CN108634098A - A kind of preparation method of pure green broad-spectrum antiseptic feed addictive - Google Patents
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive Download PDFInfo
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- CN108634098A CN108634098A CN201810389801.XA CN201810389801A CN108634098A CN 108634098 A CN108634098 A CN 108634098A CN 201810389801 A CN201810389801 A CN 201810389801A CN 108634098 A CN108634098 A CN 108634098A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract
The invention discloses a kind of preparation methods of pure green broad-spectrum antiseptic feed addictive, belong to animal feeding-stuff antibacterial additives technical field.The present invention spends this pure natural plant flower to extract broad-spectrum antiseptic substance with Paulownia elongata; it is the green broad spectrum antiseptic feed additive that carrier prepares prepared by the preparation method of pure green broad-spectrum antiseptic feed addictive that graphene, which is used in combination; it solves feed in livestock large-scale cultivation and adds antibiotic; antibiotic retains the problem of influencing food security in livestock body; this pure green broad-spectrum antiseptic feed addictive is easily digested and assimilated by livestock, and food security will not be impacted by not leading to the problem of residue.
Description
Technical field
The invention belongs to animal feeding-stuff antibacterial additives technical fields, are specifically related to a kind of pure green broad-spectrum antiseptic feed
The preparation method of additive.
Background technology
In recent years, as country carries forward vigorously centralization, the scale of aquaculture, aquaculture scale stable breeding has obtained length
The development of foot, the farm compared to traditional breeding way centralization scale need special feed, while scale stable breeding
Since the density of cultivation livestock is big, livestock obtains easily to be infected after being ill, and it is greatly loss to be brought to raiser, in order to reduce loss,
Raiser often adds a large amount of antibiotic in feed and falls ill to prevent livestock.
From the 50's ends of 20th century find the cause of disease bacterium to antibiotic have drug resistance since, antibiotic adds in feed
Caused safety issue becomes focus of people's attention.Harm of the antibiotic in livestock and poultry cultivation is mainly manifested in:(1)
So that pathogen is generated drug resistance, increases the artificial and fund input for the treatment of livestock and poultry, and existing veterinary drug can not be controlled
It treats, causes mortality of livestock high, cultivation loss is larger.(2) it is remained in body, influences the immune effect of humans and animals.For a long time
It uses, especially abuses, antibiotic can be caused to increase in the residual quantity of body.Drug remains in body, on the one hand may lure
Hair generates resistance to medication bacterium, and on the other hand remaining antibiotic reduces the immune effect of epidemic preventing vaccine again, in order to control the hair of epidemic disease
Life hides some dangers for.(3) it is also easy to produce the cross-infection of pathogenic bacteria.Using antibiotic, especially Use out of range, can destroy in enteron aisle
On the one hand microecological balance reduces the microorganism that Antibiotic Sensitivity is strong in gastrointestinal tract, and the flora of sensibility difference is taken advantage of the occasion
Mass propagation causes Dysbiosis;On the other hand it is the intrusion of micro-organisms in vitro after microorganism is eliminated by antibiotic in vivo
Breeding creates condition, to be also easy to produce pathogenic cross-infection.
Graphene is a kind of novel nano-material for the individual layer laminated structure being made of carbon atom, is the two of monoatomic thickness
Carbon atom crystal is tieed up, basic structural unit is most stable of benzene hexatomic ring in organic material, is current optimal two-dimensional nano
Material, graphene theoretical specific surface area are up to 2630m2/ g, adsorption capacity is extremely strong, and is hardly happened to the substance of absorption surface
Reaction, graphene itself is also nontoxic without other side effects, and good to bioaffinity, thus is that a kind of excellent drug carries
Body,
Fortune paulownia flower is the flower of goatweed paulownia, and paulownia are China native country species, have extensive distribution and China in China
One of the economic seed of forest of fast-growing, fortune paulownia flower is harvested when opening in spring, is dried or using fresh herb, has clearing heat and detoxicating, wind-dispelling heat-dissipating, eliminating dampness
Stop dysentery, the effect of clearing liver and improving vision.《Journal of Shanxi Agricultural University(Natural science edition)》6th phase in 2014 total 34th phase page 571
To the paper of page 576《The research of paulownia flower extract broad-spectrum antibacterial performance》Show that the extract of fortune paulownia flower has the anti-of wide spectrum
Bacterium performance, to aspergillus niger, aspergillus oryzae, bread mold, the wooden poison of green, bacillus subtilis, staphylococcus aureus, salmonella etc.
Common strain has stronger inhibitory activity.
In consideration of it, it is necessary to develop a kind of green broad spectrum antiseptic feed additive to substitute existing antibiotic, to promoting
The sustainable development of livestock large-scale cultivation, it is food-safe to have important meaning.
The Chinese patent that publication No. is CN105831445A discloses a kind of pig green feed of alternative antibiotic and adds
Add agent, belongs to feed additive field.The feed addictive is in parts by weight by 6-10 parts of fermentation feather fan bean dregs, Lactobacillus casei
0.4-0.8 parts of 3-5 parts of bacterium powder, 1-3 parts of plant polyose, 3-6 parts of Herba Lycopi, 2-5 parts of Longstamen Onion Bulb, 1-3 parts of Fructus Corni, multi-vitamins groups
At.The feed addictive is made of natural products, is had the characteristics that nontoxic, noresidue, is had no drug resistance, alternative antibiotic is in life
It is applied in swine rations, pig growth, strengthen immunity can not only be effectively facilitated, while pig-breeding environment can also be improved,
Lower feed safety hidden danger, market prospects are very wide.This additive belongs to the additive of Chinese herbal medicine, plays the work of prevention
With, but in the feed added, the additive amount needed is relatively more, furthermore the price of these Chinese herbal medicines itself is also somewhat expensive, it is uncomfortable
It closes and promotes.
The Chinese patent literature of Publication No. CN107549476A disclose a kind of high antibacterial feed nano additive and its
Preparation method belongs to feed and technical field of nano material.High antibacterial feed nano additive is Nanometer Copper and nano zine oxide
Compound, wherein Nanometer Copper and nano zine oxide weight ratio are 1:1-6.The present invention high antibacterial feed nano additive with
Nanometer Copper and nano zine oxide replace conventional antibiotic, can not only prevent and treat germ infection, enhance body's immunity
And antistress function, moreover it is possible to effectively facilitate growth of animal, improve efficiency of feed utilization, and do not generate drug resistance, be a kind of green, peace
Full functional feedstuff additive.Secondly, high antibacterial feed nano additive preparation process of the invention is simple, production cost compared with
It is low, have important economy and social effect, development prospect wide.There is also metal enrichments to be deposited in for actually this additive
In livestock body, hidden danger is brought to food security.
Invention content
In view of this, in view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of pure green broad-spectrum antiseptic feeds
The preparation method of additive spends this pure natural plant flower to extract broad-spectrum antiseptic substance, graphene is used in combination with Paulownia elongata
Pure green broad-spectrum antiseptic feed addictive is prepared for carrier, feed in livestock large-scale cultivation is solved and adds antibiotic, antibiosis
Element is retained the problem of influencing food security in livestock body, and this pure green broad-spectrum antiseptic feed addictive is easily digested by livestock and inhaled
It receives, food security will not be impacted by not leading to the problem of residue.
In order to achieve the above objectives, the present invention uses following technical scheme:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(1):Prepare graphene suspension;Prepare graphene or graphene oxide with oxidation-reduction method, be added to pure water or
In ethanol water, disperse graphene suspension or graphene oxide suspension, institute to be made in 1-24 hours under ul-trasonic irradiation
It is 20-60 DEG C to state and control the temperature of solution in ultrasonic wave dispersion process, and the frequency of the ultrasonic wave is 40HKz, the graphene
Or graphene oxide and the weight ratio of pure water or ethanol water are 1-4:1000.
Step(2):It prepares Paulownia elongata and spends extracting solution;Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, is used
Spin vibration sieve is sieved, and is solvent with pure water or 50% ethyl alcohol, 75% ethyl alcohol or 90% ethyl alcohol, ultrasonic wave stirring, standing, ultrasonic wave stirs again
It mixes, stand again, then in the lower temperature ultrasonic wave extraction 1 hour less than 100 DEG C, the frequency of the ultrasonic wave is 40HKz, then
To be solvent with pure water or 50% ethyl alcohol, 75% ethyl alcohol or 90% ethyl alcohol again, ultrasonic wave stirring, standing, ultrasonic wave stirs, is quiet again again
It sets, is then repeated twice in the step of lower temperature ultrasonic wave extraction 1 hour less than 100 DEG C, extracting solution three times is blended in
Paulownia elongata flower extracting solution is made together, the mesh number of the sieving is more than or equal to 40 mesh.
Step(3):Graphene suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure green of carrier
Color feed addictive;Graphene suspension is added in Paulownia elongata flower extracting solution, wherein graphene is spent dry with Paulownia elongata
Colored weight ratio is 2-8:100, it is then stirred by ultrasonic 1-24 hours, is put into drying box and removes most of moisture, wait for that moisture is waved
It takes out, is cooled to room temperature when being sent to solution into viscous pasty state, then dried with low temperature vacuum drier, the pure green that powdery is made is wide
Compose antiseptic feed additive.The temperature that solution is controlled in the ultrasonic wave dispersion process is 20-60 DEG C, the frequency of the ultrasonic wave
For 40HKz, the drying box is electric drying oven with forced convection, and the temperature of moisture removal of going of the electric drying oven with forced convection is 60-80
℃.The drying temperature of the low temperature vacuum drier is 25-50 DEG C, vacuum degree 1000-10000Pa.
The pre- prior art is compared, the beneficial effects of the invention are as follows:
1, the present invention has high specific surface using the carrier that graphene is green broad spectrum antiseptic feed additive, graphene
Product, specific surface area is bigger, and adsorption capacity is stronger, and a large amount of broad-spectrum antiseptic substance can be adsorbed with a small amount of graphene.
2, the graphene or graphene oxide for the oxidation-reduction method production that the present invention uses, technology maturation is cheap, makes
The great application value of the present invention, has a extensive future.
3, the present invention is using the green additive for substituting antibiotic is made of Paulownia elongata flower, with chemically synthesized antibiotic phase
Than being a kind of pure natural, noresidue, being the antibacterial additives of feed addition from now on to the green plants antibacterial of person poultry harmless
Developing direction, and eliminate antibiotic residue in livestock body, influence health of people, food security is promoted to play certain work
With.
4, the present invention compares other antibacterial green feed addictives, and active ingredient concentration is high, is bacterium suppression to various be harmful to
Effect processed is strong, has extensive preventive effect to the main pathogenic occurred in livestock large-scale cultivation.
5, Paulownia elongata of the invention is widely distributed at home, and ownership is huge, and Paulownia elongata flower can be collected nearby, no
It is limited by the place of production, moreover it is possible to promote the Advantageous developments of green environment.
6, the suitable large-scale industrial production of the present invention, helps to further reduce the cost, be brought to aquaculture maximum
Interests.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.
Embodiment one:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(1)Prepare graphene suspension;
The graphene prepared with oxidation-reduction method is added in pure water, is hanged with disperse to be made for 7 hours graphene under ul-trasonic irradiation
Supernatant liquid, the temperature of control solution is 40 DEG C in ultrasonic wave dispersion process, and the frequency of ultrasonic wave is 40KHz, graphene and pure water
Weight ratio is 3:1000.
Step(2)It prepares Paulownia elongata and spends extracting solution;
Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, 40 mesh sieve is crossed with spin vibration sieve, is solvent, Lankao with pure water
The weight ratio of fortune paulownia flower and pure water is 1:20, ultrasonic wave stirs 1 hour, stands 2 hours, then ultrasonic wave stirs 1 hour, then stands
2 hours, the frequency of then ultrasonic extraction 1 hour at 80 DEG C, ultrasonic wave was 40KHz, then again by Paulownia elongata flower and pure water
Ratio be 1:20, ultrasonic wave stirs 1 hour, stands 2 hours, then ultrasonic wave stirs 1 hour, then stands 2 hours, then 80
The step of ultrasonic extraction 1 hour, is repeated twice at DEG C, extracting solution three times is mixed, Paulownia elongata flower extracting solution is made.
Step(3)Graphene suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure green of carrier
Broad-spectrum antiseptic feed addictive.Graphene suspension is added in Paulownia elongata flower extracting solution, graphene is spent with Paulownia elongata
Weight ratio be 4:100, it is then stirred by ultrasonic 1.5 hours, the temperature of control solution is 60 DEG C in ultrasonic wave dispersion process, ultrasound
The frequency of wave is 40KHz, is put into electric drying oven with forced convection and removes most of moisture, and the temperature of electric heating forced air drying is 70 DEG C,
It takes out, is cooled to room temperature when moisture evaporation to solution is at viscous pasty state, then dried with low temperature vacuum drier, at 30 DEG C,
Vacuum degree is 10000Pa, and the pure green broad-spectrum antiseptic feed addictive of powdery is made.
Embodiment two:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(1)Prepare graphene suspension;
The graphene prepared with oxidation-reduction method is added in 90% ethanol water, disperses to be made for 3 hours under ul-trasonic irradiation
Graphene suspension, the temperature of control solution is 50 DEG C in ultrasonic wave dispersion process, and the frequency of ultrasonic wave is 40KHz, graphene
Weight ratio with 90% ethanol water is 2:1000.
Step(2)It prepares Paulownia elongata and spends extracting solution;
Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, 60 mesh sieve are crossed with spin vibration sieve, it is molten with 90% ethanol water
The weight ratio of agent, Paulownia elongata flower and 90% ethanol water is 1:30, ultrasonic wave stirs 1 hour, stands 12 hours, then ultrasound
Wave stirs 1 hour, then stands 12 hours, then ultrasonic extraction 1 hour at 95 DEG C, and the frequency of ultrasonic wave is 40KHz, then again
Ratio by Paulownia elongata flower and 90% ethanol water is 1:30, ultrasonic wave stirs 1 hour, stands 12 hours, then ultrasonic wave stirs
It mixes 1 hour, then stands 12 hours, be then repeated twice the step of ultrasonic extraction 1 hour at 95 DEG C, extracting solution three times is mixed
It is combined and Paulownia elongata flower extracting solution is made.
Step(3)Graphene suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure green of carrier
Broad-spectrum antiseptic feed addictive.Graphene suspension is added in Paulownia elongata flower extracting solution, graphene is spent with Paulownia elongata
Weight ratio be 6:100, it is then stirred by ultrasonic 1 hour, the temperature of control solution is 55 DEG C in ultrasonic wave dispersion process, ultrasonic wave
Frequency be 40KHz, be put into electric drying oven with forced convection and remove most of moisture, the temperature of electric heating forced air drying is 60 DEG C, is waited for
Moisture evaporation to solution at viscous pasty state when take out, be cooled to room temperature, then dried with low temperature vacuum drier, at 50 DEG C, very
Reciprocal of duty cycle is 6000Pa, and the pure green broad-spectrum antiseptic feed addictive of powdery is made.
Embodiment three:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(1)Prepare graphene oxide suspension;
The graphene oxide prepared with oxidation-reduction method is added in 75% ethanol water, small with dispersion 10 under ul-trasonic irradiation
When be made graphene oxide suspension, the temperature of control solution is 30 DEG C in ultrasonic wave dispersion process, and the frequency of ultrasonic wave is
The weight ratio of 40KHz, graphene oxide and 75% ethanol water is 3.5:1000.
Step(2)It prepares Paulownia elongata and spends extracting solution;
Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, 50 mesh sieve is crossed with spin vibration sieve, is solvent with 75% ethyl alcohol,
It is 1 that Paulownia elongata, which is spent with the weight ratio of 75% ethanol water,:10, ultrasonic wave stirs 1 hour, stands 3 hours, then ultrasonic wave stirs
It mixes 1 hour, then stands 3 hours, then ultrasonic extraction 1 hour at 60 DEG C, the frequency of ultrasonic wave is 40KHz, then again will be blue
The ratio for examining fortune paulownia flower and 75% ethanol water is 1:10, ultrasonic wave stirs 1 hour, stands 3 hours, then ultrasonic wave stirring 1 is small
When, then 3 hours are stood, is then repeated twice the step of ultrasonic extraction 1 hour at 60 DEG C, extracting solution three times is blended in one
It rises and Paulownia elongata flower extracting solution is made.
Step(3)Graphene oxide suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure of carrier
Green broad spectrum antiseptic feed additive.Graphene oxide suspension is added in Paulownia elongata flower extracting solution, graphene oxide
Weight ratio with Paulownia elongata flower is 8:100, it is then stirred by ultrasonic 2 hours, the temperature of solution is controlled in ultrasonic wave dispersion process
It it is 35 DEG C, the frequency of ultrasonic wave is 40KHz, is put into electric drying oven with forced convection and removes most of moisture, electric heating forced air drying
Temperature is 65 DEG C, takes out, is cooled to room temperature when moisture evaporation to solution is at viscous pasty state, then dry with low temperature vacuum drier
Dry, at 40 DEG C, the pure green broad-spectrum antiseptic feed addictive of powdery is made in vacuum degree 5000Pa.
Example IV:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(A)Prepare graphene oxide suspension;
The graphene oxide prepared with oxidation-reduction method is added in 50% ethanol water, small with dispersion 12 under ul-trasonic irradiation
When be made graphene oxide suspension, the temperature of control solution is 45 DEG C in ultrasonic wave dispersion process, and the frequency of ultrasonic wave is
The weight ratio of 40KHz, graphene oxide and 50% ethanol water is 4:1000.
Step(B)It prepares Paulownia elongata and spends extracting solution;
Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, 45 mesh sieve is crossed with spin vibration sieve, is solvent with 50% ethyl alcohol,
It is 1 that Paulownia elongata, which is spent with the weight ratio of 50% ethanol water,:8, ultrasonic wave stirs 1 hour, stands 5 hours, then ultrasonic wave stirring
1 hour, then stand 5 hours, then ultrasonic extraction 1 hour at 65 DEG C, the frequency of ultrasonic wave was 40KHz, then again by Lankao
The ratio of fortune paulownia flower and 50% ethanol water is 1:8, ultrasonic wave stirs 1 hour, stands 5 hours, then ultrasonic wave stirs 1 hour,
5 hours are stood again, are then repeated twice the step of ultrasonic extraction 1 hour at 65 DEG C, extracting solution three times is mixed
Paulownia elongata flower extracting solution is made.
Step(C)Graphene oxide suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure of carrier
Green broad spectrum antiseptic feed additive.Graphene oxide suspension is added in Paulownia elongata flower extracting solution, graphene oxide
Weight ratio with Paulownia elongata flower is 2:100, it is then stirred by ultrasonic 2 hours, the temperature of solution is controlled in ultrasonic wave dispersion process
It it is 55 DEG C, the frequency of ultrasonic wave is 40KHz, is put into electric drying oven with forced convection and removes most of moisture, electric heating forced air drying
Temperature is 75 DEG C, takes out, is cooled to room temperature when moisture evaporation to solution is at viscous pasty state, then dry with low temperature vacuum drier
Dry, at 43 DEG C, the pure green broad-spectrum antiseptic feed addictive of powdery is made in vacuum degree 1000Pa.
Embodiment five:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(A)Prepare graphene oxide suspension;
The graphene oxide prepared with oxidation-reduction method is added in pure water, disperses oxidation to be made in 12 hours under ul-trasonic irradiation
Graphene suspension, the temperature of control solution is 55 DEG C in ultrasonic wave dispersion process, and the frequency of ultrasonic wave is 40KHz, aoxidizes stone
The weight ratio of black alkene and pure water is 1.2:1000.
Step(B)It prepares Paulownia elongata and spends extracting solution;
Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, 45 mesh sieve are crossed with spin vibration sieve, with pure water solvent, Lan Kaopao
The weight ratio of paulownia and pure water is 1:15, ultrasonic wave stirs 2 hours, stands 8 hours, then ultrasonic wave stirs 2 hours, then stands 8
Hour, the frequency of then ultrasonic extraction 1 hour at 85 DEG C, ultrasonic wave is 40KHz, then again by Paulownia elongata flower and pure water
Ratio is 1:15, ultrasonic wave stirs 2 hours, stands 8 hours, then ultrasonic wave stirs 2 hours, then stands 8 hours, then at 85 DEG C
Lower ultrasonic extraction 1 hour, the step of be repeated twice, extracting solution three times is mixed be made Paulownia elongata flower extracting solution.
Step(C)Graphene oxide suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure of carrier
Green broad spectrum antiseptic feed additive.Graphene oxide suspension is added in Paulownia elongata flower extracting solution, graphene oxide
Weight ratio with Paulownia elongata flower is 2.3:100, it is then stirred by ultrasonic 2 hours, the temperature of solution is controlled in ultrasonic wave dispersion process
Degree is 65 DEG C, and the frequency of ultrasonic wave is 40KHz, is put into electric drying oven with forced convection and removes most of moisture, electric heating forced air drying
Temperature be 78 DEG C, take out, be cooled to room temperature when moisture evaporation to solution is at viscous pasty state, then is dry with low temperature vacuum drier
Dry, at 50 DEG C, the pure green broad-spectrum antiseptic feed addictive of powdery is made in vacuum degree 1000Pa.
Embodiment six:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(A)Prepare graphene oxide suspension;
The graphene oxide prepared with oxidation-reduction method is added in 75% ethanol water, small with dispersion 12 under ul-trasonic irradiation
When be made graphene oxide suspension, the temperature of control solution is 45 DEG C in ultrasonic wave dispersion process, and the frequency of ultrasonic wave is
The weight ratio of 40KHz, graphene oxide and 75% ethanol water is 3.6:1000.
Step(B)It prepares Paulownia elongata and spends extracting solution;
Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, 45 mesh sieve is crossed with spin vibration sieve, is with 75% ethanol water
The weight ratio of solvent, Paulownia elongata flower and 75% ethanol water is 1:25, ultrasonic wave stirs 1 hour, stands 5 hours, then ultrasound
Wave stirs 1 hour, then stands 5 hours, then ultrasonic extraction 1 hour at 65 DEG C, and the frequency of ultrasonic wave is 40KHz, then again
Ratio by Paulownia elongata flower and 75% ethanol water is 1:25, ultrasonic wave stirs 1 hour, stands 5 hours, then ultrasonic wave stirs
It mixes 1 hour, then stands 5 hours, be then repeated twice the step of ultrasonic extraction 1 hour at 65 DEG C, extracting solution three times is mixed
It is combined and Paulownia elongata flower extracting solution is made.
Step(C)Graphene oxide suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure of carrier
Green broad spectrum antiseptic feed additive.Graphene oxide suspension is added in Paulownia elongata flower extracting solution, graphene oxide
Weight ratio with Paulownia elongata flower is 3.4:100, it is then stirred by ultrasonic 2 hours, the temperature of solution is controlled in ultrasonic wave dispersion process
Degree is 65 DEG C, and the frequency of ultrasonic wave is 40KHz, is put into electric drying oven with forced convection and removes most of moisture, electric heating forced air drying
Temperature be 70 DEG C, take out, be cooled to room temperature when moisture evaporation to solution is at viscous pasty state, then is dry with low temperature vacuum drier
Dry, at 51 DEG C, the pure green broad-spectrum antiseptic feed addictive of powdery is made in vacuum degree 10000Pa.
Embodiment seven:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(A)Prepare graphene suspension;
The graphene prepared with oxidation-reduction method is added in pure water, is hanged with disperse to be made for 12 hours graphene under ul-trasonic irradiation
Supernatant liquid, the temperature of control solution is 45 DEG C in ultrasonic wave dispersion process, and the frequency of ultrasonic wave is 40KHz, graphene oxide with it is pure
The weight ratio of water is 3.2:1000.
Step(B)It prepares Paulownia elongata and spends extracting solution;
Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, 45 mesh sieve is crossed with spin vibration sieve, is solvent, Lankao with pure water
The weight ratio of fortune paulownia flower and pure water is 1:23, ultrasonic wave stirs 1 hour, stands 5 hours, then ultrasonic wave stirs 1 hour, then stands
5 hours, the frequency of then ultrasonic extraction 1 hour at 70 DEG C, ultrasonic wave was 40KHz, then again by Paulownia elongata flower and pure water
Ratio be 1:23, ultrasonic wave stirs 1 hour, stands 5 hours, then ultrasonic wave stirs 1 hour, then stands 5 hours, then 70
The step of ultrasonic extraction 1 hour, is repeated twice at DEG C, extracting solution three times is mixed, Paulownia elongata flower extracting solution is made.
Step(C)Graphene suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure green of carrier
Broad-spectrum antiseptic feed addictive.Graphene suspension is added in Paulownia elongata flower extracting solution, graphene is spent with Paulownia elongata
Weight ratio be 2.9:100, it is then stirred by ultrasonic 2 hours, the temperature of control solution is 53 DEG C in ultrasonic wave dispersion process, ultrasound
The frequency of wave is 40KHz, is put into electric drying oven with forced convection and removes most of moisture, and the temperature of electric heating forced air drying is 69 DEG C,
It takes out, is cooled to room temperature when moisture evaporation to solution is at viscous pasty state, then dried with low temperature vacuum drier, at 44 DEG C,
Vacuum degree is 1000Pa, and the pure green broad-spectrum antiseptic feed addictive of powdery is made.
Embodiment eight:
A kind of preparation method of pure green broad-spectrum antiseptic feed addictive:Include the following steps:
Step(A)Prepare graphene suspension;
The graphene prepared with oxidation-reduction method is added in 75% ethanol water, is made with disperseing 12 hours under ul-trasonic irradiation
At graphene suspension, the temperature of control solution is 45 DEG C in ultrasonic wave dispersion process, and the frequency of ultrasonic wave is 40KHz, graphite
The weight ratio of alkene and 75% ethanol water is 3.7:1000.
Step(B)It prepares Paulownia elongata and spends extracting solution;
Paulownia elongata flower dry product Study on Supermicro-pulverization of Traditional Chinese Drugs machine is crushed, 45 mesh sieve is crossed with spin vibration sieve, is with 75% ethanol water
The weight ratio of solvent, Paulownia elongata flower and 75% ethanol water is 1:18, ultrasonic wave stirs 1 hour, stands 6 hours, then ultrasound
Wave stirs 1 hour, then stands 6 hours, then ultrasonic extraction 1 hour at 77 DEG C, and the frequency of ultrasonic wave is 40KHz, then again
Ratio by Paulownia elongata flower and 75% ethanol water is 1:18, ultrasonic wave stirs 1 hour, stands 6 hours, then ultrasonic wave stirs
It mixes 1 hour, then stands 6 hours, be then repeated twice the step of ultrasonic extraction 1 hour at 77 DEG C, extracting solution three times is mixed
It is combined and Paulownia elongata flower extracting solution is made.
Step(C)Graphene oxide suspension is added in Paulownia elongata flower extracting solution and is prepared using graphene as the pure of carrier
Green broad spectrum antiseptic feed additive.Graphene suspension is added in Paulownia elongata flower extracting solution, graphene and Lan Kaopao
The weight ratio of paulownia is 2.7:100, then it is stirred by ultrasonic 2 hours, the temperature of control solution is 60 DEG C in ultrasonic wave dispersion process,
The frequency of ultrasonic wave is 40KHz, is put into electric drying oven with forced convection and removes most of moisture, and the temperature of electric heating forced air drying is 78
DEG C, it takes out, is cooled to room temperature when moisture evaporation to solution is at viscous pasty state, then dried with low temperature vacuum drier, at 44 DEG C
Under, the pure green broad-spectrum antiseptic feed addictive of powdery is made in vacuum degree 1000Pa.
There is good absorption property, graphene surface can adsorb a large amount of substance for graphene or graphene oxide, very
The pharmaceutical carrier for being suitable as broad-spectrum antiseptic.Graphene or graphene oxide granularity itself prepared by oxidation-reduction method just compares
Small, usually between several microns to 100 microns, therefore, graphene or graphene oxide prepared by this method does not need special place
Reason can be used as the carrier of drug, and drug can be made to pass through blood vessel in animal body and arrived in animal body everywhere, play
The purpose of prevention.
Paulownia elongata extract prepared by different embodiments is to Escherichia coli, pseudomonas aeruginosa, salmonella, full yellow
Staphylococcus, Candida albicans MIC(Minimum Inhibitory Concentration, minimal inhibitory concentration)Value difference
For 10.12-10.76,1.28-1.41,5.03-5.98,0.63-0.69,10.25-11.57mg/ml, to Aspergillus niger fungus, rice
Aspergillus fungal, Penicillium citrinum fungi, the malicious fungi of green wood, bread mold fungi bacteriostasis rate be respectively 65.4%-67.2%, 42.7%-
43.1%、23.6%-25.1%、75.2%-76.8%、76.1%-77.6%。
Paulownia elongata is spent as a kind of economic forest plant of widely distributed plantation, and raw material sources are extensive, and due to being to plant
Object, remaining time is short in livestock body, can completely decompose within a couple of days or be excreted by digestion, not in livestock body
Enrichment is retained, not only eliminates artificial synthesized antibiotic concentration height, residual life is long, is still remained very to when slaughtering in livestock
It is more, the problem of influencing health of people, but also make livestock during stable breeding, and it is few sick, reduce the production at large-scale cultivation family
Cost
Finally illustrate, the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, ordinary skill
Other modifications or equivalent replacement that personnel make technical scheme of the present invention, without departing from the essence of technical solution of the present invention
God and range, are intended to be within the scope of the claims of the invention.
Claims (5)
1. a kind of preparation method of pure green broad-spectrum antiseptic feed addictive:It is characterized by comprising following steps:
Step(1):Prepare graphene suspension;The graphene or graphene oxide prepared with oxidation-reduction method, is added to pure water
Or in ethanol water, with disperseing graphene suspension or graphene oxide suspension to be made in 1-24 hours under ul-trasonic irradiation,
Graphene or graphene oxide and the weight ratio of pure water or ethanol water are 1-4:1000;
Step(2):It prepares Paulownia elongata and spends extracting solution;Paulownia elongata flower dry product is crushed, sieving, with pure water or 50% ethyl alcohol or
75% ethyl alcohol is solvent, and ultrasonic wave stirring, standing, ultrasonic wave is stirred, stood again again, then in the lower temperature ultrasound less than 100 DEG C
Wave extracts 1 hour, then will be solvent with pure water or 50% ethyl alcohol or 75% ethyl alcohol or 90% ethyl alcohol again, and ultrasonic wave stirs, is quiet
Set, again ultrasonic wave stirring, stand again, be then repeated twice in the step of lower ultrasonic wave extraction 1 hour less than 100 DEG C, by three
Secondary extracting solution, which mixes, is made Paulownia elongata flower extracting solution;
Step(3):Graphene suspension or graphene oxide suspension are added in Paulownia elongata flower extracting solution and prepared with graphite
Alkene is the pure green feed addictive of carrier;Graphene suspension or graphene oxide suspension are added to Paulownia elongata flower to carry
It takes in liquid, the weight ratio of wherein graphene and Paulownia elongata flower dried flower is 2-8:100, then it is stirred by ultrasonic 1-24 hours, it is dry
Case removes most of moisture, is dried when solution is in viscous pasty state, then with low temperature vacuum drier, the pure green that powdery is made is wide
Compose antiseptic feed additive.
2. a kind of preparation method of pure green broad-spectrum antiseptic feed addictive according to claim 1, it is characterised in that:Institute
State step(1)With(3)The temperature that solution is controlled in middle ultrasonic wave dispersion process is 20-60 DEG C, and the frequency of ultrasonic wave is 40KHz,
The step(2)The frequency of middle ultrasonic wave is 40KHz.
3. a kind of preparation method of pure green broad-spectrum antiseptic feed addictive according to claim 1, it is characterised in that:Institute
State step(2)Middle Paulownia elongata flower pulverizer is Study on Supermicro-pulverization of Traditional Chinese Drugs machine, and sieving is sieved with spin vibration sieve, and sieve minimum mesh number is 40
Mesh.
4. a kind of preparation method of pure green broad-spectrum antiseptic feed addictive according to claim 1, it is characterised in that:Institute
State step(3)In drying box be electric drying oven with forced convection, drying temperature when dry is 60-80 DEG C.
5. a kind of preparation method of pure green broad-spectrum antiseptic feed addictive according to claim 1, it is characterised in that:Institute
State step(3)In low temperature vacuum drier drying temperature be 25-50 DEG C, vacuum degree 1000-10000Pa.
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