CN105522165B - Preparation method for nano-silver particles - Google Patents
Preparation method for nano-silver particles Download PDFInfo
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- CN105522165B CN105522165B CN201510948285.6A CN201510948285A CN105522165B CN 105522165 B CN105522165 B CN 105522165B CN 201510948285 A CN201510948285 A CN 201510948285A CN 105522165 B CN105522165 B CN 105522165B
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- 239000002245 particle Substances 0.000 title claims abstract description 44
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006228 supernatant Substances 0.000 claims abstract description 16
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 15
- 235000009566 rice Nutrition 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000005273 aeration Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- 239000004382 Amylase Substances 0.000 claims abstract description 7
- 102000013142 Amylases Human genes 0.000 claims abstract description 7
- 108010065511 Amylases Proteins 0.000 claims abstract description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 7
- 235000019418 amylase Nutrition 0.000 claims abstract description 7
- 238000010792 warming Methods 0.000 claims abstract description 7
- 238000007710 freezing Methods 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 5
- 240000007594 Oryza sativa Species 0.000 claims abstract 4
- 238000003756 stirring Methods 0.000 claims description 35
- 238000009413 insulation Methods 0.000 claims description 18
- 238000009835 boiling Methods 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 230000004044 response Effects 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 7
- 239000007858 starting material Substances 0.000 claims description 7
- 235000009436 Actinidia deliciosa Nutrition 0.000 claims description 6
- 244000298697 Actinidia deliciosa Species 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 6
- 229940043237 diethanolamine Drugs 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 6
- 235000019674 grape juice Nutrition 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000002390 rotary evaporation Methods 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 3
- 241000196324 Embryophyta Species 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 26
- 239000007788 liquid Substances 0.000 abstract description 9
- 239000000047 product Substances 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- 238000001704 evaporation Methods 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000006227 byproduct Substances 0.000 abstract 1
- 125000002791 glucosyl group Chemical class C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- 239000000463 material Substances 0.000 description 14
- 241000209094 Oryza Species 0.000 description 11
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 208000015181 infectious disease Diseases 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 241000790917 Dioxys <bee> Species 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- -1 antibacterial Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- ACIAHEMYLLBZOI-ZZXKWVIFSA-N Unsaturated alcohol Chemical compound CC\C(CO)=C/C ACIAHEMYLLBZOI-ZZXKWVIFSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a preparation method for nano-silver particles, and belongs to the field of preparation of the nano-silver particles. The preparation method includes the steps that rice is washed, water is added for stewing the rice, yeast powder and amylase are added to be stirred, and a reaction under the heat preservation condition is made; then glucose class matter is added to be mixed, and centrifugal separation is carried out after standing to obtain a supernatant for standby application; an ultrasonic container is opened, the infrared wave length is controlled, an ammonium chloride solution is added, the pH of the solution is adjusted to be alkaline through sodium hydroxide, and the solution, ethyl acetate and the like are mixed; carbon dioxide is led in from the bottom of the container for aeration, and silver nitrate and the supernatant for standby application are dropwise added while aeration is carried out; and standing filtering is carried out to obtain filtration matter, and warming evaporation is carried out after freezing to prepare the nano-silver particles. The preparation method has the beneficial effects that the preparing method is simple, the nano-silver particles are evenly scattered in the preparing process, solid-liquid separating is easy, and by-products are fewer; and obtained products are regular in shape and broad and even in size distribution, and the purity of the obtained product is more than 6% higher than those obtained through other methods.
Description
Technical field
The present invention relates to a kind of preparation method of nano silver particles, belong to nano silver particles preparation field.
Background technology
Nano material refers to that nanostructured is piled up by certain way or disperses the macroscopic material to be formed nanometer in certain matrix
Material has quantum size effect, small-size effect, skin effect and macro quanta tunnel effect and shows different from common
The unusual performance of the aspects such as the light of material, electricity, magnetic, thermodynamics and chemical reaction, is a kind of important functional material.Nanometer silver granuel
Significant properties of the son with nanostructured, can be widely applied to the multiple fields such as catalyst, medicine, antibacterial, composite.In recent years
Come, the technology of preparing of nano silver particles is developed rapidly, and domestic and international preparation method is varied.Because some of nano silver particles are special
Different property：Such as good electric conductivity, superpower sterilizing ability, laser excitation efficiency higher and extremely strong third-order non-linear system
The properties such as number so that nano silver particles or using the prepared composite of nano silver particles doping be widely used in superconduction,
The industries such as chemical industry, medical science, optics, electronics, electrical equipment.Because nano silver particles have very big Raman active, with surface enhanced
The development of Raman technology, the preparation of nano silver particles also obtains great development.
The method for preparing nano silver particles at present has solution phase chemical reduction, physical crushing method, vacuum condensation method and precipitation
Method, solution phase chemical reduction is that silver is sunk in powder form from its salt or the complex aqueous solution or organic system with reducing agent
Product is out.Conventional reducing agent has compound of ascorbic acid, unsaturated alcohol, sodium citrate, hydrazine and hydrazine etc..The advantage of the method is
Apparatus and process is simple, yield is high, be easy to industrialized production, and obtained silver powder granularity is small, favorable reproducibility, be current laboratory and
Industrial widely used method.But obtained nano-Ag particles have that separation of solid and liquid is difficult, size distribution is wide, easy group
Poly- the shortcomings of.Physical crushing method is to crush raw material by methods such as mechanical crushing, ultrasonic wave, electric spark blasts to obtain Nano Silver
Particle.By in inert gas, on the substrate of low temperature, being sputtered using high-pressure magnetic, containing nano silver particles two have been made
Silicon oxide film.The characteristics of the method is that operation is simple, low cost, but product purity is low, and distribution of particles is uneven, and not
It is readily available the product compared with small particle.Vacuum condensation method be in vacuum or atmosphere of inert gases, it is high with heating, laser, electric arc
The methods such as frequency sensing produce high temperature, silver material is gasified or form plasma, and then quenching is allowed to condensation and obtains a nanometer silver granuel
Son.In atmosphere of inert gases, nano silver particles are prepared by the method for condensing.The method has that purity is high, crystallization group
Weave, the advantage that granularity is controllable, but technical equipment requirement is high, typically requires purity silver material very high, and there is Nano Silver
The shortcoming of particle coalescence.The precipitation method are that precipitating reagent is added in salting liquid, and the active ingredient of raw material is given birth to by chemical reaction
Into precipitation, then nano silver particles are obtained through filtering, washing, dry, drying.In the condition that PVP is present
Under, reduce silver ionized water solution, the nano silver particles for having obtained with urotropine.The method is at present using widely
A kind of method, its advantage is that technological process is short, easy to operate, raw material is readily available, but is easily introduced impurity, and purity is low, particle diameter
Greatly, it is difficult to prepare the nano silver particles for comparing small particle.
The content of the invention
The technical problems to be solved by the invention：Easily reunite for nano silver particles in current method preparation process, consolidate
Liquid separates difficult, and accessory substance is more, cause that products obtained therefrom pattern is irregular, particle diameter distribution it is wide in range it is uneven, the drawbacks of purity is low, carry
Supply one kind to clean the boiling that adds water by by rice, added insulation reaction after starter powder and amylase stirring, add glucose
Material mixing, to obtain supernatant standby for centrifugation after standing, then opens ultrasonic container, controls infrared wavelength, adds chlorination
Ammonium salt solution, it is alkalescence to adjust its pH with NaOH, mix with ethyl acetate etc., and being passed through carbon dioxide from container bottom is aerated,
Silver nitrate and standby supernatant is added dropwise in aeration, then stands and filters to obtain filtrate, the prepared Nano Silver of evaporation is heated after freezing
The method of particle.Preparation process solid-liquid of the present invention is easily separated, and products obtained therefrom particle diameter distribution is uniform, and purity is high.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
(1) 1~2kg rice is taken, 30~40min of immersion in clear water is put into, circular bottom pot is put into after rinsing 1~2 time with current
In, water is added thereto to, make it not have 7~8cm of rice to be advisable, 50~60 DEG C, boiling are warming up to the speed program of 5 DEG C/min
After 20~30min, stir-fried 3~4 times with iron spoon bottom from pot, then heat to 100~105 DEG C, 1~2h of insulation boiling；
(2) treat it is secondary boiled after the completion of, the starch of 20~30g starter powders and gross mass 0.3~0.5% is separately added into thereto
Enzyme, controls temperature for 40~50 DEG C, controls rotating speed for 200~300r/min, stirs 20~30min, it is sufficiently mixed uniformly,
1~2h of insulation reaction, after the completion for the treatment of insulation reaction, then is added thereto to 20~22mL kiwi-fruit juices, keeps rotating speed, temperature not
Become, stir 50~60min；
(3) while stirring with the speed of 2~3mL/min to the grape juice that 8~10mL is added in said mixture, stirring 20
~30min, it is 60~80r/min then to reduce rotating speed, stirs 20~25min, stands 1~2h, after standing is finished, is put into rotating speed
For 10~15min is centrifuged in the centrifuge of 2000~3000r/min, supernatant is obtained standby；
(4) ultrasonic response container is opened, 25~35kHz of supersonic frequency is set, control infrared wavelength for 200~300 μm,
The ammonium chloride solution that 20~30mL mass fractions are 60~80% is added thereto to, while adding 15~20mL NaOH molten
Liquid, it is 11.2~12.2 to adjust its pH value, then is added to 10~15mL diethanol amine and 10~15mL ethyl acetate respectively,
Control rotating speed for 500~700r/min, 50~60min of magnetic agitation is well mixed；
(5) after after above-mentioned being well mixed, it is passed through carbon dioxide from ultrasonic response container bottom and is aerated, controls dioxy
Change carbon and be passed through speed for 10~15mL/s, 30~40mL mass point is added dropwise with the speed of 10~12mL/min thereto in aeration
Number is 20~30% silver nitrate solution, while 180~360mL steps (3) are added dropwise thereto with the speed of 60~100mL/min
Standby supernatant；
(6) after after above-mentioned completion of dropping, continuing to be aerated 40~50min, 1~2h is stood, then carries out filtering to obtain filtrate,
At being placed in -20~-18 DEG C freeze 5~7h, it is to be frozen finish after, be heated up to 100~105 DEG C, 2~3h of rotary evaporation makes
Obtain a kind of nano silver particles.
Application process of the invention：Obtained nano silver particles are added in the coating such as paint, pigment, addition be 5~
7g/kg, is coated on sheet material after stirring, and can effectively kill the germ that is attached on sheet material and the duration is long, so as to drop
The probability of low people's bacteria infection, is worthy to be popularized and uses.
Compared with other method, Advantageous Effects are the present invention：
(1) preparation method of the present invention is simple, in preparation process nano silver particles be uniformly dispersed, solid-liquid it is easily separated, accessory substance
It is few；
(2) the wide in range uniform, purity of products obtained therefrom pattern rule, particle diameter distribution is higher than other method more than 6%.
Specific embodiment
1~2kg rice is taken first, 30~40min of immersion in clear water is put into, and circular bottom pot is put into after rinsing 1~2 time with current
In, water is added thereto to, make it not have 7~8cm of rice to be advisable, 50~60 DEG C, boiling are warming up to the speed program of 5 DEG C/min
After 20~30min, stir-fried 3~4 times with iron spoon bottom from pot, then heat to 100~105 DEG C, 1~2h of insulation boiling；Treat
After the completion of secondary boiled, the amylase of 20~30g starter powders and gross mass 0.3~0.5% is separately added into thereto, control the temperature to be
40~50 DEG C, control rotating speed for 200~300r/min, stir 20~30min, it is sufficiently mixed uniformly, insulation reaction 1~
2h, after the completion for the treatment of insulation reaction, then is added thereto to 20~22mL kiwi-fruit juices, keeps rotating speed, temperature-resistant, and stirring 50~
60min；While stirring with the speed of 2~3mL/min in said mixture add 8~10mL grape juice, stirring 20~
30min, it is 60~80r/min then to reduce rotating speed, stirs 20~25min, stands 1~2h, and after standing is finished, being put into rotating speed is
10~15min is centrifuged in the centrifuge of 2000~3000r/min, supernatant is obtained standby；Then ultrasonic response container is opened, if
Put 25~35kHz of supersonic frequency, control infrared wavelength for 200~300 μm, be added thereto to 20~30mL mass fractions for 60~
80% ammonium chloride solution, while adding 15~20mL sodium hydroxide solutions, adjusts its pH value for 11.2~12.2, then respectively to
10~15mL diethanol amine and 10~15mL ethyl acetate are wherein added, rotating speed is controlled for 500~700r/min, magnetic agitation 50
~60min is well mixed；After after above-mentioned being well mixed, it is passed through carbon dioxide from ultrasonic response container bottom and is aerated, controls
Carbon dioxide processed is passed through speed for 10~15mL/s, and 30~40mL is added dropwise thereto with the speed of 10~12mL/min in aeration
Mass fraction is 20~30% silver nitrate solution, while 180~360mL is added dropwise thereto with the speed of 60~100mL/min
Standby supernatant；Finally after after above-mentioned completion of dropping, continuing to be aerated 40~50min, 1~2h is stood, then carry out filtering
Filtrate, freezes 5~7h at being placed in -20~-18 DEG C, it is to be frozen finish after, be heated up to 100~105 DEG C, rotary evaporation 2~
3h, that is, be obtained a kind of nano silver particles.
Example 1
1kg rice is taken first, is put into clear water and is soaked 30min, be put into circular bottom pot after rinsing 1 time with current, thereto
Add water, make it not have rice 7cm to be advisable, be warming up to 50 DEG C, after boiling 20min with the speed program of 5 DEG C/min, with iron spoon from
Bottom stir-fries 3 times in pot, then heats to 100 DEG C, insulation boiling 1h；Treat it is secondary boiled after the completion of, 20g is separately added into thereto
The amylase of starter powder and gross mass 0.3%, controls temperature for 40 DEG C, controls rotating speed for 200r/min, stirs 20min, fills it
Point well mixed, insulation reaction 1h, after the completion for the treatment of insulation reaction, then is added thereto to 20mL kiwi-fruit juices, keeps rotating speed, temperature
It is constant, stir 50min；While stirring with the speed of 2mL/min to the grape juice that 8mL is added in said mixture, stirring
20min, it is 60r/min then to reduce rotating speed, stirs 20min, stands 1h, and after standing is finished, it is 2000r/min's to be put into rotating speed
10min is centrifuged in centrifuge, supernatant is obtained standby；Then ultrasonic response container is opened, supersonic frequency 25kHz, control is set
Infrared wavelength is 200 μm, is added thereto to the ammonium chloride solution that 20mL mass fractions are 60%, while adding 15mL NaOH
Solution, adjusts its pH value for 11.2, then is added to 10mL diethanol amine and 10mL ethyl acetate respectively, controls the rotating speed to be
500r/min, magnetic agitation 50min are well mixed；After after above-mentioned being well mixed, dioxy is passed through from ultrasonic response container bottom
Change carbon to be aerated, control carbon dioxide to be passed through speed for 10mL/s, be added dropwise thereto with the speed of 10mL/min in aeration
30mL mass fractions are 20% silver nitrate solution, while the standby supernatants of 180mL are added dropwise thereto with the speed of 60mL/min
Liquid；Finally after after above-mentioned completion of dropping, continuing to be aerated 40min, 1h is stood, then carry out filtering to obtain filtrate, be placed in -20 DEG C
Lower freezing 5h, it is to be frozen finish after, be heated up to 100 DEG C, rotary evaporation 2h is obtained a kind of nano silver particles.
Obtained nano silver particles are added in the coating such as paint, pigment, addition is 5g/kg, are coated after stirring
In on sheet material, can effectively killing the germ that is attached on sheet material and the duration is long, so that the probability of people's bacteria infection is reduced,
It is worthy to be popularized and uses.
Example 2
1.5kg rice is taken first, is put into clear water and is soaked 35min, be put into circular bottom pot after rinsing 2 times with current, Xiang Qi
Middle addition water, makes it not have rice 7.5cm to be advisable, and 55 DEG C are warming up to the speed program of 5 DEG C/min, after boiling 25min, uses iron
Spoon bottom from pot stir-fries 4 times, then heats to 103 DEG C, insulation boiling 1.5h；Treat it is secondary boiled after the completion of, distinguish thereto
The amylase of 25g starter powders and gross mass 0.4% is added, temperature is controlled for 45 DEG C, controls rotating speed for 250r/min, stir 25min,
It is set to be sufficiently mixed uniformly, insulation reaction 1.5h after the completion for the treatment of insulation reaction, then is added thereto to 21mL kiwi-fruit juices, keeps
Rotating speed, temperature-resistant, stirring 55min；While stirring with the speed of 3mL/min to the grape juice that 9mL is added in said mixture,
Stirring 25min, it is 70r/min then to reduce rotating speed, stirs 23min, stands 1.5h, and after standing is finished, being put into rotating speed is
13min is centrifuged in the centrifuge of 2500r/min, supernatant is obtained standby；Then ultrasonic response container is opened, supersonic frequency is set
30kHz, controls infrared wavelength for 250 μm, is added thereto to the ammonium chloride solution that 25mL mass fractions are 70%, while adding
18mL sodium hydroxide solutions, it is 11.7 to adjust its pH value, then is added to 13mL diethanol amine and 13mL ethyl acetate respectively,
Control rotating speed for 600r/min, magnetic agitation 55min is well mixed；After after above-mentioned being well mixed, from ultrasonic response container bottom
Portion is passed through carbon dioxide and is aerated, and controls carbon dioxide to be passed through speed for 13mL/s, in aeration with the speed of 11mL/min
35mL mass fractions are added dropwise thereto and are 25% silver nitrate solution, while 270mL is added dropwise thereto with the speed of 80mL/min
Standby supernatant；Finally after after above-mentioned completion of dropping, continuing to be aerated 45min, 1.5h is stood, then carry out filtering and must filtering
Thing, freezes 6h at being placed in -19 DEG C, it is to be frozen finish after, be heated up to 103 DEG C, rotary evaporation 2.5h is obtained a kind of Nano Silver
Particle.
Obtained nano silver particles are added in the coating such as paint, pigment, addition is 6g/kg, are coated after stirring
In on sheet material, can effectively killing the germ that is attached on sheet material and the duration is long, so that the probability of people's bacteria infection is reduced,
It is worthy to be popularized and uses.
Example 3
2kg rice is taken first, is put into clear water and is soaked 40min, be put into circular bottom pot after rinsing 2 times with current, thereto
Add water, make it not have rice 8cm to be advisable, be warming up to 60 DEG C, after boiling 30min with the speed program of 5 DEG C/min, with iron spoon from
Bottom stir-fries 4 times in pot, then heats to 105 DEG C, insulation boiling 2h；Treat it is secondary boiled after the completion of, 30g is separately added into thereto
The amylase of starter powder and gross mass 0.5%, controls temperature for 50 DEG C, controls rotating speed for 300r/min, stirs 30min, fills it
Point well mixed, insulation reaction 2h, after the completion for the treatment of insulation reaction, then is added thereto to 22mL kiwi-fruit juices, keeps rotating speed, temperature
It is constant, stir 60min；While stirring with the speed of 3mL/min to the grape juice that 10mL is added in said mixture, stirring
30min, it is 80r/min then to reduce rotating speed, stirs 25min, stands 2h, and after standing is finished, it is 3000r/min's to be put into rotating speed
15min is centrifuged in centrifuge, supernatant is obtained standby；Then ultrasonic response container is opened, supersonic frequency 35kHz, control is set
Infrared wavelength is 300 μm, is added thereto to the ammonium chloride solution that 30mL mass fractions are 80%, while adding 20mL NaOH
Solution, adjusts its pH value for 12.2, then is added to 15mL diethanol amine and 15mL ethyl acetate respectively, controls the rotating speed to be
700r/min, magnetic agitation 60min are well mixed；After after above-mentioned being well mixed, dioxy is passed through from ultrasonic response container bottom
Change carbon to be aerated, control carbon dioxide to be passed through speed for 15mL/s, be added dropwise thereto with the speed of 12mL/min in aeration
40mL mass fractions are 30% silver nitrate solution, while the standby supernatants of 360mL are added dropwise thereto with the speed of 100mL/min
Liquid；Finally after after above-mentioned completion of dropping, continuing to be aerated 50min, 2h is stood, then carry out filtering to obtain filtrate, be placed in -18 DEG C
Lower freezing 7h, it is to be frozen finish after, be heated up to 105 DEG C, rotary evaporation 3h is obtained a kind of nano silver particles.
Obtained nano silver particles are added in the coating such as paint, pigment, addition is 7g/kg, are coated after stirring
In on sheet material, can effectively killing the germ that is attached on sheet material and the duration is long, so that the probability of people's bacteria infection is reduced,
It is worthy to be popularized and uses.
Claims (1)
1. a kind of preparation method of nano silver particles, it is characterised in that specific preparation process is：
(1) 1~2kg rice is taken, 30~40min of immersion in clear water is put into, is put into circular bottom pot after rinsing 1~2 time with current, to
Water is wherein added, makes it not have 7~8cm of rice to be advisable, 50~60 DEG C are warming up to the speed program of 5 DEG C/min, boiling 20~
After 30min, stir-fried 3~4 times with iron spoon bottom from pot, then heat to 100~105 DEG C, 1~2h of insulation boiling；
(2) treat it is secondary boiled after the completion of, the amylase of 20~30g starter powders and gross mass 0.3~0.5% is separately added into thereto,
Temperature is controlled for 40~50 DEG C, controls rotating speed for 200~300r/min, stir 20~30min, it is sufficiently mixed uniformly, protected
Temperature 1~2h of reaction, after the completion for the treatment of insulation reaction, then is added thereto to 20~22mL kiwi-fruit juices, keeps rotating speed, temperature-resistant,
50~60min of stirring；
(3) while stirring with the speed of 2~3mL/min in said mixture add 8~10mL grape juice, stirring 20~
30min, it is 60~80r/min then to reduce rotating speed, stirs 20~25min, stands 1~2h, and after standing is finished, being put into rotating speed is
10~15min is centrifuged in the centrifuge of 2000~3000r/min, supernatant is obtained standby；
(4) ultrasonic response container is opened, 25~35kHz of supersonic frequency is set, it is 200~300 μm, Xiang Qi to control infrared wavelength
Middle addition 20~30mL mass fractions are 60~80% ammonium chloride solution, while adding 15~20mL sodium hydroxide solutions, are adjusted
It is 11.2~12.2 to save its pH value, then is added to 10~15mL diethanol amine and 10~15mL ethyl acetate respectively, is controlled
Rotating speed is 500~700r/min, and 50~60min of magnetic agitation is well mixed；
(5) after after above-mentioned being well mixed, it is passed through carbon dioxide from ultrasonic response container bottom and is aerated, controls carbon dioxide
Speed is passed through for 10~15mL/s, 30~40mL mass fractions are added dropwise thereto with the speed of 10~12mL/min in aeration is
20~30% silver nitrate solution, while it is standby that 180~360mL steps (3) are added dropwise thereto with the speed of 60~100mL/min
Supernatant；
(6) after after above-mentioned completion of dropping, continuing to be aerated 40~50min, 1~2h is stood, then carries out filtering to obtain filtrate, juxtaposition
In freezing 5~7h at -20~-18 DEG C, it is to be frozen finish after, be heated up to 100~105 DEG C, 2~3h of rotary evaporation is obtained one
Plant nano silver particles.
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|---|---|---|---|---|
| JP2007039718A (en) * | 2005-08-01 | 2007-02-15 | Dowa Holdings Co Ltd | Method for producing silver powder |
| JP2008214691A (en) * | 2007-03-02 | 2008-09-18 | Ishihara Sangyo Kaisha Ltd | Metal fine particles, metal colloidal liquid in which it is dispersed in a solvent, and methods for producing them |
| CN102343440A (en) * | 2010-07-29 | 2012-02-08 | 同济大学 | Method for preparing water-soluble nano silver by using actinidia as template |
| CN105057690A (en) * | 2015-07-20 | 2015-11-18 | 昆明理工大学 | Preparation method of high-dispersibility superfine spherical silver powder |
| CN105142829A (en) * | 2013-04-26 | 2015-12-09 | 同和电子科技有限公司 | Metal nanoparticle dispersion, process for producing metal nanoparticle dispersion, and bonding method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007039718A (en) * | 2005-08-01 | 2007-02-15 | Dowa Holdings Co Ltd | Method for producing silver powder |
| JP2008214691A (en) * | 2007-03-02 | 2008-09-18 | Ishihara Sangyo Kaisha Ltd | Metal fine particles, metal colloidal liquid in which it is dispersed in a solvent, and methods for producing them |
| CN102343440A (en) * | 2010-07-29 | 2012-02-08 | 同济大学 | Method for preparing water-soluble nano silver by using actinidia as template |
| CN105142829A (en) * | 2013-04-26 | 2015-12-09 | 同和电子科技有限公司 | Metal nanoparticle dispersion, process for producing metal nanoparticle dispersion, and bonding method |
| CN105057690A (en) * | 2015-07-20 | 2015-11-18 | 昆明理工大学 | Preparation method of high-dispersibility superfine spherical silver powder |
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