CN104551010A - Method for preparing water-soluble nano-silver by using short amylose as template - Google Patents
Method for preparing water-soluble nano-silver by using short amylose as template Download PDFInfo
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- CN104551010A CN104551010A CN201510024880.0A CN201510024880A CN104551010A CN 104551010 A CN104551010 A CN 104551010A CN 201510024880 A CN201510024880 A CN 201510024880A CN 104551010 A CN104551010 A CN 104551010A
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Abstract
The invention discloses a method for preparing water-soluble nano-silver by using short amylose as a template. The method comprises the steps that raw material processing is conducted; gelatinization is conducted; enzymolysis is conducted; low-speed centrifugation is conducted; the prepared short amylose is diluted, silver nitrate dissolves in ultrapure water, the silver nitrate and the ultrapure water are stirred to be fully mixed, and then the silver nitrate solution is added to the diluted short amylose solution to be mixed; sodium metaborate dissolves in ultrapure water, the sodium metaborate and the ultrapure water are stirred to be fully mixed, the mixture is dropwise added to the mixed solution obtained in the fifth step to be mixed, the formed solution is placed away from light, and processed in a freeze-drying mode to obtain the water-soluble nano-silver. The particle size of the water-soluble nano-silver prepared through the method ranges from 2nm to 5nm, distribution is uniform, the water-soluble nano-silver can rapidly dissolve in water, the reaction condition is moderate, the preparation process is safe and environmentally friendly, the equipment requirement is low, the technology is simple, operation is easy and convenient, the reaction time is short, the efficiency is high, and the method is suitable for large-scale production; the product performance is good, the preparation cost is low, energy consumption is low, no hazardous waste is generated, and the production requirements for green production, environmental protection and energy saving are met.
Description
Technical field
The present invention relates to a kind of with the method for short amylose for Template preparation water-soluble nano silver, belong to field of nanometer technology.
Background technology
Nano Silver, as a kind of emerging functional material, is widely used in antistatic material, catalysis material, battery electrode material, low temperature superconducting material, conductive paste material and biological sensing material.In addition, nano silver particles has very strong broad-spectrum bactericidal capacity, good bio-compatibility, is difficult to produce the advantages such as drug resistance, also in an increasingly wide range of applications in fields such as medical and health.Therefore the preparation of Nano Silver is subject to extensive concern, the method of bibliographical information is a lot, has summed up: chemical reduction method, biological reducing method, microemulsion method, gamma Rays method, magnetron sputtering method, photoreduction met hod, laser ablation, electrochemical process, seed mediator method, chemical vapour deposition technique, supercritical fluid method etc.Wherein chemical reduction method is simple to operate, cost is lower, is convenient to large-scale production, is the maximum method of research report.
But in prior art with the short amylose particle of biological enzymolysis for template, prepare that particle diameter is little, the technology of Nano Silver that can be water-soluble rapidly have not been reported, and reducing agent disclosed in prior art is less owing to producing nucleus, a large amount of silver ions grows on minority nucleus, cause diameter larger, grow uneven, aqueous stability reduces.
Summary of the invention
For solving problems of the prior art, the object of the invention is to provide a kind of method being Template preparation water-soluble nano silver with natural safe short amylose, the short amylose utilizing biological enzyme to prepare is template, preparation Nano Silver domain size distribution at 2-5nm, prepare particle diameter little, can be water-soluble rapidly.
For achieving the above object, the technology used in the present invention means are: a kind of with the method for short amylose for Template preparation water-soluble nano silver, step is:
One, Feedstock treating: accurately take sodium hydrogen phosphate and citric acid is dissolved in distilled water, stirs and makes it fully dissolve to prepare cushioning liquid; Accurately take in the blue enzyme instillation in general Shandong distilled water, stir and make it abundant mixing, by blue for general Shandong enzyme pretreatment; Taking starch adds in cushioning liquid, obtained starch emulsion;
Two, gelatinization: starch emulsion 100 DEG C of water-bath 15 ~ 25 min, make the complete gelatinization of starch, be cooled to 56 ~ 60 DEG C subsequently;
Three, enzymolysis: add the blue enzyme in pretreated general Shandong in step one in the colloidal solution after step 2 gelatinization, enzymolysis 5 ~ 7h;
Four, low-speed centrifugal: the solution that step 3 is obtained while hot with centrifugal 1 ~ 4 min of the rotating speed of 3000 r/min, to remove long linear starch; Continue heating, elevate the temperature to 100 DEG C, keep 8 ~ 12 min, enzyme is thoroughly lost activity, and low-speed centrifugal sloughs the enzyme of sex change, obtained short amylose;
Five, by concentration dilution to 0.04 ~ 0.06% of obtained short amylose, silver nitrate is dissolved in ultra-pure water, stirs and make it abundant mixing, then liquor argenti nitratis ophthalmicus is added in the short amylose solution after dilution, eddy mixer mixing 4 ~ 7min;
Six, be dissolved in ultra-pure water by sodium borohydride, stir and make it abundant mixing, then dropwise join in step 5 gained mixed liquor, with eddy mixer mixing 25 ~ 35s, lucifuge places 42 ~ 55h, and freeze-drying, obtains water-soluble nano silver.
Further, sodium hydrogen phosphate in described step one: citric acid: distilled water=2 ~ 4:1 ~ 3:200.
Further, the pH value range 4.6 ~ 4.8 of cushioning liquid in described step one.
Further, the starch in described step one refers to the one of Waxy Rice Starch, taro starch, glutinous millet starch.
Advantageous Effects of the present invention is: with natural safe short amylose for Template preparation water-soluble nano silver, utilize biology enzyme to form stable solution, the Nano Silver particle diameter of preparation is extra small, be about 2 ~ 5nm, be evenly distributed, can be water-soluble rapidly, reaction condition is gentle, safe preparation process environmental protection.Equipment requirement is low, and technique is simple, and easy and simple to handle, the reaction time is short, and efficiency is high, is applicable to large-scale production; Properties of product are good, and preparation cost is low, and energy resource consumption is few, produce without bazardous waste, meet the modern production requirement of " green production, environmental protection and energy saving ".
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described.
The particle diameter of Fig. 1 to be the short amylose of the present invention be Nano Silver of Template preparation;
Fig. 2 is the Nano Silver not having Template preparation;
Fig. 3 is with the transmission electron microscope of the short amylose Nano Silver that is Template preparation;
The short amylose of Fig. 4 is the EDS of the Nano Silver of Template preparation;
The short amylose of Fig. 5 is the X diffraction pattern of the Nano Silver of Template preparation.
Detailed description of the invention
embodiment 1
With the method for short amylose for Template preparation water-soluble nano silver, step is:
Preparation cushioning liquid: accurately take 3.27 g sodium hydrogen phosphates and 2.24 g citric acids are dissolved in 200 mL distilled water, stirs and makes it fully dissolve, stand-by; The blue enzyme pretreatment in general Shandong: accurately take the 1 blue enzyme in the general Shandong of mL and instill in 50 mL distilled water, stir and make it abundant mixing, stand-by; Prepare starch milk: take 15 g Waxy Rice Starchs and add in 100 mL cushioning liquid, the starch emulsion of obtained 10%; The pH value range 4.6 ~ 4.8 of cushioning liquid;
Gelatinization: by starch milk 100 DEG C of water-bath 20 min of preparation, make the complete gelatinization of starch, is cooled to 58 DEG C (optimum temperatures of the blue enzyme in general Shandong) subsequently; Enzymolysis: add the blue enzyme in the general Shandong handled well in the colloidal solution after gelatinization, enzymolysis 6 h; Low-speed centrifugal: by the solution that obtains while hot with centrifugal 3 min of the rotating speed of 3000 r/min, to remove long linear starch; Go out enzyme: continue heating, elevate the temperature to 100 DEG C, keep 10 min, enzyme is thoroughly lost activity, low-speed centrifugal sloughs the enzyme of sex change, obtained short amylose;
By the concentration dilution to 0.05% of obtained short amylose, stand-by; Accurately taking 0.17 g silver nitrate is dissolved in 100 ml ultra-pure waters, stirs and makes it abundant mixing, stand-by; Accurately taking 0.0756 g sodium borohydride is dissolved in 100 ml ultra-pure waters, stirs and makes it abundant mixing, stand-by; Accurately take 200 ul silver nitrates to be added in the short amylose of 2 ml, then eddy mixer mixes 5 min, stand-by; Dropwise join in the mixed liquor of silver nitrate and short amylose by 2 ml sodium borohydrides, mix 30 s with eddy mixer, lucifuge places 48 h, and namely freeze-drying obtains water-soluble nano silver.
embodiment 2
Preparation cushioning liquid: accurately take 3.27 g sodium hydrogen phosphates and 2.24 g citric acids are dissolved in 200 mL distilled water, stirs and makes it fully dissolve, stand-by; The blue enzyme pretreatment in general Shandong: accurately take the 1 blue enzyme in the general Shandong of mL and instill in 50 mL distilled water, stir and make it abundant mixing, stand-by;
Prepare starch milk: take 20g waxy corn starch and add in 100 mL cushioning liquid, the starch emulsion of obtained 10%; Gelatinization: by starch milk 100 DEG C of water-bath 25 min of preparation, make the complete gelatinization of starch, be cooled to 60 DEG C subsequently; Enzymolysis: add the blue enzyme in the general Shandong handled well in the colloidal solution after gelatinization, enzymolysis 5h;
Low-speed centrifugal: by the solution that obtains while hot with centrifugal 4 min of the rotating speed of 3000 r/min, to remove long linear starch; Go out enzyme: continue heating, elevate the temperature to 100 DEG C, and keep 12min, enzyme is thoroughly lost activity, and low-speed centrifugal sloughs the enzyme of sex change, obtained short amylose; By the concentration dilution to 0.06% of obtained short amylose, stand-by;
Accurately taking 0.17 g silver nitrate is dissolved in 100 ml ultra-pure waters, stirs and makes it abundant mixing, stand-by; Accurately taking 0.0756 g sodium borohydride is dissolved in 100 ml ultra-pure waters, stirs and makes it abundant mixing, stand-by; Accurately take 200 ul silver nitrates to be added in the short amylose of 2 ml, then eddy mixer mixing 7min, stand-by; Dropwise join in the mixed liquor of silver nitrate and short amylose by 2 ml sodium borohydrides, with eddy mixer mixing 35s, lucifuge places 55h, and freeze-drying, namely obtains water-soluble nano silver.
embodiment 3
Preparation cushioning liquid: accurately take 3.27 g sodium hydrogen phosphates and 2.24 g citric acids are dissolved in 200 mL distilled water, stirs and makes it fully dissolve, stand-by; The blue enzyme pretreatment in general Shandong: accurately take the 1 blue enzyme in the general Shandong of mL and instill in 50 mL distilled water, stir and make it abundant mixing, stand-by;
Prepare starch milk: take 15 g taro starch and add in 100 mL cushioning liquid, the starch emulsion of obtained 10%; Gelatinization: by starch milk 100 DEG C of water-bath 20 min of preparation, make the complete gelatinization of starch, be cooled to 58 DEG C subsequently; Enzymolysis: add the blue enzyme in the general Shandong handled well in the colloidal solution after gelatinization, enzymolysis 6 h; Low-speed centrifugal: by the solution that obtains while hot with centrifugal 3 min of the rotating speed of 3000 r/min, to remove long linear starch; Go out enzyme: continue heating, elevate the temperature to 100 DEG C, keep 10 min, enzyme is thoroughly lost activity, low-speed centrifugal sloughs the enzyme of sex change, obtained short amylose;
By the concentration dilution to 0.05% of obtained short amylose, stand-by; Accurately taking 0.17 g silver nitrate is dissolved in 100 ml ultra-pure waters, stirs and makes it abundant mixing, stand-by; Accurately taking 0.0756 g sodium borohydride is dissolved in 100 ml ultra-pure waters, stirs and makes it abundant mixing, stand-by; Accurately take 200 ul silver nitrates to be added in the short amylose of 2 ml, then eddy mixer mixes 5 min, stand-by; Dropwise join in the mixed liquor of silver nitrate and short amylose by 2 ml sodium borohydrides, mix 30 s with eddy mixer, lucifuge places 48 h, and namely freeze-drying obtains water-soluble nano silver.
embodiment 4
Preparation cushioning liquid: accurately take 3.27 g sodium hydrogen phosphates and 2.24 g citric acids are dissolved in 200 mL distilled water, stirs and makes it fully dissolve, stand-by; The blue enzyme pretreatment in general Shandong: accurately take the 1 blue enzyme in the general Shandong of mL and instill in 50 mL distilled water, stir and make it abundant mixing, stand-by;
Prepare starch milk: take 5 g glutinous millet starch and add in 100 mL cushioning liquid, the starch emulsion of obtained 10%; Gelatinization: by starch milk 100 DEG C of water-bath 20 min of preparation, make the complete gelatinization of starch, be cooled to 58 DEG C subsequently; Enzymolysis: add the blue enzyme in the general Shandong handled well in the colloidal solution after gelatinization, enzymolysis 6 h; Low-speed centrifugal: by the solution that obtains while hot with centrifugal 3 min of the rotating speed of 3000 r/min, to remove long linear starch;
Go out enzyme: continue heating, elevate the temperature to 100 DEG C, keep 10 min, enzyme is thoroughly lost activity, low-speed centrifugal sloughs the enzyme of sex change, obtained short amylose; By the concentration dilution to 0.05% of obtained short amylose, stand-by; Accurately taking 0.17 g silver nitrate is dissolved in 100 ml ultra-pure waters, stirs and makes it abundant mixing, stand-by; Accurately taking 0.0756 g sodium borohydride is dissolved in 100 ml ultra-pure waters, stirs and makes it abundant mixing, stand-by; Accurately take 200 ul silver nitrates to be added in the short amylose of 2 ml, then eddy mixer mixes 5 min, stand-by; Dropwise join in the mixed liquor of silver nitrate and short amylose by 2 ml sodium borohydrides, mix 30 s with eddy mixer, lucifuge places 48 h, and namely freeze-drying obtains water-soluble nano silver.
embodiment 5
the Nano Silver Performance Detection of preparation
1.the particle size of Nano Silver
1.1 dynamic light scattering scanning spectras
As shown in Figure 1, the particle diameter of Nano Silver is distributed in 2-6 about nm substantially, is mainly distributed in 2-4 nm.
1.2 observe under transmission electron microscope
As seen from Figure 2, do not have the nano-Ag particles shape of Template preparation to differ, what have is spherical in shape, some ovalizes, and the particle of the Nano Silver obtained for template with short amylose is as seen from Figure 3 spherical in shape, regular shape, and is evenly distributed.
The Nano Silver formed as seen from Figure 4 does not have impurity, and the existence of copper comes from copper mesh.
2. X diffraction patterns
As shown in Figure 5, with the Nano Silver that short amylose is Template preparation, there is face-centered cubic crystal, characteristic peak 38.9 ° (111), 45 ° (200), 64.1 ° (220), and 76.0 ° (311).
The present invention for Template preparation water-soluble nano silver, utilizes biology enzyme to form stable solution with natural safe short amylose, and the Nano Silver particle diameter of preparation is extra small, be about 2 ~ 5nm, be evenly distributed, can be water-soluble rapidly, reaction condition is gentle, safe preparation process environmental protection.Equipment requirement is low, and technique is simple, and easy and simple to handle, the reaction time is short, and efficiency is high, is applicable to large-scale production; Properties of product are good, and preparation cost is low, and energy resource consumption is few, produce without bazardous waste, meet the modern production requirement of " green production, environmental protection and energy saving ".
Disclosed embodiment of this invention is only as the explanation to the inventive method, and not as a kind of restriction, the change of any those skilled in the art of belonging in the disclosure of invention all belongs to protection scope of the present invention.
Claims (4)
1. with the method for short amylose for Template preparation water-soluble nano silver, it is characterized in that, step is:
One, Feedstock treating: accurately take sodium hydrogen phosphate and citric acid is dissolved in distilled water, stirs and makes it fully dissolve to prepare cushioning liquid; Accurately take in the blue enzyme instillation in general Shandong distilled water, stir and make it abundant mixing, by blue for general Shandong enzyme pretreatment; Taking starch adds in cushioning liquid, obtained starch emulsion;
Two, gelatinization: starch emulsion 100 DEG C of water-bath 15 ~ 25 min, make the complete gelatinization of starch, be cooled to 56 ~ 60 DEG C subsequently;
Three, enzymolysis: add the blue enzyme in pretreated general Shandong in step one in the colloidal solution after step 2 gelatinization, enzymolysis 5 ~ 7h;
Four, low-speed centrifugal: the solution that step 3 is obtained while hot with centrifugal 1 ~ 4 min of the rotating speed of 3000 r/min, to remove long linear starch; Continue heating, elevate the temperature to 100 DEG C, keep 8 ~ 12 min, enzyme is thoroughly lost activity, and low-speed centrifugal sloughs the enzyme of sex change, obtained short amylose;
Five, by concentration dilution to 0.04 ~ 0.06% of obtained short amylose, silver nitrate is dissolved in ultra-pure water, stirs and make it abundant mixing, then liquor argenti nitratis ophthalmicus is added in the short amylose solution after dilution, eddy mixer mixing 4 ~ 7min;
Six, be dissolved in ultra-pure water by sodium borohydride, stir and make it abundant mixing, then dropwise join in step 5 gained mixed liquor, with eddy mixer mixing 25 ~ 35s, lucifuge places 42 ~ 55h, and freeze-drying, obtains water-soluble nano silver.
2. according to claim 1 with the method for short amylose for Template preparation water-soluble nano silver, it is characterized in that: sodium hydrogen phosphate in described step one: citric acid: distilled water=2 ~ 4:1 ~ 3:200.
3. according to claim 1 with the method for short amylose for Template preparation water-soluble nano silver, it is characterized in that: the pH value range 4.6 ~ 4.8 of cushioning liquid in described step one.
4. according to claim 1 with the method for short amylose for Template preparation water-soluble nano silver, it is characterized in that: the starch in described step one refers to the one of Waxy Rice Starch, taro starch, glutinous millet starch.
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