discoloration problem, cheap, its anti-microbial property is low, it is impossible to meets antibacterial requirement.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Nanometer Copper antibacterial granule, with overcome it is of the prior art not Foot.
To achieve the above object, the present invention provides following technical scheme:
The embodiment of the present application discloses a kind of preparation method of Nanometer Copper antibacterial granule, including step:
(1), carboxymethyl chitosan and copper sulfate solution are dissolved in distilled water, and are stirred;
(2) mixed solution, is warming up to 40~50 DEG C, N is added under stirring2H4·H2O, continue to be stirred;
(3), centrifugation, supersound washing and drying, Nanometer Copper antibacterial granule is obtained.
Preferably, in the preparation method of above-mentioned Nanometer Copper antibacterial granule, in step (1), the system of carboxymethyl chitosan Preparation Method includes:Dissolve chitosan in absolute ethyl alcohol and stir, then add sodium hydroxide solution and carry out swell 4~5 Hour;Add monoxone to be well mixed, be then centrifuged for separation, supersound washing and drying, obtain carboxymethyl chitosan.
Preferably, in the preparation method of above-mentioned Nanometer Copper antibacterial granule, the concentration of the sodium hydroxide solution is 40%.
Preferably, in the preparation method of above-mentioned Nanometer Copper antibacterial granule, the chitosan and chloroacetic mass ratio For (2.7~3):2.
Preferably, in the preparation method of above-mentioned Nanometer Copper antibacterial granule, the copper sulfate solution concentration is 0.078mol/L。
Preferably, in the preparation method of above-mentioned Nanometer Copper antibacterial granule, the carboxymethyl chitosan and copper sulphate Mol ratio is (2~3):1.
Compared with prior art, the advantage of the invention is that:Nanometer Copper antibacterial granule of the present invention is to Escherichia coli, golden yellow Staphylococcus has good antibacterial, bactericidal action, Durability of antimicrobial effect length.
Embodiment
The present invention is described further by the following example:According to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
Embodiment 1
The preparation method of Nanometer Copper antibacterial granule
(1), dissolve chitosan in absolute ethyl alcohol and stir, then add sodium hydroxide solution and carry out swell 4~5 Hour, the concentration of sodium hydroxide solution is 40%;Add monoxone to be well mixed, be then centrifuged for separation, supersound washing and drying, Obtain carboxymethyl chitosan.
Chitosan is 3 with chloroacetic mass ratio:2.
(2), carboxymethyl chitosan and copper sulfate solution are dissolved in distilled water, and are stirred, copper sulphate Concentration of aqueous solution is 0.078mol/L.
The mol ratio of carboxymethyl chitosan and copper sulphate is 3:1.
(3) mixed solution, is warming up to 50 DEG C, N is added under stirring2H4·H2O, continue to be stirred;
(4), centrifugation, supersound washing and drying, Nanometer Copper antibacterial granule is obtained.
Product is characterized using the methods of SEM, TEM, XRD, obtaining product has the crystal structure of face-centered cubic copper, Nano copper particle is flower-like structure, and particle size distribution is between 10~15nm.
Obtained product has good antibacterial, bactericidal action, Durability of antimicrobial effect to Escherichia coli, staphylococcus aureus It is long.
Embodiment 2
The preparation method of Nanometer Copper antibacterial granule
(1), dissolve chitosan in absolute ethyl alcohol and stir, then add sodium hydroxide solution and carry out swell 4~5 Hour, the concentration of sodium hydroxide solution is 40%;Add monoxone to be well mixed, be then centrifuged for separation, supersound washing and drying, Obtain carboxymethyl chitosan.
Chitosan is 2.8 with chloroacetic mass ratio:2.
(2), carboxymethyl chitosan and copper sulfate solution are dissolved in distilled water, and are stirred, copper sulphate Concentration of aqueous solution is 0.078mol/L.
The mol ratio of carboxymethyl chitosan and copper sulphate is 2.2:1.
(3) mixed solution, is warming up to 50 DEG C, N is added under stirring2H4·H2O, continue to be stirred;
(4), centrifugation, supersound washing and drying, Nanometer Copper antibacterial granule is obtained.
Product is characterized using the methods of SEM, TEM, XRD, obtaining product has the crystal structure of face-centered cubic copper, Nano copper particle is flower-like structure, and particle size distribution is in 13nm or so.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and Also include the other element that is not expressly set out, or also include for this process, method, article or equipment inherently Key element.

Claims (6)

1. a kind of preparation method of Nanometer Copper antibacterial granule, it is characterised in that including step:
(1), carboxymethyl chitosan and copper sulfate solution are dissolved in distilled water, and are stirred;
(2) mixed solution, is warming up to 40~50 DEG C, N is added under stirring2H4·H2O, continue to be stirred;
(3), centrifugation, supersound washing and drying, Nanometer Copper antibacterial granule is obtained.
2. the preparation method of Nanometer Copper antibacterial granule according to claim 1, it is characterised in that:In step (1), carboxymethyl The preparation method of chitosan includes:Dissolve chitosan in absolute ethyl alcohol and stir, then add sodium hydroxide solution and enter Row swell 4~5 hours;Add monoxone to be well mixed, be then centrifuged for separation, supersound washing and drying, obtain carboxymethyl chitosan Sugar.
3. the preparation method of Nanometer Copper antibacterial granule according to claim 1, it is characterised in that:The sodium hydroxide solution Concentration be 40%.
4. the preparation method of Nanometer Copper antibacterial granule according to claim 1, it is characterised in that:The chitosan and chloroethene The mass ratio of acid is (2.7~3):2.
5. the preparation method of Nanometer Copper antibacterial granule according to claim 1, it is characterised in that:The copper sulfate solution Concentration is 0.078mol/L.
6. the preparation method of Nanometer Copper antibacterial granule according to claim 1, it is characterised in that:The carboxymethyl chitosan Mol ratio with copper sulphate is (2~3):1.
CN201610452682.9A 2016-06-21 2016-06-21 A kind of preparation method of Nanometer Copper antibacterial granule Withdrawn CN107518004A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610452682.9A CN107518004A (en) 2016-06-21 2016-06-21 A kind of preparation method of Nanometer Copper antibacterial granule

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610452682.9A CN107518004A (en) 2016-06-21 2016-06-21 A kind of preparation method of Nanometer Copper antibacterial granule

Publications (1)

Publication Number Publication Date
CN107518004A true CN107518004A (en) 2017-12-29

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113016823A (en) * 2021-02-02 2021-06-25 南京师范大学 Preparation method of photo-thermal antibacterial near-infrared bimetallic nanoparticles
CN113273580A (en) * 2021-06-07 2021-08-20 广东顾纳凯材料科技有限公司 Antibacterial agent and preparation method thereof, antibacterial polyolefin composite material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101223887A (en) * 2008-01-31 2008-07-23 吴继贤 Nano silver antimicrobial solution and preparing method thereof
CN102388908A (en) * 2011-09-20 2012-03-28 合肥学院 Preparation process of silver/chitosan composite antimicrobial agents
CN104145993A (en) * 2014-08-04 2014-11-19 太原理工大学 Method for preparing complex antimicrobial agent by blending chitosan and silver copper
CN104642385A (en) * 2015-01-07 2015-05-27 安徽瀚驰生物科技有限公司 Composite bactericide of nano copper and polyhexamethylene guanidine and processing technic

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101223887A (en) * 2008-01-31 2008-07-23 吴继贤 Nano silver antimicrobial solution and preparing method thereof
CN102388908A (en) * 2011-09-20 2012-03-28 合肥学院 Preparation process of silver/chitosan composite antimicrobial agents
CN104145993A (en) * 2014-08-04 2014-11-19 太原理工大学 Method for preparing complex antimicrobial agent by blending chitosan and silver copper
CN104642385A (en) * 2015-01-07 2015-05-27 安徽瀚驰生物科技有限公司 Composite bactericide of nano copper and polyhexamethylene guanidine and processing technic

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113016823A (en) * 2021-02-02 2021-06-25 南京师范大学 Preparation method of photo-thermal antibacterial near-infrared bimetallic nanoparticles
CN113273580A (en) * 2021-06-07 2021-08-20 广东顾纳凯材料科技有限公司 Antibacterial agent and preparation method thereof, antibacterial polyolefin composite material and preparation method thereof

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