CN107498067B - The method that Bao internal organ degradation product green quickly prepares nano silver colloidal sol - Google Patents
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Abstract
The present invention quickly prepares nano silver colloidal sol using Bao internal organ degradation product green, belongs to technical field of nano-processing.Preparation method are as follows: in aqueous phase system, by after Bao internal organ degradation product and silver nitrate mixed dissolution, using microwave heating, hot bath, oil bath or ultraviolet radiation method, prepare be uniformly dispersed, the nano silver colloidal sol that stability is good.The preparation method is simple, safe, quick, provides a kind of green, environmentally friendly, quick method for the preparation of nano silver colloidal sol.Bao internal organ belong to the by-product of Bao processing industry, are reproducible living resources, and the present invention provides new method for the synthesis of nano silver colloidal sol, while also achieving the higher value application of Bao internal organ.
Description
Technical field
The invention belongs to field of nanometer technology, and in particular to a kind of Bao internal organ degradation product green is quick to prepare nano silver colloidal sol
Method.
Background technique
Nano silver colloidal sol because have the characteristics that efficiently, antibacterial is wide, does not produce drug resistance, and in clothes, food, coating, makeup
It is used widely in the fields such as product, Medical Devices, plastics and textile.The relevant technologies are using chemistry such as hydrazine hydrate, sodium borohydrides
Reagent prepares nano silver colloidal sol as reducing agent and nitric acid silver reaction.But the chemical reagent such as hydrazine hydrate, sodium borohydride have certain
Bio-toxicity, residue not only brings a negative impact to environment, but also influences the biological safety of nano silver colloidal sol, this is big
It is limited greatly in the application in the fields such as medicine and biology.
For the bio-toxicity for overcoming chemical reducing agent, the relevant technologies prepare nanometer as reducing agent and stabilizer using polysaccharide
Silver sol.Though these technologies overcome the chemical residual problem of chemical reducing agent, polysaccharide is directlyed adopt as raw material, is produced into
This height, and can not solve the problems, such as the easy aggregate and precipitate of nano silver colloidal sol.
In conclusion nano silver colloidal sol in the related technology is because of high production cost, chemical residual problem, can not medicine,
The fields such as biology and cosmetics are widely used.Therefore, a kind of biological safety height and lower-cost nano silver colloidal sol are developed,
As current urgent problem to be solved.
Bao internal organ are the principal by product of Bao Jiagong, and yield is high, are a kind of important renewable biomass resources.In Bao
It is dirty based on protein, polysaccharide, inorganic impurity content is less.It, can not be as food since Bao internal organ are not belonging to edible resource
Product raw material carries out deep processing.Currently, most of Bao internal organ are as waste, processing and utilization rate is extremely low, this not only causes resource
Waste, and easily cause environmental pollution.Currently, it is molten to prepare nano silver using Bao internal organ degradation product as reducing agent and stabilizer
The research of glue has not been reported.
The present invention provides a kind of methods that Bao internal organ degradation product green quickly prepares nano silver colloidal sol.For the first time using in Bao
Dirty degradation product is as reducing agent and stabilizer, in aqueous environment, utilizes microwave radiation, hot bath, oil bath heating or ultraviolet
The method of beta radiation prepares nano silver colloidal sol.The present invention can not only efficiently utilize Bao internal organ degradation product, and not need to add
Add any chemical reducing agent, stabilizer and dispersing agent, preparation process complies fully with green chemical concept.Therefore, system of the present invention
Standby nano silver colloidal sol medical treatment, biology, in terms of have great application prospect.The present invention is not only nano silver colloidal sol
Preparation technological guidance is provided, and new thinking is provided for the higher value application of Bao internal organ.
Summary of the invention
The invention discloses the methods that Bao internal organ degradation product green quickly prepares nano silver colloidal sol.
The present invention is realized especially by following technical scheme:
In aqueous phase system, Bao internal organ degradation product and silver nitrate mixed solution are placed in microwave reactor, oil bath or water-bath
Carry out redox reaction in heater or UV reactive device, prepare be uniformly dispersed, the nano silver colloidal sol that stability is good.
Preferably, the Bao internal organ degradation product includes at least following one: Bao internal organ acid hydrolysis products, Bao internal organ basic hydrolysis
Product, Bao visceral protein enzymic hydrolysates, Bao internal organ polysaccharide enzymic hydrolysates, hydrogen peroxide degradation Bao internal organ product, gamma-radiation drop
Solve Bao internal organ product, ultrasonic degradation Bao internal organ product, nano metal photocatalytic degradation Bao internal organ product.
Preferably, the Bao visceral protein enzymic hydrolysates refer to product of the Bao internal organ after protease hydrolytic.Wherein, egg
White enzyme is selected from one or more of following protease mixture: trypsase, papain, neutral proteinase, alkalinity
Protease, flavor protease.
Preferably, the Bao internal organ polysaccharide enzymic hydrolysates refer to product of the Bao internal organ after polysaccharide enzyme hydrolysis.Wherein, more
Carbohydrase is selected from one or more of following polysaccharase mixture: inscribe β-(1,4)-seminase, alpha-amylase, β-starch
Enzyme, grape enzyme amylase, isoamylase, circumscribed 1,4 beta-glucanase, Endo-β-glucanase and beta-glucosidase, xylan
Enzyme.
Preferably, the nano metal photocatalytic degradation Bao internal organ product, refers to Bao internal organ through nano metal photocatalysis
Product after degradation.Wherein, nano metal is selected from one or more of following nano metal mixture: nano-TiO2, receive
Rice ZnO, nano SnO2, nanometer WO3, nano-tube/CdS, nanometer Fe2O3, nanometer Bi2O3, nanometer Ag.
Preferably, the Bao internal organ degradation product includes: powdered Bao internal organ degradation product, and is dissolved in water, You Jirong
Bao internal organ degradation product solution in agent.
Preferably, above-mentioned Bao internal organ degradation product is specific the preparation method comprises the following steps: Bao internal organ are crushed after drying, 40 meshes excessively
As enzymatic hydrolysis raw material, protease is then added in aqueous phase system and carries out single or multiple heat preservation enzymatic hydrolysis, enzymolysis liquid is through being centrifuged
Afterwards, waste takes supernatant dry to get Bao internal organ degradation product.
Preferably, above-mentioned Bao internal organ degradation product prepares nano silver colloidal sol specific step is as follows:
1, under agitation, Bao internal organ degradation product and silver nitrate crystal are gradually added in deionized water, are allowed to complete
Dissolution, the concentration of Bao internal organ degradation product is 0.01mg/mL~100mg/mL in solution after dissolution, the concentration of silver nitrate is 1.0 ×
10-5Mol/L~10.0mol/L.
2, above-mentioned solution is subjected to redox reaction by one of following three kinds of modes:
(1) mode one: above-mentioned solution is placed in microwave reactor, and adjusting microwave power is 700~1000W, microwave temperature
Degree is 60~100 DEG C, and the nano silver colloidal sol of stably dispersing can be obtained after 10~70min of microwave reaction.
(2) mode two: above-mentioned solution is placed in heat in oil bath or water-bath and is reacted, control reaction temperature is 35 DEG C~200
DEG C, after heating reaction 5min~2400min, the nano silver colloidal sol of stably dispersing can be obtained, reaction is being protected from light lower progress.
(3) mode three: above-mentioned solution being placed in ultraviolet light chemical reactor and carries out radioreaction, and radiating light source wavelength is
190nm~400nm, radiation luminous intensity are 1.65 × 1015~1.98 × 1018photons/sec/cm3, radiation 5min~
After 2400min, the nano silver colloidal sol of stably dispersing can be obtained.
In the above method, reaction is carried out in aqueous phase system, do not need to add in reaction process any chemical reducing agent,
Stabilizer and dispersing agent.
In the above method, the nano silver partial size of preparation is 10~40nm, and size is uniform, form is regular.
The nano silver colloidal sol of above method preparation can also again stable, equably divide after high speed long-time centrifugation
It dissipates in aqueous solution, the centrifugal condition is 15000~18000r/min, 30~40min.
Compared with prior art, the invention has the following advantages that
(1) present invention uses Bao internal organ degradation product as reducing agent and stabilizer and prepares nano silver colloidal sol, is not required to add other
Chemical reducing agent, stabilizer and dispersing agent, obtained nano silver colloidal sol have excellent dispersion stabilization and high biology
Safety has huge application prospect in the fields such as medical treatment, biology, food.
(2) present invention improves the utility value of Bao internal organ, no using Bao internal organ degradation product as reducing agent and stabilizer
The synthesis of only nano silver colloidal sol provides new thinking, and also the deep processing and utilization for processing of aquatic products waste opens new canal
Road.
(3) nano silver colloidal sol that the present invention prepares, after centrifugation, still can uniformly and stably be scattered in aqueous solution,
Nano metal is efficiently solved to be easy to reunite, be difficult to the problems such as dispersing.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
The UV-vis spectroscopy spectrum of nano silver colloidal sol prepared by Fig. 1 embodiment of the present invention 1, absorption peak 420nm,
It is consistent with the reported values of document.
The transmission electron microscope picture of nano silver colloidal sol prepared by Fig. 2 embodiment of the present invention 1, as shown, nano-Ag particles are high
Molecule package, and its partial size is less than 40nm.
Specific embodiment
Below in conjunction with embodiment, the present invention will be described in detail.It should be noted that in the absence of conflict, this Shen
Please in embodiment and embodiment in feature can be combined with each other.
Bao internal organ degradation product used in following embodiment is using a kind of following production that degradation preparation method obtains
Object, in other embodiments, the mixture for the catabolite that can also be obtained with different preparation methods.
Proteasome degradation Bao internal organ preparation method: Bao internal organ are dry, crushing crosses 40 meshes, prepares Bao internal organ powder.It will
50g Bao internal organ powder is dissolved in the deionized water of 2L, and 625g alkali protease is added, and is placed in 50 DEG C of water-baths and heats 12h.So
The enzyme deactivation 20min in 95 DEG C of water-baths afterwards is centrifuged (4000r/min, 20min) after cooling, takes supernatant.It is added in supernatant
6g flavor protease, 50 DEG C of heating water bath 12h, then the enzyme deactivation 20min in 95 DEG C of water-baths, is centrifuged (4000r/ after cooling
Min, 20min), take supernatant dry to get Bao internal organ degradation product.
Sour water solution Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao internal organ powder.By 100g Bao
Internal organ powder is dissolved in the deionized water of 4L, and sulfuric acid, nitric acid or hydrochloric acid is added, and adjusting pH value of solution is pH3.0, is placed in 70 DEG C of water-baths
Upper heating 12h.After cooling, adjusting pH is pH7.0, is desalted with hyperfiltration process, and ultrafiltrate is dry to get the degradation of Bao internal organ
Object.
Basic hydrolysis Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao internal organ powder.It will be in 80g Bao
Dirty powder is dissolved in the deionized water of 4L, and NaOH is added, and adjusting pH value of solution is pH10.0, is placed in 65 DEG C of water-baths and heats 12h.To
After cooling, adjusting pH is pH7.0, is desalted with hyperfiltration process, and ultrafiltrate is dry to get Bao internal organ degradation product.
Polysaccharide enzyme hydrolysis Bao internal organ method: Bao internal organ are dry, crushing crosses 40 meshes, prepares Bao internal organ powder.By 50g
Bao internal organ powder is dissolved in the deionized water of 2L, and 10g beta-glucosidase is added, and is placed in 60 DEG C of water-baths and heats 12h.Then
The enzyme deactivation 30min in 95 DEG C of water-baths is centrifuged (5000r/min, 30min) after cooling, takes supernatant dry to get Bao internal organ drop
Solve object.
Hydrogen peroxide degradation Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao internal organ powder.By 60g
Bao internal organ powder is dissolved in the deionized water of 4L, and hydrogen peroxide is added, makes hydrogen peroxide concentration 2.0mol/L, is placed in 40 DEG C of water-baths
Heating is for 24 hours.After cooling, adjusting pH is pH7.0, and hydrolyzate is dry to get Bao internal organ degradation product.
Gamma-radiation degradation Bao internal organ method: Bao internal organ are dry, crushing crosses 300 meshes, prepares Bao internal organ powder.It will
100g Bao internal organ powder is encapsulated in polyethylene plastic bag, is used60Co is irradiated at normal temperature, and dosage 10-100kGy, treated
Sample is in 4 DEG C of freezer storages to get Bao internal organ degradation product.
Ultrasonic degradation Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao internal organ powder.It will
100g Bao internal organ powder is dissolved in the deionized water of 4L, and solution is placed in sonicator processing, ultrasonic amplitude 80%, ultrasound
Frequency 20kHz, ultrasound intensity 50W/cm2, after handling 120min, solution is dry to get Bao internal organ degradation product.
Nano metal photocatalytic degradation Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao visceral meal
End.100g Bao internal organ powder is dissolved in the deionized water of 4L, 20g nano zine oxide is added, is placed in light reaction generator, spoke
Penetrating optical source wavelength is 280nm, and radiation luminous intensity is 1.98 × 1019photons/sec/cm3, radiate 1000min.It then will reaction
Liquid is centrifuged (10000r/min, 30min), takes supernatant dry to get Bao internal organ degradation product.
Embodiment 1
Under agitation, Bao internal organ degradation product (Bao visceral protein enzyme degradation product) and silver nitrate crystal are gradually added
It in ionized water, is allowed to be completely dissolved, the concentration of Bao internal organ degradation product is 1mg/mL in solution after dissolution, and the concentration of silver nitrate is
1.0×10-2mol/L.Above-mentioned solution is placed in microwave reactor, adjusting microwave power is 700W, and microwave temperature is 60 DEG C, micro-
To get the nano silver colloidal sol for arriving stably dispersing after wave reaction 30min.
Embodiment 2
Under agitation, Bao internal organ degradation product (Bao internal organ acid hydrolysate) and silver nitrate crystal are gradually added deionization
It in water, is allowed to be completely dissolved, the concentration of Bao internal organ degradation product is 0.5mg/mL in solution after dissolution, and the concentration of silver nitrate is 5.0
×10-2mol/L.Above-mentioned solution is placed in microwave reactor, adjusting microwave power is 1000W, and microwave temperature is 70 DEG C, microwave
To get the nano silver colloidal sol for arriving stably dispersing after reaction 10min.
Embodiment 3
Under agitation, Bao internal organ degradation product (Bao internal organ basic hydrolysis object) and silver nitrate crystal are gradually added deionization
It in water, is allowed to be completely dissolved, the concentration of Bao internal organ degradation product is 0.25mg/mL in solution after dissolution, and the concentration of silver nitrate is 5.0
×10-1mol/L.Above-mentioned solution is placed in 60 DEG C of water-baths after heating 120min to get the nano silver colloidal sol for arriving stably dispersing.
Embodiment 4
Under agitation, Bao internal organ degradation product (Bao internal organ polysaccharide protease hydrolysate) and silver nitrate crystal are gradually added
It in ionized water, is allowed to be completely dissolved, the concentration of Bao internal organ degradation product is 0.45mg/mL, the concentration of silver nitrate in solution after dissolution
For 1.0mol/L.Above-mentioned solution is placed in 90 DEG C of water-baths after heating 60min to get the nano silver colloidal sol for arriving stably dispersing.
Embodiment 5
Under agitation, Bao internal organ degradation product (Bao internal organ hydrogen peroxide degradation product) and silver nitrate crystal are gradually added
It in ionized water, is allowed to be completely dissolved, the concentration of Bao internal organ degradation product is 0.75mg/mL, the concentration of silver nitrate in solution after dissolution
It is 1.0 × 10-1mol/L.Above-mentioned solution is placed in ultraviolet light chemical reactor and carries out radioreaction, radiating light source wavelength is
280nm, radiation luminous intensity are 1.98 × 1017photons/sec/cm3, radiate 1000min after to get arrive stably dispersing nanometer
Silver sol.
Embodiment 6
Under agitation, Bao internal organ degradation product (Bao internal organ gamma-radiation degradation product) and silver nitrate crystal are gradually added
It in deionized water, is allowed to be completely dissolved, the concentration of Bao internal organ degradation product is 2mg/mL in solution after dissolution, and the concentration of silver nitrate is
8.0×10-2mol/L.Above-mentioned solution is placed in ultraviolet light chemical reactor and carries out radioreaction, radiating light source wavelength is
350nm, radiation luminous intensity are 2.30 × 1016photons/sec/cm3, radiate 600min after to get arrive stably dispersing nanometer
Silver sol.
It should be noted that the parameter that the preparation in above-described embodiment uses is merely to illustrate that, it is not used as to this
The limitation of application to those skilled in the art can according to actual needs, flexible choice preparation parameter.
Bao internal organ degradation product of the present invention can be using one of all Bao internal organ catabolites in the related technology
And its mixture, the present invention specified by Bao internal organ degradation product be only intended to enumerate, be not the type to Bao internal organ degradation product
It is limited.
In addition to the Bao internal organ degradation product specified by the present invention, it can also be used for Bao internal organ degradation product prepared by other methods
The present invention prepares nano silver colloidal sol.Core of the invention is exactly the reduction by Bao internal organ degradation product to silver ion, and
To the complexing coating function of nano-Ag particles, received by the way that Bao internal organ degradation product is carried out redox reaction with silver nitrate to prepare
Rice silver sol, using following Bao internal organ degradation product as example in specific embodiment and more specific technical solution: Bao internal organ
Acid hydrolysis products, Bao internal organ basic hydrolysis product, Bao visceral protein enzymic hydrolysates, Bao internal organ polysaccharide enzymic hydrolysates, hydrogen peroxide
Degradation Bao internal organ product, gamma-radiation degradation Bao internal organ product, ultrasonic degradation Bao internal organ product, nano metal photocatalytic degradation
Bao internal organ product.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Since the present invention uses the characteristic of Bao internal organ degradation product, the Bao internal organ degradation product do not enumerated of the present invention can also be with
It is used to prepare nano silver colloidal sol.Although the present invention has listed the type of some Bao internal organ degradation products, structure according to the present invention
Thinking other Bao internal organ degradation products can also be used for nano silver colloidal sol, we can not all enumerate herein.
Claims (1)
1. the method that Bao internal organ degradation product green quickly prepares nano silver colloidal sol, which is characterized in that, will be in Bao in aqueous phase system
The mixed solution of dirty degradation product and silver nitrate is placed in microwave reactor, oil bath or water-bath heater and carries out redox reaction,
Prepare be uniformly dispersed, the nano silver colloidal sol that stability is good；
Step includes:
1) under agitation, Bao internal organ degradation product and silver nitrate crystal are gradually added in deionized water, are allowed to be completely dissolved,
The concentration of Bao internal organ degradation product is the mg/mL of 0.01 mg/mL ~ 100 in solution after dissolution, and the concentration of silver nitrate is 1.0 × 10-5
mol/L ~ 10.0mol/L；
2) above-mentioned solution is subjected to redox reaction by one of following two mode:
(1) mode one: above-mentioned solution is placed in microwave reactor, and adjusting microwave power is 700 ~ 1000 W, and microwave temperature is
60 ~ 100 DEG C, the nano silver colloidal sol of stably dispersing can be obtained after 10 ~ 70 min of microwave reaction；
(2) mode two: above-mentioned solution being placed in heat in oil bath or water-bath and is reacted, and control reaction temperature is 35 DEG C ~ 200 DEG C, is added
After thermal response 5 min ~ 2400 min, the nano silver colloidal sol of stably dispersing can be obtained；
Wherein, used Bao internal organ degradation product is the product obtained using at least one of following degradation preparation method:
Proteasome degradation Bao internal organ preparation method: Bao internal organ are dry, crushing crosses 40 meshes, prepares Bao internal organ powder；By 50g
Bao internal organ powder is dissolved in the deionized water of 2L, and 625g alkali protease is added, and is placed in 50 DEG C of water-baths and heats 12h；Then
The enzyme deactivation 20min in 95 DEG C of water-baths, is centrifuged after cooling, and 4000r/min, 20min take supernatant；6g is added in supernatant
Flavor protease, 50 DEG C of heating water bath 12h, then the enzyme deactivation 20min in 95 DEG C of water-baths, is centrifuged, 4000r/min after cooling,
20min takes supernatant dry to get Bao internal organ degradation product；
Sour water solution Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao internal organ powder；By 100g Bao internal organ
Powder is dissolved in the deionized water of 4L, and sulfuric acid, nitric acid or hydrochloric acid is added, and adjusting pH value of solution is pH3.0, is placed in 70 DEG C of water-baths and adds
Hot 12h；After cooling, adjusting pH is pH7.0, is desalted with hyperfiltration process, and ultrafiltrate is dry to get Bao internal organ degradation product；
Basic hydrolysis Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao internal organ powder；By 80g Bao visceral meal
End is dissolved in the deionized water of 4L, and NaOH is added, and adjusting pH value of solution is pH10.0, is placed in 65 DEG C of water-baths and heats 12h；It is to be cooled
Afterwards, adjusting pH is pH7.0, is desalted with hyperfiltration process, and ultrafiltrate is dry to get Bao internal organ degradation product；
Polysaccharide enzyme hydrolysis Bao internal organ method: Bao internal organ are dry, crushing crosses 40 meshes, prepares Bao internal organ powder；It will be in 50g Bao
Dirty powder is dissolved in the deionized water of 2L, and 10g beta-glucosidase is added, and is placed in 60 DEG C of water-baths and heats 12h；Then 95
Enzyme deactivation 30min in DEG C water-bath, is centrifuged, 5000r/min, 30min after cooling, takes supernatant dry to get Bao internal organ degradation product；
Hydrogen peroxide degradation Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao internal organ powder；It will be in 60g Bao
Dirty powder is dissolved in the deionized water of 4L, and hydrogen peroxide is added, makes 2.0 mol/L of hydrogen peroxide concentration, is placed in 40 DEG C of water-baths and adds
Heat is for 24 hours；After cooling, adjusting pH is pH7.0, and hydrolyzate is dry to get Bao internal organ degradation product；
Gamma-radiation degradation Bao internal organ method: Bao internal organ are dry, crushing crosses 300 meshes, prepares Bao internal organ powder；By 100g Bao
Internal organ powder is encapsulated in polyethylene plastic bag, is irradiated at normal temperature with 60Co, and dosage is 10-100 kGy, treated sample
In 4 DEG C of freezer storages to get Bao internal organ degradation product；
Ultrasonic degradation Bao internal organ method: Bao internal organ are dry, crushing sieves with 100 mesh sieve, prepares Bao internal organ powder；By 100g Bao
Internal organ powder is dissolved in the deionized water of 4L, and solution is placed in sonicator processing, ultrasonic amplitude 80%, supersonic frequency 20
KHz, 50 W/cm of ultrasound intensity2, after handling 120 min, solution is dry to get Bao internal organ degradation product.
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| CN102898538B (en) * | 2012-11-06 | 2014-08-27 | 中国海洋大学 | Abalone viscera acidic polysaccharose and health-care product containing abalone viscera acidic polysaccharose and application of abalone viscera acidic polysaccharose |
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