CN104625084B - A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol - Google Patents
A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol Download PDFInfo
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- CN104625084B CN104625084B CN201410850968.3A CN201410850968A CN104625084B CN 104625084 B CN104625084 B CN 104625084B CN 201410850968 A CN201410850968 A CN 201410850968A CN 104625084 B CN104625084 B CN 104625084B
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Abstract
The present invention relates to a kind of utilize cryogenic technique preparation and the method that preserves colourless nano silver colloidal sol, comprise the following steps: 1) silver material will be contained it will be added to the water, mix homogeneously, obtain the aqueous solution containing silver material, freezing, pulverize, obtain the Sorbet containing silver material；2) reducing agent is added to the water, mix homogeneously, obtains the aqueous solution containing reducing agent, freezing, pulverize, obtain the Sorbet containing reducing agent；3) step 1) Sorbet containing silver material that obtains and step 2) obtain the Sorbet mixing containing reducing agent, grind, obtain the ice crystal containing nanometer silver；4) step 3 is preserved) the nanometer silver ice crystal that obtains.Preparation of the present invention and preserve the method for colourless nanometer silver and have and need not pyroreaction, need not separation process, it is not necessary to protective agent, dispersant, and the nanometer silver prepared has, and nucleus height little, active, purity is high and safety advantages of higher.
Description
Technical field
The invention belongs to technical field of nano material, relate to cryogenic technique solid phase and prepare nano material, a kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol.
Background technology
Particle diameter is accomplished nano level argent simple substance by nanometer silver exactly.It is reported that nanometer silver all has broad application prospects in fields such as anti-biotic material, effective catalyst, lubricant, light absorbing material, coating, sensor, electrocondution slurry, high performance electrode materials, become functional material theoretical research and the important topic of application and development with property.As added a small amount of nanometer silver in chemical fibre, some performance of chemical fibre product can be improved, and make it have the strongest sterilizing ability；Adulterate in silicon oxide film appropriate nanometer silver, and the glass of this thin film of plating can be made to have certain Photoluminescence；It is coated with burn wound and cureless hemorrhoid with Nanometer silver dressing, can achieve good results.
At present, the preparation of nanometer silver and store method, it is primarily present problems with:
1) preparation method of nanometer silver is based on methods such as support methods/template, sol-gel process, solid phase method, irradiation methods at present, and step is more, preparation technology is wayward, and preparation condition is harsh；
2) nanometer silver preparation method is shown in the process-intensive that document is reported at present, and the nanometer silver prepared varies in color, along with the changes colour of particle diameter presents glassy yellow, brown color, brownish red, aubergine, bluish violet and brown etc..Chinese patent 200410069105.9 discloses the preparation method of a kind of nano silver colloid aqueous solution; the method is to use double injecting control technology; under the stirring of agitator; the Dual Implantations while of silver ammonia spirit and reducing agent aqueous solution is contained in the reaction system of protective agent aqueous solution; generate nano silver particles; through ultrafiltration desalination, obtain the nano silver colloid aqueous solution of nanometer.200810143657.8 preparation methoies disclosing a kind of nanometer silver, its principal character, with high-pressure sterilizing pot as reaction environment, utilizes silver nitrate as protective agent, to prepare nano silver colloidal sol for silver source, the polysaccharide material such as soluble starch.201010215387.4 preparation methoies disclosing a kind of nano silver colloidal sol, it comprises the following steps, and a) is dissolved in ultra-pure water by silver nitrate, obtains silver nitrate solution；B) described silver nitrate solution is quickly stirred with agitator；C) heat described silver nitrate solution by oil bath, after being heated to uniform temperature, reduce the mixing speed of described agitator；D) it is continually fed into silver nitrate solution described in hydrogen reducing and prepares nano silver colloidal sol.201310574416.X disclose a kind of nano silver colloidal sol and preparation thereof and purification process; use silver salt, protective agent and cosolvent; with water as solvent; by silver salt solution, protective agent aqueous solution; add the reduction of a certain amount of reducing agent; obtain initial nano silver colloidal sol, this colloidal sol be adjusted pH value, precipitate, separate, wash, weight the most molten after obtain the nano silver colloidal sol of required concentration.The 201410344102.5 disclosure of the invention preparation method of a kind of nano silver colloidal sol, mixes water-soluble with poly-D-lysine to silver nitrate solution or silver ammino solution, stirring reaction 30-180min under conditions of 50-100 DEG C, it is thus achieved that nano silver colloidal sol.
Above invention existence utilizes protective agent, protection gas, elevated temperature heating stage, and the nanometer silver particle size distribution obtained is wide, wayward, unstable properties, preserves perishable problem.And using of protective agent and dispersant etc. inevitably brings problem to the application security of nano-class silver colloidal solution in a large number.The field that color requirements is harsh is restricted at weaving load silver etc. with applying of color nano silver colloidal sol.
Summary of the invention
The technical problem to be solved is, in view of in prior art, nanometer silver must add protective agent, dispersant in preparation process, and the use field that coloured nanometer silver also makes nano silver colloidal sol is restricted.The present invention provides a kind of and utilizes cryogenic technique preparation and the method that preserves colourless nano silver colloidal sol, and described preparation method need not protective agent, dispersant, it is not required that separation process, and the colourless nanometer silver prepared has that granularity is little, purity is high and the advantage such as easy preservation.
The technical scheme is that
A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol, comprises the following steps:
1) silver material will be contained to be added to the water, mix homogeneously, and obtain the aqueous solution containing silver material, freezing, pulverizing, obtain the Sorbet containing silver material；
2) reducing agent is added to the water, mix homogeneously, obtains the aqueous solution containing reducing agent, freezing, pulverize, obtain the Sorbet containing reducing agent；
3) step 1) Sorbet containing silver material that obtains and step 2) obtain the Sorbet mixing containing reducing agent, grind, obtain nanometer silver ice crystal；
4) step 3 is preserved) the nanometer silver ice crystal that obtains.
Further, step 1) in, described is silver nitrate containing silver material, and in described silver nitrate aqueous solution, the molar concentration of silver nitrate is 0.1-0.5mol/L.
Further, step 2) in, the molar concentration of described reducing agent is 0.1-0.5mol/L.
Further, step 2) in, described reducing agent is one or more in ascorbic acid, hydrazine hydrate, hydrogen peroxide.
Further, step 1) and step 2) in, described cryogenic temperature is-4 DEG C to-24 DEG C, cooling time 8-24h；Described grinding particle size is 1-3 μm, and temperature during pulverizing is-15 DEG C to-18 DEG C.
Further, step 3) in, in described reaction, silver material is 4: 3-2: 1 with the mol ratio of reducing agent.
Further, step 3) in, described milling time is 12-48h, and grind size is 0.1-0.3 μm, and temperature during grinding is-15 DEG C to-18 DEG C.
Further, step 4) in, described preservation condition is-4 DEG C to-24 DEG C, can preserve 3 years.
The invention has the beneficial effects as follows:
Preparation of the present invention and the method preserving nanometer silver are to react at low temperatures; directly react at low temperatures with containing silver material (silver nitrate solution) and reducing agent; without protective atmosphere; also without protective agent, dispersant; need not follow-up separation process; time to be used directly with required compound material with the use of, preparation method is simple.
Owing to reaction is to carry out under low temperature state, the nanocrystal of reaction is little, it is not necessary to protective agent, dispersant, directly prepares colourless nano silver colloidal sol ice crystal, and the product that reaction obtains uses cryogenic technique to preserve, and stability is high, the holding time is long.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, is not intended to limit the scope of the present invention.
A kind of method utilizing cryogenic technique to prepare and preserve colourless nano silver colloidal sol, comprises the following steps:
1) silver nitrate is added to the water, mix homogeneously, obtain silver nitrate aqueous solution (in silver nitrate aqueous solution, the molar concentration of silver nitrate is 0.1-0.5mol/L), freezing 8-24h under the conditions of-4 DEG C to-24 DEG C, it is placed in the Sorbet machine with low temperature chuck pulverizing afterwards, grinding particle size is 1-3 μm, and temperature during pulverizing is-15 DEG C to-18 DEG C, obtains the Sorbet containing silver material；
2) one or more of ascorbic acid, hydrogen peroxide or hydrazine hydrate are added to the water, mix homogeneously, obtain the aqueous solution containing reducing agent (wherein the molar concentration of reducing agent is 0.1-0.5mol/L), freezing 8-24h under the conditions of-4 DEG C to-24 DEG C, it is placed on afterwards in the Sorbet machine with low temperature chuck and pulverizes under the conditions of-15 DEG C to-18 DEG C, grinding particle size is 1-3 μm, obtains the Sorbet containing reducing agent；
3) step 1) Sorbet containing silver material that obtains and step 2) obtain the Sorbet containing reducing agent and be concurrently placed in freezing agitating ball mill and mix, temperature during mixing is-15 DEG C to-18 DEG C, 12-48h is ground under the conditions of-15 DEG C to-18 DEG C, granularity after grinding is 0.1-0.3 μm, obtains colourless nanometer silver ice crystal；
4) by step 3) in colourless nanometer silver ice crystal take out be placed on-4 DEG C to-24 DEG C preservations.
Embodiment 1
1) 8.5g silver nitrate is added in 100mL water, mix homogeneously, obtain the silver nitrate aqueous solution of 0.5mol/L, under the conditions of-4 DEG C after cooling time 8h, being placed in the Sorbet machine with low temperature chuck and pulverize under the conditions of-15 DEG C to-18 DEG C, grinding particle size is 1-3 μm, obtains the Sorbet containing silver material；
2) 4.5g ascorbic acid is added in 250mL water, mix homogeneously, obtain 0.1mol/L aqueous ascorbic acid,-4 DEG C of freezing 8h, being placed in the Sorbet machine with low temperature chuck and pulverize under the conditions of-15 DEG C to-18 DEG C, grinding particle size is 1-3 μm, obtains the Sorbet containing ascorbic acid；
3) step 1) Sorbet containing silver material that obtains and step 2) obtain the Sorbet containing ascorbic acid and be concurrently placed in freezing agitating ball mill and mix, temperature during mixing is-15 DEG C to-18 DEG C, 12h is ground under the conditions of-15 DEG C to-18 DEG C, granularity after grinding is 0.1-0.3 μm, obtains colourless nanometer silver ice crystal 359.3g；
4) by step 3) in colourless nanometer silver ice crystal take out be placed on-4 DEG C of preservations.
Embodiment 2
1) 8.5g silver nitrate is added in 500mL water, mix homogeneously, obtain 0.1mol/L silver nitrate aqueous solution, freezing 24h under the conditions of-15 DEG C, it is placed in the Sorbet machine with low temperature chuck pulverizing, grinding particle size is 1-3 μm, and temperature during pulverizing is-15 DEG C to-18 DEG C, obtains the Sorbet containing silver material；
2) the hydrazine hydrate 2.2mL of mass fraction 85% is taken, dilute is to 75mL, obtain the aqueous solution of hydrazine hydrate (wherein, molar concentration 0.5mol/L of hydrazine hydrate), freezing 24h under the conditions of-15 DEG C, being placed in the Sorbet machine with low temperature chuck and pulverize under the conditions of-15 DEG C to-18 DEG C, grinding particle size is 1-3 μm, obtains the Sorbet containing hydrazine hydrate；
3) step 1) Sorbet containing silver material that obtains and step 2) obtain the Sorbet containing hydrazine hydrate and be concurrently placed in freezing agitating ball mill and mix, temperature during mixing is-15 DEG C to-18 DEG C, 48h is ground under the conditions of-15 DEG C to-18 DEG C, granularity after grinding is 0.1-0.3 μm, obtains colourless nanometer silver ice crystal 577.5g；
4) by step 3) in colourless nanometer silver ice crystal take out be placed on-15 DEG C of preservations.
Embodiment 3
1) 8.5g silver nitrate is added in 125mL water, mix homogeneously, obtain silver nitrate aqueous solution (wherein, molar concentration 0.4mol/L of silver nitrate), freezing 10h under the conditions of-24 DEG C, being placed on afterwards in the Sorbet machine with low temperature chuck and pulverize under the conditions of-15 DEG C to-18 DEG C, grinding particle size is 1-3 μm, obtains the Sorbet containing silver material；
2) taking the hydrogen peroxide 2.5mL of 30%, dilute, to 125mL, obtains 0.2mol/L hydrogen peroxide solution,-24 DEG C of freezing 10h, being placed on afterwards in the Sorbet machine with low temperature chuck and pulverize under the conditions of 15 DEG C to-18 DEG C, grinding particle size is 1-3 μm, obtains the Sorbet containing hydrogen peroxide；
3) step 1) Sorbet containing silver material that obtains and step 2) obtain the Sorbet containing hydrogen peroxide and be concurrently placed in freezing agitating ball mill and mix, temperature during mixing is-15 DEG C to-18 DEG C, 24h is ground under the conditions of-15 DEG C to-18 DEG C, granularity after grinding is 0.1-0.3 μm, obtains colourless nanometer silver ice crystal 255.5g；
4) by step 3) in colourless nanometer silver ice crystal take out be placed on-24 DEG C of preservations.
Embodiment 4
1) 8.5g silver nitrate is added in 100mL water, mix homogeneously, obtain the silver nitrate aqueous solution of 0.5mol/L, under the conditions of-24 DEG C after cooling time 8h, it is placed in the Sorbet machine with low temperature chuck and pulverizes under the conditions of-15 DEG C to-18 DEG C, grinding particle size is 1-3 μm, obtains the Sorbet containing silver material；
2) 2.25g ascorbic acid is added in 125mL water, mix homogeneously, obtain 0.1mol/L aqueous ascorbic acid；Taking the hydrogen peroxide 2.0mL of 30%, dilute, to 102.5mL, obtains 0.2mol/L hydrogen peroxide solution；By 0.1mol/L aqueous ascorbic acid obtained above and obtain 0.2mol/L hydrogen peroxide solution mix homogeneously, freezing 8h under the conditions of being placed in-24 DEG C, it is placed in the Sorbet machine with low temperature chuck and pulverizes under the conditions of-15 DEG C to-18 DEG C, grinding particle size is 1-3 μm, obtains the Sorbet containing ascorbic acid and hydrogen peroxide；
3) step 1) Sorbet containing silver material that obtains and step 2) obtain the Sorbet containing ascorbic acid and hydrogen peroxide and be concurrently placed in freezing agitating ball mill and mix, temperature during mixing is-15 DEG C to-18 DEG C, 12h is ground under the conditions of-15 DEG C to-18 DEG C, granularity after grinding is 0.1-0.3 μm, obtains colourless nanometer silver ice crystal 334.5g；
4) by step 3) in colourless nanometer silver ice crystal take out be placed on-24 DEG C of preservations.
In currently available technology, the nano silver colloidal sol of preparation is general all with color.Such as: the prior art (research of glycol method synthesizing stable nano silver colloidal sol, chemistry world, 5th phase 257-259 in 2009) color of nano silver colloidal sol for preparing, present brown color, milky, brown, rufous, khaki, lark, orange etc.；The nano silver colloidal sol that prior art (research being electrode ultrasonic electrolysis synthesizing nano-silver colloidal sol with electro-conductive glass, chemistry world, calendar year 2001 the 6th phase 323-326) prepares is rufous, green, celadon, brown, yellow green etc..And be water white transparency nano silver colloidal sol by the nano silver colloidal sol prepared by the present invention.
Carrying the deficiencies such as the general particle diameter of coloured nano silver colloidal sol is big, particle diameter distribution is wide in prior art, the most coloured nano silver colloidal sol carries silver field by significant limitation in weaving.
And water white transparency nano silver colloidal sol prepared by the present invention can overcome that above-mentioned particle diameter is big, particle diameter distribution is wide and carries coloured deficiency, have that particle diameter is little, narrow particle size distribution, an advantage such as colourless, the limitation carrying the application of silver field in weaving can be eliminated.
The colourless nano silver colloidal sol stability of cryogenic technique synthesis is more preferable than coloured nano silver colloidal sol prepared by prior art, existing coloured nano silver colloidal sol shelf-life is up to 2 years, the general shelf-life is 6-12 month, it is susceptible to layering, the phenomenon of sedimentation by the change of external environment, thus lose the stability of colloidal sol, and the present invention utilizes the colourless nano silver colloidal sol that cryogenic technique synthesizes, shelf-life is at least 3 years, the nano silver colloidal sol ice crystal preserved through 3 years, the effect that can reach freshly prepared nano silver colloidal sol compounding with other raw material after thawing.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in this, within bright protection domain.
Claims (7)
1. one kind utilizes cryogenic technique preparation and the method preserving colourless nano silver colloidal sol, it is characterised in that
Comprise the following steps:
1) silver material will be contained to be added to the water, mix homogeneously, obtain the aqueous solution containing silver material, freezing, powder
Broken, obtain the Sorbet containing silver material；
2) reducing agent is added to the water, mix homogeneously, obtains the aqueous solution containing reducing agent, freezing,
Pulverize, obtain the Sorbet containing reducing agent；
3) step 1) Sorbet containing silver material that obtains and step 2) obtain the Sorbet mixing containing reducing agent,
Grinding, described milling time is 12-48h, and grind size is 0.1-0.3 μm, and temperature during grinding is
-15 DEG C to-18 DEG C, obtain nanometer silver ice crystal；
4) step 3 is preserved) the nanometer silver ice crystal that obtains.
A kind of utilize cryogenic technique preparation and preserve colourless nano silver colloidal sol
Method, it is characterised in that step 1) in, described is silver nitrate containing silver material；Described silver nitrate aqueous solution
The molar concentration of middle silver nitrate is 0.1-0.5mol/L.
A kind of utilize cryogenic technique preparation and preserve colourless nano silver colloidal sol
Method, it is characterised in that step 2) in, in the described aqueous solution containing reducing agent, reducing agent is mole dense
Degree is 0.1-0.5mol/L.
A kind of utilize cryogenic technique preparation and preserve colourless nano silver colloidal sol
Method, it is characterised in that step 2) in, described reducing agent is in hydrogen peroxide, ascorbic acid or hydrazine hydrate
One or more.
A kind of utilize cryogenic technique preparation and preserve colourless nano silver colloidal sol
Method, it is characterised in that in molal quantity silver-colored in the described Sorbet containing silver material and described reducing agent Sorbet
The mole ratio of reducing agent is 4:3 to 2:1.
6. utilize cryogenic technique preparation according to one described in any one of claim 1 to 5 and preserve colourless receiving
The method of rice silver sol, it is characterised in that step 1) and step 2) in, described cryogenic temperature is-4 DEG C
To-24 DEG C, cooling time 8-24h；Described grinding particle size is 1-3 μm, and temperature during pulverizing is-15 DEG C
To-18 DEG C.
7. utilize cryogenic technique preparation according to one described in any one of claim 1 to 5 and preserve colourless receiving
The method of rice silver sol, it is characterised in that step 4) in, described preservation condition is-4 DEG C to-24 DEG C.
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| CN101384388A (en) * | 2006-03-10 | 2009-03-11 | 三井金属矿业株式会社 | Process for production of ultrafine silver particles and ultrafine silver particles produced by the process |
| RU2451578C1 (en) * | 2010-11-30 | 2012-05-27 | Общество с ограниченной ответственностью Научно Производственный Центр "Квадра" | Method of producing biocide inorganic zinc oxide-based composite nanoparticles |
| CN102699341A (en) * | 2012-04-26 | 2012-10-03 | 蔡雄辉 | Wet-chemical preparation method for silver micro/nanowires |
| CN103302307A (en) * | 2013-06-25 | 2013-09-18 | 通化师范学院 | Preparation method of silver nano particles and method for facilitating germination of cucumber seeds and growth and development of seedlings with silver nano particles |
| CN103567431A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer silver colloid solution and preparation method thereof |
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| KR101406588B1 (en) * | 2012-09-21 | 2014-06-11 | 제주대학교 산학협력단 | Method for preparing linear metal nanoparticles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101384388A (en) * | 2006-03-10 | 2009-03-11 | 三井金属矿业株式会社 | Process for production of ultrafine silver particles and ultrafine silver particles produced by the process |
| RU2451578C1 (en) * | 2010-11-30 | 2012-05-27 | Общество с ограниченной ответственностью Научно Производственный Центр "Квадра" | Method of producing biocide inorganic zinc oxide-based composite nanoparticles |
| CN102699341A (en) * | 2012-04-26 | 2012-10-03 | 蔡雄辉 | Wet-chemical preparation method for silver micro/nanowires |
| CN103567431A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer silver colloid solution and preparation method thereof |
| CN103302307A (en) * | 2013-06-25 | 2013-09-18 | 通化师范学院 | Preparation method of silver nano particles and method for facilitating germination of cucumber seeds and growth and development of seedlings with silver nano particles |
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Denomination of invention: A method of preparing and preserving colorless nano silver sol by low temperature technology Effective date of registration: 20221111 Granted publication date: 20160824 Pledgee: Yantai Fushan huiran Private Capital Management Co.,Ltd. Pledgor: YANTAI JIALONG NANO INDUSTRY CO.,LTD. Registration number: Y2022980021675 |