CN107549476A - A kind of high antimicrobial nano feed addictive and preparation method thereof - Google Patents
A kind of high antimicrobial nano feed addictive and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high antimicrobial nano feed addictive and preparation method thereof, belong to feed and technical field of nano material.High antimicrobial nano feed addictive is the compound of Nanometer Copper and nano zine oxide, wherein, Nanometer Copper is 1 with nano zine oxide weight ratio:1~6.The high antimicrobial nano feed addictive of the present invention is with Nanometer Copper and nano zine oxide substitution conventional antibiotic, courses of infection can not only be prevented and treated, strengthen body's immunity and antistress function, growth of animal can also be effectively facilitated, improve efficiency of feed utilization, and drug resistance is not produced, it is a kind of green, the functional feedstuff additive of safety.Secondly, high antimicrobial nano feed addictive preparation technology of the invention is simple, and production cost is relatively low, has important economy and social effect, and development prospect is wide.
Description
Technical field
The invention belongs to feed and technical field of nano material, and in particular to a kind of high antimicrobial nano feed addictive and its
Preparation method.
Background technology
Modern Animal Husbandry is intensive, maximization, mechanization feeding and management condition under, the ecological environment of animal feeding is disliked
Change, epidemic disease infection, nutritional deficiency the problems such as occur in succession, traditional prevention and controls such as by antibioticses growth promoter, high-copper,
High zinc preparation etc. is used as feed addictive, not only promotes giving full play to for breeding performonce fo animals, and prevents courses of infection,
The economic benefit of aquaculture is drastically increased, so far, Antibiotic Additive is still in global feed addictive sales volume
The maximum a kind of additive of proportion.But the abuse of antibiotic to animal in itself, livestock products and environment etc. bring one
The adverse effect of series, such as make pathogen produce drug resistance, reduce body's immunity, be also easy to produce the cross-infections of pathogenic bacteria with
And antibiotic a large amount of residuals etc. in body;Secondly, use lack of standardization of high-copper, high zinc preparation be easily caused animal body be poisoned,
The seondary effect such as environmental pollution and the wasting of resources.In recent years, people increasingly pay close attention to food security, feed safety and the resistance of bacterium
Property the problems such as, European Union completely forbade since 2006 and antibiotic is added in animal feed, China and it is some other country
Antibiotic is successively gradually limited as feed addictive.Therefore, green, safety, the research and development application meaning of functional feedstuff additive
Justice is great.
Nano material refer in three dimensions at least one dimension be in nanoscale scope (1~100nm) or by
The material that they are formed as basic component units.Nano-space is the relatively independent middle neck between both macro and micro
Domain.Nano-particle has small-size effect, surface and interfacial effect, quantum size effect and macro quanta tunnel effect, makes
Nano-particle has many special natures not available for conventional particle.Research shows, metal nanoparticle such as silver, zinc, copper
Deng having good antibiotic property.Wherein, nano silver antimicrobials excellent performance, but silver is noble metal, and application cost is higher, and Ag+
Can be with the Cl in aqueous medium-、HS-、S2-And SO4 2-Reacted etc. a variety of anion, form AgCl and Ag not soluble in water2S, from
And lose antibacterial activity.Compared with Nano Silver, Nanometer Copper and Nano-Zinc cost are relatively low, and bactericidal effect is only second to Nano Silver, and has
Have higher chemical stability and environmental safety, secondly, copper and zinc are the necessary trace elements of human body, harm to the human body compared with
It is small, had broad application prospects in field of fodder.Because China's nano anti-biotic material studies starting evening, weak foundation, application
Research hysteresis, technology is incomplete, and therefore, the applied basic research field innovation in technology source has important economic and social valency
Value.
The content of the invention
It is an object of the present invention in view of the shortcomings of the prior art, there is provided a kind of high antimicrobial nano feed addictive, the feeding
Feed additives can not only prevent and treat courses of infection, strengthen body's immunity and antistress function, moreover it is possible to effectively facilitate
Growth of animal, efficiency of feed utilization is improved, and do not produce drug resistance, be a kind of green, the functional feedstuff additive of safety.
It is a further object to provide a kind of preparation technology of high antimicrobial nano feed addictive, feed addition
Agent preparation technology is simple, and production cost is relatively low, has important economy and social effect, and development prospect is wide.
The present invention is achieved through the following technical solutions:
A kind of high antimicrobial nano feed addictive, including following raw materials:Nanometer Copper, nano zine oxide, wherein, Nanometer Copper with
Nano zine oxide weight ratio is 1:1~6.
Preferably, a kind of high antimicrobial nano feed addictive, including following raw materials:Nanometer Copper, nano zine oxide, wherein,
Nanometer Copper is 1 with nano zine oxide weight ratio:1~3.
A kind of preparation method of high antimicrobial nano feed addictive, comprises the following steps:
A, the preparation of Nanometer Copper
(1) copper nitrate solution and ascorbic acid solution is respectively configured;
(2) a certain amount of polyvinylpyrrolidone is weighed, is dissolved in copper nitrate solution, the water-bath under magnetic agitation effect
It is heated to 30~70 DEG C;
(3) ascorbic acid solution is added into step (2) resulting solution, is well mixed, is placed in ultrasonic reactor and reacts
After a period of time, room temperature is gradually cooling to;
(4) solution of cooling is diluted with ethanol, 10000r/min, centrifuges 10min, remove supernatant liquor, this process weight
It is multiple 3 times;
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, produces nano copper particle;
B, the preparation of nano zine oxide
(1) weigh a certain amount of zinc nitrate to be dissolved in deionized water, configure certain density zinc nitrate solution;
(2) sucrose ester is added in zinc nitrate solution obtained by step (1) and carries out dispersing and dissolving, be configured to sucrose ester-nitre
Sour zinc solution;
(3) step (2) resulting solution is added dropwise in sodium hydroxide solution, 30~90min of electric stirring, solution has
White opacity generates;
(4) the white opacity liquid that step (3) generates is transferred in ultrasonic reactor and carries out ultrasonic reaction;
(5) reaction mixture obtained by step (4) is centrifuged into 10min under 4000r/min, removes supernatant liquor, production
Thing is washed 3 times with distilled water and absolute ethyl alcohol successively;
(6) step (5) products therefrom is placed in 60 DEG C of vacuum drying chambers and dries 12h, produce nano granular of zinc oxide;
C, the preparation of high antimicrobial nano feed addictive
Nanometer Copper obtained by step A is well mixed with step B gained nano zine oxides by certain weight ratio, both it is of the invention
The high antimicrobial nano feed addictive.
Preferably, in the step A, step (1) copper nitrate solution concentration is 0.06~0.35mol/L;Ascorbic acid is molten
Liquid concentration is 0.5~1.5mol/L, and solvent is ethanol.
Preferably, in the step A, step (2) copper nitrate is 1 with polyvinylpyrrolidone mol ratio:1~1:30;Step
Suddenly (3) copper nitrate and ascorbic acid mol ratio are 1:1~1:3.
Preferably, in the step A, step (3) the ultrasonic reaction time is 10~40min.
Preferably, in the step B, step (1) nitric acid zinc concentration is 0.1~1.0mol/L;Step (2) resulting solution sugarcane
Sugar ester concentration is 0.01~0.5g/L.
Preferably, in the step B, the concentration proportion of step (3) sodium hydroxide and zinc nitrate is 1.0~3.0.
Preferably, in the step B, step (4) ultrasonic reaction condition is:50~90 DEG C of reaction temperature, the reaction time 5~
25min, 200~800W of reaction power.
Each composition mechanism of action of the present invention is as follows:
Nanometer Copper:Copper is distributed mainly in liver, brain, kidney, the heart, the pigment part of eye and the hair of animal, is both a variety of enzymes
Important component, be again hematopoiesis and prevent trace element necessary to alimentary anemia;Copper can be catalyzed ferroheme and red blood cell
Formation, and can safeguards the integrality of eucaryotic cell structure and function, to the hematolymphiod function of animal body, nerve cell, bone,
Connective tissue and hair grow and breeding performonce fo animals have positive facilitation.Nanometer Copper is reduced by copper ion
It is made into zerovalent copper, compared with traditional elemental copper, Nanometer Copper also has in addition to the nutrition physiology effect with common elemental copper
Small-size effect and surface-active effect, in animal body, it can be reduced by Passive diffusion or itself unique absorption pattern
To carrier, the needs of energy and consumption, its absorption and use efficiency is improved, reduces the addition in feed, so as to improve animal
Production cultivation comprehensive benefit.Secondly, Nanometer Copper also has significant antibacterial action, and research shows, its to staphylococcus aureus,
The pathogens such as Escherichia coli, Pseudomonas aeruginosa have excellent restraining and sterilizing bacteria effect.
Nano zine oxide:Zinc is the composition or activating agent of many enzymes of animal body, be archaeal dna polymerase, RNA polymerase,
The important composition composition of thymidine, nucleotidase, participate in a series of processes such as DNA replication dna, transcription and regulation protein synthesis.
Nano zine oxide, it is nonpoisonous and tasteless, nonirritant, it can effectively kill staphylococcus aureus, Candida albicans, Escherichia coli etc.
Pathogen, and there is slow release long-acting due to its spongy multi-cellular structure.Nano zine oxide Antibacterial Mechanism includes:I zinc from
Sub- active antibacterial mechanism:Bacterium is generally negatively charged, and the zinc ion of positively charged is firmly tied by Coulomb attraction with bacterial cell membrane
Be combined into cell, reacted with the sulfydryl in cell, make protein denaturation so that bacterium lose division growth ability and
Death, after thalline is killed, zinc ion is contacted by sedimentation equilibrium again separate out with other bacterium colonies, and it is thin to carry out a new round
Bacterium is killed;Secondly, zinc ion can also destroy electric transmission system, respiratory system and the transport of substances system of microorganism;II light is urged
Change Antibacterial Mechanism:After nano zine oxide receives the irradiation of light, the electron hole with strong oxidizing property, oxidation Decomposition bacterium are produced
Cell membrane and cell membrane, play bactericidal action;III active oxygen Antibacterial Mechanism:Nano zine oxide contacts meeting with water in atmosphere
Produce the H with strong oxidizing property2O2, the materials such as bacteria cell wall are destroyed, so as to reach sterilization purpose.
Polyvinylpyrrolidone:Polyvinylpyrrolidone abbreviation PVP, is a kind of non-ionic macromolecule compound, has
Hypotoxicity, physiological compatibility and excellent solubility property, are widely used in fields such as medicine, food, cosmetics.In PVP molecules
O, N lone pair electrons can be with Cu2+Between form covalent bond, PVP-Cu is formed in reaction system2+Complicated complexing body, when also
Former agent is Cu2+When being reduced into copper nano-particle, the steric hindrance that this complexing body is formed can play the work for preventing copper particle from reuniting
With.For copper nanoparticle because particle is smaller, the atom number for being in wafer surface areas is more so that its activity is than in crystal
The atom in portion is high, extremely unstable.Therefore, appropriate PVP is added in preparation process as protective agent, can effectively be prevented
Only nano copper particle is reunited, and is increased granule stability, is preferably received so as to obtain narrow particle size distribution range, good dispersion, crystal formation
Rice copper powder.
Sucrose ester:Sucrose fatty ester abbreviation sucrose ester, it is the ester type compound as made from pure sugar and fat oil, is applicable
In nontoxic, the biodegradable nonionic surface active agent of food and beverage.The steric hindrance effect of sucrose ester can have
Effect suppresses the adhesion of nanocrystal, prevents the reunion of nano zinc oxide particles, reduce toxicity in nano material building-up process and
Pollution to environment.In recent years, sucrose ester has been used as surfactant nano materials in microemulsion method, such as vulcanizes
Lead, cadmium sulfide, nickel sulfide and brushite etc..
Beneficial effects of the present invention:
1st, the effect of of the invention composition Nanometer Copper and nano zine oxide there is good stability, Cell permeable, medicine
Slow release and concerted effect, thus more significant biological effect can be played when being contacted with pathogenic microorganism, there is stronger antibacterial
Activity.
2nd, a kind of high antimicrobial nano feed addictive of the invention can not only prevent and treat courses of infection, strengthen body
Immunologic function and antistress function, moreover it is possible to effectively facilitate growth of animal, improve efficiency of feed utilization, and do not produce drug resistance, be one
Kind green, the functional feedstuff additive of safety.
3rd, a kind of high antimicrobial nano feed addictive of the invention, preparation technology is simple, and production cost is relatively low, has important
Economy and social effect, development prospect is wide.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
A kind of high antimicrobial nano feed addictive, including following raw materials:Nanometer Copper, nano zine oxide, wherein, Nanometer Copper with
Nano zine oxide weight ratio is 1:1.
A kind of preparation method of above-mentioned high antimicrobial nano feed addictive, comprises the following steps:
A, the preparation of Nanometer Copper
(1) 0.06mol copper nitrates and 1.5mol ascorbic acid are weighed respectively, is dissolved in respectively in 1L ethanol, and configuration concentration is
0.06mol/L copper nitrate solution and concentration is 1.5mol/L ascorbic acid solution;
(2) 1.8mol polyvinylpyrrolidones are weighed, is dissolved in 1L0.06mol/L copper nitrate solutions, makes copper nitrate
It is 1 with polyvinylpyrrolidone mol ratio:30, heating water bath is to 50 DEG C under magnetic agitation effect;
(3) 40mL1.5mol/L ascorbic acid solution is added into step (2) resulting solution, makes copper nitrate and Vitamin C
Sour mol ratio is 1:1, it is well mixed, is placed in ultrasonic reactor after reacting 40min, is gradually cooling to room temperature;
(4) after the solution of cooling is diluted with ethanol, 10000rpm/min centrifugation 10min, supernatant liquor, this process are removed
It is repeated 3 times;
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, produces nano copper particle;
B, the preparation of nano zine oxide
(1) 0.1mol zinc nitrates are weighed to be dissolved in 1L deionized waters, configure 0.1mol/L zinc nitrate solution;
(2) 0.01g sucrose esters are added in zinc nitrate solution obtained by step (1) and carry out dispersing and dissolving, be configured to sucrose
Ester-zinc nitrate solution;
(3) step (2) resulting solution is added dropwise in 0.3mol/L sodium hydroxide solution, makes hydroxide in solution
The concentration proportion of sodium and zinc nitrate is 3.0, and electric stirring 30min, solution has white opacity generation;
(4) the white opacity liquid that step (3) generates is transferred in ultrasonic reactor, is 50 DEG C, reacts in reaction temperature
Under conditions of power is 200W, ultrasonic reaction 25min;
(5) reaction mixture obtained by step (4) is centrifuged into 10min under 4000r/min, removes supernatant liquor, production
Thing is washed 3 times with distilled water and absolute ethyl alcohol successively;
(6) step (5) products therefrom is placed in 60 DEG C of vacuum drying chambers and dries 12h, produce nano granular of zinc oxide;
C, the preparation of high antimicrobial nano feed addictive
It is 1 by Nanometer Copper obtained by step A and nano zine oxide weight ratio obtained by step B:1 is well mixed, both it is of the invention
The high antimicrobial nano feed addictive.
Embodiment 2
A kind of high antimicrobial nano feed addictive, including following raw materials:Nanometer Copper, nano zine oxide, wherein, Nanometer Copper with
Nano zine oxide weight ratio is 1:6.
A kind of preparation method of above-mentioned high antimicrobial nano feed addictive, comprises the following steps:
A, the preparation of Nanometer Copper
(1) 0.2mol copper nitrates and 1.0mol ascorbic acid are weighed respectively, is dissolved in respectively in 1L ethanol, and configuration concentration is
0.2mol/L copper nitrate solution and concentration is 1.0mol/L ascorbic acid solution;
(2) 4mol polyvinylpyrrolidones are weighed, are dissolved in 1L0.2mol/L copper nitrate solutions, make copper nitrate with gathering
Vinylpyrrolidone mol ratio is 1:20, heating water bath is to 30 DEG C under magnetic agitation effect;
(3) into step (2) resulting solution add 400mL1.0mol/L ascorbic acid solution, make copper nitrate with it is anti-bad
Hematic acid mol ratio is 1:2, it is well mixed, is placed in ultrasonic reactor after reacting 20min, is gradually cooling to room temperature;
(4) after the solution of cooling is diluted with ethanol, 10000rpm/min centrifugation 10min, supernatant liquor, this process are removed
It is repeated 3 times;
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, produces nano copper particle;
B, the preparation of nano zine oxide
(1) 1.0mol zinc nitrates are weighed to be dissolved in 1L deionized waters, configure 1.0mol/L zinc nitrate solution;
(2) 0.5g sucrose esters are added in zinc nitrate solution obtained by step (1) and carry out dispersing and dissolving, be configured to sucrose
Ester-zinc nitrate solution;
(3) step (2) resulting solution is added dropwise in 1.0mol/L sodium hydroxide solution, makes hydroxide in solution
The concentration proportion of sodium and zinc nitrate is 1.0, and electric stirring 90min, solution has white opacity generation;
(4) the white opacity liquid that step (3) generates is transferred in ultrasonic reactor, is 90 DEG C, reacts in reaction temperature
Under conditions of power is 800W, ultrasonic reaction 5min;
(5) reaction mixture obtained by step (4) is centrifuged into 10min under 4000r/min, removes supernatant liquor, production
Thing is washed 3 times with distilled water and absolute ethyl alcohol successively;
(6) step (5) products therefrom is placed in 60 DEG C of vacuum drying chambers and dries 12h, produce nano granular of zinc oxide;
C, the preparation of high antimicrobial nano feed addictive
It is 1 by Nanometer Copper obtained by step A and nano zine oxide weight ratio obtained by step B:6 is well mixed, both it is of the invention
The high antimicrobial nano feed addictive.
Embodiment 3
A kind of high antimicrobial nano feed addictive, including following raw materials:Nanometer Copper, nano zine oxide, wherein, Nanometer Copper with
Nano zine oxide weight ratio is 1:3.
A kind of preparation method of above-mentioned high antimicrobial nano feed addictive, comprises the following steps:
A, the preparation of Nanometer Copper
(1) 0.35mol copper nitrates and 0.5mol ascorbic acid are weighed respectively, is dissolved in respectively in 1L ethanol, and configuration concentration is
0.35mol/L copper nitrate solution and concentration is 0.5mol/L ascorbic acid solution;
(2) 0.35mol polyvinylpyrrolidones are weighed, is dissolved in 1L0.35mol/L copper nitrate solutions, makes copper nitrate
It is 1 with polyvinylpyrrolidone mol ratio:1, heating water bath is to 70 DEG C under magnetic agitation effect;
(3) into step (2) resulting solution add 2100mL0.5mol/L ascorbic acid solution, make copper nitrate with it is anti-bad
Hematic acid mol ratio is 1:3, it is well mixed, is placed in ultrasonic reactor after reacting 10min, is gradually cooling to room temperature;
(4) after the solution of cooling is diluted with ethanol, 10000rpm/min centrifugation 10min, supernatant liquor, this process are removed
It is repeated 3 times;
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, produces nano copper particle;
B, the preparation of nano zine oxide
(1) 0.4mol zinc nitrates are weighed to be dissolved in 1L deionized waters, configure 0.4mol/L zinc nitrate solution;
(2) 0.2g sucrose esters are added in zinc nitrate solution obtained by step (1) and carry out dispersing and dissolving, be configured to sucrose
Ester-zinc nitrate solution;
(3) step (2) resulting solution is added dropwise in 0.8mol/L sodium hydroxide solution, makes hydroxide in solution
The concentration proportion of sodium and zinc nitrate is 2.0, and electric stirring 70min, solution has white opacity generation;
(4) the white opacity liquid that step (3) generates is transferred in ultrasonic reactor, is 70 DEG C, reacts in reaction temperature
Under conditions of power is 400W, ultrasonic reaction 15min;
(5) reaction mixture obtained by step (4) is centrifuged into 10min under 4000r/min, removes supernatant liquor, production
Thing is washed 3 times with distilled water and absolute ethyl alcohol successively;
(6) step (5) products therefrom is placed in 60 DEG C of vacuum drying chambers and dries 12h, produce nano granular of zinc oxide;
C, the preparation of high antimicrobial nano feed addictive
It is 1 by Nanometer Copper obtained by step A and nano zine oxide weight ratio obtained by step B:3 is well mixed, both it is of the invention
The high antimicrobial nano feed addictive.
Application Example
A kind of inhibitory action of the high antimicrobial nano feed addictive of the present invention to pathogen
1st, test sample:High antimicrobial nano feed addictive prepared by above-described embodiment 1~3.
2nd, pathogen is tested:Staphylococcus aureus, Escherichia coli, pseudomonas aeruginosa, Candida albicans.
3rd, test culture medium:Bacterium is beef extract-peptone bacteria culture media;Candida albicans is husky Bao Shi culture mediums.
4th, assay method:
(1) in 250mL triangular flasks plus people's 70mL0.03mol/L phosphate buffers, high pressure steam sterilization is standby, and (pressure is
9.8×104Pa, temperature are 121 DEG C, time 30min);
(2) in above-mentioned triangular flask, the feed addictive to be measured of the preparation of above-described embodiment 1~3 and disease to be measured are separately added into
Opportunistic pathogen bacterium solution, make the μ g/mL of concentration 500 of feed addictive, the concentration of bacterium solution is 2 × 104Cfu/mL, bacterium solution is through micro- sem observation
It is determined that without other living contaminantses;
(3) control sample is not added with feed addictive, and other steps are with treating that test sample is identical;
(4) above-mentioned triangular flask is fixed on vibration shaking table, 250r/min, 37 DEG C of constant temperature oscillation lh, takes 0.5mL triangular flasks
Interior sample is added in a diameter of 9cm sterile petri dish, is added after 18mL melts and is cooled to 45 DEG C of culture medium, rapid light
Jog is dynamic to be mixed, and is lain against on platform;
(5) after culture medium solidifying, culture dish is overturn, makes bottom upward, put culture 48h (Candida albicans in 37 DEG C of insulating boxs
Bacterium cultivates 72h), observation clump count (i.e. remaining number of viable), the antibacterial of feed addictive prepared by comparing embodiment 1~3
Performance.
According to above method, each all product to be measured and control sample respectively do 3 parts of experiments of a formula, and replication 3 times, take
The mean value calculation of 3 experiments goes out sterilization rate.Due to the death of bacterium and saccharomycete be it is disposable, can by the use of sterilization rate as
Index evaluates the anti-microbial property of feed nano additive.Sterilization rate is calculated using following formula:
Sterilization rate=(control group average colony number-sample group average colony number) × 100%/control group average colony number
5th, test result:Testing result is as shown in table 1 below.
The high antimicrobial nano feed addictive sterilization rate measurement result of table 1
6th, conclusion
After testing, it is (golden yellow can effectively to suppress gram-positive bacteria with a kind of high antimicrobial nano feed addictive of the invention
Color staphylococcus, Candida albicans) and Gram-negative bacteria (Escherichia coli, pseudomonas aeruginosa) growth, and to gram
The inhibition of negative bacterium is better than gram-positive bacteria, and this may be with the two cell wall structure, composition and growthform
It is different related.Secondly, bacteriostatic experiment shows, embodiment 3 shows embodiment 3 for the present invention sterilizing rate highest of 4 kinds of pathogens
Optimal preparation technology.
Claims (9)
1. a kind of high antimicrobial nano feed addictive, it is characterised in that including following raw materials:Nanometer Copper, nano zine oxide, its
In, Nanometer Copper is 1 with nano zine oxide weight ratio:1~6.
2. a kind of high antimicrobial nano feed addictive according to claim 1, it is characterised in that including following raw materials:Receive
Rice copper, nano zine oxide, wherein, Nanometer Copper is 1 with nano zine oxide weight ratio:1~3.
3. a kind of preparation method of high antimicrobial nano feed addictive as claimed in claim 1 or 2, comprises the following steps:
A, the preparation of Nanometer Copper
(1) copper nitrate solution and ascorbic acid solution is respectively configured;
(2) a certain amount of polyvinylpyrrolidone is weighed, is dissolved in copper nitrate solution, the heating water bath under magnetic agitation effect
To 30~70 DEG C;
(3) ascorbic acid solution is added into step (2) resulting solution, be well mixed, be placed in ultrasonic reactor and react one section
After time, room temperature is gradually cooling to;
(4) solution of cooling is diluted with ethanol, 10000r/min, centrifuges 10min, remove supernatant liquor, this process repeats 3
It is secondary;
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, produces nano copper particle;
B, the preparation of nano zine oxide
(1) weigh a certain amount of zinc nitrate to be dissolved in deionized water, configure certain density zinc nitrate solution;
(2) sucrose ester is added in zinc nitrate solution obtained by step (1) and carries out dispersing and dissolving, be configured to sucrose ester-zinc nitrate
Solution;
(3) step (2) resulting solution is added dropwise in sodium hydroxide solution, 30~90min of electric stirring, solution has white
Muddiness generation;
(4) the white opacity liquid that step (3) generates is transferred in ultrasonic reactor and carries out ultrasonic reaction;
(5) reaction mixture obtained by step (4) is centrifuged into 10min under 4000r/min, removes supernatant liquor, product according to
It is secondary to be washed 3 times with distilled water and absolute ethyl alcohol;
(6) step (5) products therefrom is placed in 60 DEG C of vacuum drying chambers and dries 12h, produce nano granular of zinc oxide;
C, the preparation of high antimicrobial nano feed addictive
Nanometer Copper obtained by step A is well mixed with step B gained nano zine oxides by certain weight ratio, both it is of the present invention
High antimicrobial nano feed addictive.
A kind of 4. preparation method of high antimicrobial nano feed addictive according to claim 3, it is characterised in that the step
In rapid A, step (1) copper nitrate solution concentration is 0.06~0.35mol/L;Ascorbic acid solution concentration is 0.5~1.5mol/L,
Solvent is ethanol.
A kind of 5. preparation method of high antimicrobial nano feed addictive according to claim 3, it is characterised in that the step
In rapid A, step (2) copper nitrate is 1 with polyvinylpyrrolidone mol ratio:1~1:30;Step (3) copper nitrate and ascorbic acid
Mol ratio is 1:1~1:3.
A kind of 6. preparation method of high antimicrobial nano feed addictive according to claim 3, it is characterised in that the step
In rapid A, step (3) the ultrasonic reaction time is 10~40min.
A kind of 7. preparation method of high antimicrobial nano feed addictive according to claim 3, it is characterised in that the step
In rapid B, step (1) nitric acid zinc concentration is 0.1~1.0mol/L;Step (2) resulting solution sucrose ester concentration is 0.01~0.5g/
L。
A kind of 8. preparation method of high antimicrobial nano feed addictive according to claim 3, it is characterised in that the step
In rapid B, the concentration proportion of step (3) sodium hydroxide and zinc nitrate is 1.0~3.0.
A kind of 9. preparation method of high antimicrobial nano feed addictive according to claim 3, it is characterised in that the step
In rapid B, step (4) ultrasonic reaction condition is:50~90 DEG C of reaction temperature, 5~25min of reaction time, reaction power 200~
800W。
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CN110051837A (en) * | 2019-04-08 | 2019-07-26 | 南京师范大学 | A kind of CuO/ZnO/Au nanoparticle and its preparation method and application |
CN113080316A (en) * | 2021-04-22 | 2021-07-09 | 宁夏京成天宝饲料添加剂有限公司 | Preparation method of antibiotic substitute nano zinc oxide |
CN114668021A (en) * | 2021-04-08 | 2022-06-28 | 上海涂固安高科技有限公司 | Food-grade multifunctional nano-composite and preparation and application thereof |
CN115024391A (en) * | 2022-06-27 | 2022-09-09 | 广东粤港澳大湾区国家纳米科技创新研究院 | Antibacterial feed additive and preparation method and application thereof |
WO2024063664A1 (en) * | 2022-09-23 | 2024-03-28 | Beointech D.O.O. Beograd | Ultrasonic low temperature synthesis of an advanced multifunctional additive for application in animal feed production |
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CN110051837A (en) * | 2019-04-08 | 2019-07-26 | 南京师范大学 | A kind of CuO/ZnO/Au nanoparticle and its preparation method and application |
CN110051837B (en) * | 2019-04-08 | 2021-05-11 | 南京师范大学 | CuO/ZnO/Au nano-particles and preparation method and application thereof |
CN114668021A (en) * | 2021-04-08 | 2022-06-28 | 上海涂固安高科技有限公司 | Food-grade multifunctional nano-composite and preparation and application thereof |
CN114668021B (en) * | 2021-04-08 | 2023-10-27 | 上海涂固安高科技有限公司 | Food-grade multifunctional nano-composite and preparation and application thereof |
CN113080316A (en) * | 2021-04-22 | 2021-07-09 | 宁夏京成天宝饲料添加剂有限公司 | Preparation method of antibiotic substitute nano zinc oxide |
CN113080316B (en) * | 2021-04-22 | 2022-09-30 | 宁夏京成天宝科技有限公司 | Preparation method of antibiotic substitute nano zinc oxide |
CN115024391A (en) * | 2022-06-27 | 2022-09-09 | 广东粤港澳大湾区国家纳米科技创新研究院 | Antibacterial feed additive and preparation method and application thereof |
WO2024063664A1 (en) * | 2022-09-23 | 2024-03-28 | Beointech D.O.O. Beograd | Ultrasonic low temperature synthesis of an advanced multifunctional additive for application in animal feed production |
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