CN1565976A - Nano-class silver oxide and preparation method thereof - Google Patents
Nano-class silver oxide and preparation method thereof Download PDFInfo
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- CN1565976A CN1565976A CN 03142646 CN03142646A CN1565976A CN 1565976 A CN1565976 A CN 1565976A CN 03142646 CN03142646 CN 03142646 CN 03142646 A CN03142646 A CN 03142646A CN 1565976 A CN1565976 A CN 1565976A
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Abstract
The invention relates to a nano-class silver oxide and preparation method thereof which comprises, using dual injection control technology, stirring through a stirrer, charging silver nitrate water solution and sodium-hydroxide water solution simultaneously into reaction system containing protective agent water solution, obtaining silver oxide particles and performing cooling down, filtering, washing and drying.
Description
Technical field
The present invention relates to nanometer level silver oxide and preparation method thereof.
Background technology
Silver suboxide is widely used in industries such as electronic devices and components, button cell, sanitas, scavenging agent, glass colorant, abrasive and chemical catalyst.Have 30% silver to be used for silver suboxide or Silver Nitrate production in the industrial silver, wherein the silver suboxide that consumed of electronic devices and components industry accounts for 90% of silver suboxide ultimate production.At present, the production of state's internal oxidized Ag is mainly adopted silver nitrate solution is added drop-wise to method in the sodium hydroxide solution, obtain the silver suboxide post precipitation, obtain the silver suboxide finished product through washing, separation and drying, but the particle diameter of product is difficult to satisfy the Application Areas requirement the smaller the better to the silver oxide particle degree generally in the micron order size.
Chinese patent CN1308102A discloses a kind of silver suboxide and production technique thereof.This method is that Silver Nitrate is made silver ammino solution, under agitation joins gradually to contain in protectant aqueous sodium hydroxide solution, promptly generates nano phase ag_2 o, and its median size is between 80～100 nanometers.But this method is used ammoniacal liquor in a large number, and the production scene needs the air draft explosion-proof equipment, and is having under the condition of ammonia, and the possibility that generates silver azide is arranged in the reaction system, and this matter-pole explosive belongs to hazardous substance.
What above preparation method used all is single dropping methods of annotating.For realization response thing lower concentration is participated in reaction, usually adopt the mode that drips at a slow speed, though this has reduced wherein a kind of concentration of reactants to a certain extent, help reducing the speed of growth of silver suboxide particle, but two kinds of reactants are all reacted with lower concentration, can not maximum amplitude ground reduce the speed of growth of particle, and lack the auxiliary reactant concn problem that solves of corresponding corollary apparatus, finally cause the particle that generates bigger.In a word, above preparation method's production cycle is long, product particle is bigger, is also needing further improvement aspect preparation technology and the preparation facilities.
Summary of the invention
The purpose of this invention is to provide a kind of nanometer level silver oxide and preparation method thereof, the silver oxide particle that this method obtains is stable, good dispersity, particle diameter is little and be evenly distributed.
Technical scheme of the present invention is: a kind of preparation method of nanometer level silver oxide; it is characterized in that; adopt double injecting control technology; under the stirring of agitator; silver nitrate aqueous solution and two simultaneously injection of aqueous sodium hydroxide solution are contained in the reaction system of the protective material aqueous solution; generate the silver suboxide particle, through cooling, filtration, washing and dry, obtaining median size is the silver suboxide particle of 10～30 nanometers.
A kind of preferred version, wherein said protective material are polyvinylpyrrolidone or polyvinyl alcohol.
A kind of preferred version, wherein said agitator are the rotor-stator agitators.
A kind of preferred version, wherein said agitator are that the patent No. is the agitator of ZL01278630.6.
The preparation of silver suboxide is a kind of quick moment precipitin reaction, and the generation of particle has comprised the generation of nucleus and two stages of growth of nucleus.In order to obtain the particle that particle diameter is little and be evenly distributed, need long nucleation period and relative of short duration growth stage during reaction.
The preparation method of nanometer level silver oxide of the present invention; be to adopt double injecting control technology; under the stirring of agitator; silver nitrate aqueous solution and two simultaneously injection of aqueous sodium hydroxide solution are contained in the reaction system of the protective material aqueous solution; generate the silver suboxide particle; through cooling, filtration, washing and dry, obtaining median size is the silver suboxide particle of 10～30 nanometers.
Among the present invention, the reaction system before the beginning is for containing protectant weak alkaline aqueous solution, the PH=8 of its aqueous solution～10, and protective material wherein is polyvinylpyrrolidone or polyvinyl alcohol; This reaction system also is furnished with agitator, and this agitator is that pre-dilution function, rotor-stator agitator that mixed performance is good are arranged.Under the turning effort of agitator rotor high-speed, silver nitrate aqueous solution and aqueous sodium hydroxide solution inject in the agitator stator simultaneously by filling tube, and respectively with the water-soluble liquid-phase mixing of a large amount of systems, thereby make reaction density obtain the dilution.Afterwards, the Silver Nitrate of lower concentration and sodium hydroxide meet in the stator exit, and the rapid precipitation reaction takes place, because reactant concn is very low, thereby the silver suboxide particle that generates is tiny.Protective material protects the silver suboxide that generates simultaneously, finally makes the little nanoparticle of particle diameter.Reaction finishes after scouring and drying, obtains stability and good dispersity, granularity is little and the nano oxidized silver particles of distribution uniform.
Preparation method of the present invention, owing to adopt double injecting control technology and pre-dilution function, rotor-stator agitator that mixed performance is good arranged, can under the bigger situation of higher, the two beam amount of dosing concentration, still realize the lower concentration reaction, and finally obtain the little nanoparticle of particle diameter, production cycle is obviously shortened, and cost is low, yield is high, is more suitable for suitability for industrialized production.
Double injecting control technology of the present invention is the double injecting control technology that adopts in the emulsion preparation, and this technology is disclosed in the U.S. Pat 4439215.
In the preparation process of nano phase ag_2 o, the effect of agitator is extremely important, and suitable agitator of the present invention is the rotor-stator agitator, and the wherein preferred patent No. is the agitator of ZL01278630.6.
Specific practice is:
200～500 parts of Silver Nitrates (quality, down together) are dissolved in 960～900 parts of pure water, are made into silver nitrate solution; 55～130 parts of solid sodium hydroxides are dissolved in 990～970 parts of pure water, are made into sodium hydroxide solution; In reactor 2～10 parts of protective materials being added pure water is made into the reaction system aqueous solution for 1200 parts in addition, and regulates the pH value between 8～10 with sodium hydroxide.The rotor-stator agitator is housed in the reactor.This agitator is made up of stator and rotor, when agitator turns round, aqueous solution liquid in a large amount of systems is inhaled into the inner chamber of agitator, simultaneously silver nitrate solution and sodium hydroxide solution enter the agitator stator interior by opening for feed respectively by filling tube, thus reactant at inner chamber respectively by system aqueous solution, dilution.Afterwards, the Silver Nitrate and the sodium hydroxide of lower concentration meet in the exit, and the rapid precipitation reaction takes place, and moment generates the silver suboxide particle.Among this preparation method, mixing speed is 2000～2500rpm, and two liquid are at the uniform velocity two to be annotated 10～60 minutes.Two notes finish the back and continued ripe 20～60 minutes, and through cooling, sedimentation filters out silver suboxide then.Product washs to pH=7～8 with pure water, filters with absolute ethanol washing again, vacuum drying oven inner drying 4 hours, promptly gets nano phase ag_2 o under 80 ℃.
Adopting the nano phase ag_2 o color of the inventive method preparation is chocolate, and median size is 10～30 nanometers, and product content is greater than 99.5%, and yield is more than 99%, and stability and favorable dispersity.
Beneficial effect
The nano phase ag_2 o particle that adopts the inventive method to obtain, granularity is little, distribution uniform, stability and good dispersity; The inventive method level of automation height, with short production cycle, cost is low, yield is high, is applicable to suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
Silver Nitrate 200 grams are dissolved in 960 ml pure waters, are made into silver nitrate solution; 55 gram solid sodium hydroxides are dissolved in 990 ml pure waters, are made into sodium hydroxide solution; In addition protective material polyvinylpyrrolidone 2 grams are added pure water and are made into mother liquor for 1200 milliliters, and with sodium hydroxide adjust pH=8, in set rotor agitator (patent No. is ZL01278630.6).Silver nitrate solution and sodium hydroxide solution enter the agitator stator interior by opening for feed up and down respectively by filling tube, and obtain dilution in stator interior, two kinds of reaction solution contact reactss when throwing away stator then, and moment generates the silver suboxide particle.Mixing speed is 2000rpm, and two liquid are at the uniform velocity two to be annotated 60 minutes.Two notes finish the back and continued ripe 20 minutes, and cooling, filters out silver suboxide at sedimentation.Product washs to pH=7～8 with pure water, filters with absolute ethanol washing again, the vacuum drying oven inner drying of 80 ℃ of temperature 4 hours, promptly gets nano phase ag_2 o.The nanometer level silver oxide particle diameter of this method preparation is about 5～15 nanometers.
Embodiment 2
Silver Nitrate 500 grams are dissolved in 900 ml pure waters, are made into silver nitrate solution; 130 gram solid sodium hydroxides are dissolved in 970 ml pure waters, are made into sodium hydroxide solution; In addition protective material polyvinylpyrrolidone 10 grams are added pure water and are made into mother liquor for 1200 milliliters, and with sodium hydroxide adjust pH=10, in set rotor agitator (patent No. is ZL01278630.6).Silver nitrate solution and sodium hydroxide solution enter the agitator stator interior by opening for feed up and down respectively by filling tube, and obtain dilution in stator interior, two kinds of reaction solution contact reactss when throwing away stator then, and moment generates the silver suboxide particle.Mixing speed is 2500rpm, and two liquid are at the uniform velocity two to be annotated 20 minutes.Two notes finish the back and continued ripe 60 minutes, and cooling, filters out silver suboxide at sedimentation.Product washs to pH=7～8 with pure water, filters with absolute ethanol washing again, the vacuum drying oven inner drying of 80 ℃ of temperature 4 hours, promptly gets nano phase ag_2 o.The nanometer level silver oxide particle diameter of this method preparation is in 10～30 nanometers.
Embodiment 3
Silver Nitrate 350 grams are dissolved in 930 ml pure waters, are made into silver nitrate solution; 93 gram solid sodium hydroxides are dissolved in 980 ml pure waters, are made into sodium hydroxide solution; In addition protective material polyvinyl alcohol 5 grams are added pure water and are made into mother liquor for 1200 milliliters, and with sodium hydroxide adjust pH=9, in set rotor agitator (patent No. is ZL01278631.4).Silver nitrate solution and sodium hydroxide solution enter the agitator stator interior respectively by filling tube, and obtain dilution in stator interior, two kinds of reaction solution contact reactss then, and moment generates the silver suboxide particle.Mixing speed is 2200rpm, and two liquid are at the uniform velocity two to be annotated 10 minutes.Two notes finish the back and continued ripe 40 minutes, and cooling, filters out silver suboxide at sedimentation.Product washs to pH=7～8 with pure water, filters with absolute ethanol washing again, the vacuum drying oven inner drying of 80 ℃ of temperature 4 hours, promptly gets nano phase ag_2 o.The nanometer level silver oxide particle diameter of this method preparation is in 10～30 nanometers.
Claims (4)
1. the preparation method of a nanometer level silver oxide; it is characterized in that adopting double injecting control technology; under the stirring of agitator; silver nitrate aqueous solution and two simultaneously injection of aqueous sodium hydroxide solution are contained in the reaction system of the protective material aqueous solution; generate the silver suboxide particle; through cooling, filtration, washing and dry, obtaining median size is the silver suboxide particle of 10～30 nanometers.
2. the preparation method of nanometer level silver oxide according to claim 1 is characterized in that, described protective material is polyvinylpyrrolidone or polyvinyl alcohol.
3. the preparation method of nanometer level silver oxide according to claim 1 is characterized in that, described agitator is the rotor-stator agitator.
4. the preparation method of nanometer level silver oxide according to claim 3 is characterized in that, described agitator is that the patent No. is the agitator of ZL01278630.6.
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| CN 03142646 CN1280198C (en) | 2003-06-10 | 2003-06-10 | Nano-class silver oxide and preparation method thereof |
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| CN 03142646 CN1280198C (en) | 2003-06-10 | 2003-06-10 | Nano-class silver oxide and preparation method thereof |
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| CN1565976A true CN1565976A (en) | 2005-01-19 |
| CN1280198C CN1280198C (en) | 2006-10-18 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259905A (en) * | 2010-05-26 | 2011-11-30 | 昆明其化新材料科技有限公司 | Preparation method of superfine silver oxide |
| CN104787795A (en) * | 2015-04-14 | 2015-07-22 | 东华理工大学 | Method for preparing micro silver oxide |
| CN107051432A (en) * | 2017-04-21 | 2017-08-18 | 滨州学院 | A kind of preparation method of photochemical catalyst and the equipment suitable for the preparation method |
| CN107603493A (en) * | 2017-08-31 | 2018-01-19 | 兰溪市拜瑞珂科技服务有限公司 | A kind of fungi-proofing light maintaining agent of fur clothing and preparation method thereof |
| CN107938100A (en) * | 2017-11-07 | 2018-04-20 | 海盐县硕创服装研究所 | A kind of processing technology of the soft anti-denim that fades |
| CN114671455A (en) * | 2022-03-03 | 2022-06-28 | 先导薄膜材料（广东）有限公司 | Method for industrially producing silver oxide for battery |
-
2003
- 2003-06-10 CN CN 03142646 patent/CN1280198C/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102259905A (en) * | 2010-05-26 | 2011-11-30 | 昆明其化新材料科技有限公司 | Preparation method of superfine silver oxide |
| CN104787795A (en) * | 2015-04-14 | 2015-07-22 | 东华理工大学 | Method for preparing micro silver oxide |
| CN104787795B (en) * | 2015-04-14 | 2016-08-31 | 东华理工大学 | A kind of method preparing micron silver oxide |
| CN107051432A (en) * | 2017-04-21 | 2017-08-18 | 滨州学院 | A kind of preparation method of photochemical catalyst and the equipment suitable for the preparation method |
| CN107603493A (en) * | 2017-08-31 | 2018-01-19 | 兰溪市拜瑞珂科技服务有限公司 | A kind of fungi-proofing light maintaining agent of fur clothing and preparation method thereof |
| CN107938100A (en) * | 2017-11-07 | 2018-04-20 | 海盐县硕创服装研究所 | A kind of processing technology of the soft anti-denim that fades |
| CN114671455A (en) * | 2022-03-03 | 2022-06-28 | 先导薄膜材料（广东）有限公司 | Method for industrially producing silver oxide for battery |
| CN114671455B (en) * | 2022-03-03 | 2023-10-17 | 先导薄膜材料（广东）有限公司 | Method for industrially producing silver oxide for battery |
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| CN1280198C (en) | 2006-10-18 |
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Owner name: CHINA LUCKY GROUP CORPORATION Free format text: FORMER NAME: CHINESE LEKAI FILM GROUP CO |
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Address after: South Street, new urban lucky 071054 Hebei province Baoding City No. 6 Patentee after: CHINA LUCKY Group Corp. Address before: 071054 No. 1 Jianshe South Road, Hebei, Baoding Patentee before: CHINA LUCKY FILM Group Corp. |
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Granted publication date: 20061018 |