CN101856726B - Method for preparing multifunctional nano silver solution - Google Patents
Method for preparing multifunctional nano silver solution Download PDFInfo
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- CN101856726B CN101856726B CN201010201949XA CN201010201949A CN101856726B CN 101856726 B CN101856726 B CN 101856726B CN 201010201949X A CN201010201949X A CN 201010201949XA CN 201010201949 A CN201010201949 A CN 201010201949A CN 101856726 B CN101856726 B CN 101856726B
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Abstract
The invention discloses a method for preparing a multifunctional nano silver solution. A nano silver solution with the grain diameter of 20-100nm is carried by utilizing a surface modified tourmaline particle. The preparation method has simple process, mild reaction condition and lower preparation cost and meanwhile has the characteristics of broad-spectrum antibacterial property, anion release performance, favorable water absorptivity, and the like. The invention can be widely applied to a hygienic product and an appliance for daily life.
Description
Technical field
The present invention is a kind of have multifunctional nano silver solution manufacturing method and application.
Background technology
Silver has broad spectrum antibacterial.The silver of trace just has the ability of kill bacteria in solution.Silver ion can pass through the respiratory enzyme system of blocking-up bacterium, thereby the interfere with bacterial metabolism causes bacterial death, applies but the unstability of silver ion in solution limits it.Nano Silver is that argent is processed into nano-scale particle, thereby makes the sterilizing ability of silver produce qualitative leap, under the concentration of a few millionths, can kill pathogenic microorganisms such as common bacterium, fungi, mycoplasma, Chlamydia.Utilize the Nano Silver of nanometer technology preparation, have stable chemical characteristic, have very excellent characteristic at aspects such as electricity, optics and catalysis.Nano Silver has been widely used in the preparation of anti-biotic material at present, has occurred anti-bacteria ceramic material, antibiotic paint and antibiotic fabric etc. on the market.But synthetic Nano Silver major part is a powdery, has increased practical problems such as ultra-fine efflorescence, equipment reinvestment, energy consumption, cost is improved greatly, but also influenced ecological environment.The general production method that adopts is chemical precipitation method, solvent-thermal method, vapor phase method etc., and its production technology is difficult to control, yield poorly, and investment is big.
Summary of the invention
The objective of the invention is to overcome above-mentioned technical deficiency, a kind of preparation method of multifunctional nano silver solution is provided.Not only have low, the simple operation and other advantages of cost, and Nano silver solution has broad spectrum antibacterial, discharges anion and good wetting characteristics.Nano silver solution of the present invention has no side effect, and has stability preferably.
The objective of the invention is to realize by following step preparation:
(a) take by weighing solid nitric acid silver 5～25g and be dissolved in the deionized water, drip 1～30% ammoniacal liquor and disappear to deposition, the gained complex solution is labeled as component A, and wherein silver nitrate concentration is 0.01～0.3mol/l, and the concentration of ammonia is 0.2～1mol/l;
(b) select the micron order tourmaline powder for use, particle diameter adds dispersant at 0.2～2 μ m; Obtain suspension, leave standstill 5～24h after, get supernatant liquor; Add surface modifier; Make its micron tourmaline surface connect hydrophilic radical, obtain B component solution, wherein the weight ratio of tourmaline particle, dispersant and surface modifier is 4.3～9: 5～10: 10～20;
(c) complex solution A is joined in the B solution, the volume ratio of solution B and solution A is 1: 1.4～1: 10, under 20～45 ℃, stirs 1～6h, makes silver ammino ion be adsorbed on the tourmaline surface, obtains suspension;
(d) suspension that step (c) is obtained adds reducing agent, and its concentration is 0.04～1mol/l; Under 70～90 ℃; Continue 2～7h and obtain nano silver colloidal sol C, the lip-deep silver ammino ion of modification this moment micron order tourmaline is reduced into Nano Silver, its particle diameter 20～100nm;
(e) in nano silver colloidal sol C component, add a certain amount of deionized water, the volume ratio of C component and deionized water is 1: 70～1: 200, suspends, and leaves standstill, and gets supernatant liquor, thereby obtains multifunctional nano silver solution.The concentration of Nano Silver is at 500～2000nm in the Nano silver solution that obtains.Dispersant is deionized water, triethanolamine, tween.Reducing agent is citric acid, potassium borohydride, sodium sulfite, natrium citricum.Surface modifier is the surfactant that contains hydrophilic radical, is neopelex, SDS.Described micron order tourmaline powder can commercially availablely obtain.
Solution of the present invention contains the micron order tourmaline that is loaded with Nano Silver, thereby when having antibacterial action, has also kept the characteristics that tourmaline had, as discharging anion, far infrared radiation etc.Tourmaline has hydrophilic radical through surface modification, thereby increases the characteristic of suction.
Multifunctional nano silver solution of the present invention can be handled fabrics such as underwear, sanitary napkin, panty liner, tapon, wet towel, paper diaper, paper urine pad, shoe-pad, towel, mouth masks; Fabric after the processing not only has the broad-spectrum antiseptic function, and has excellent wetting capacity.For example, the application aspect sanitary napkin can be played antibiotic effect, can discharge anion again simultaneously, because the hydrophilic group exists in the solution, thereby has good water imbibition, has increased the permeability of sanitary napkin.
The specific embodiment
Case study on implementation 1
Silver nitrate 6g is dissolved in the 500ml deionized water, and Dropwise 5 % ammoniacal liquor disappears to deposition becomes complex solution, and the concentration of silver nitrate is about 0.07mol/l among the gained complex solution A, and the concentration of ammonia is 0.6mol/l.With the 5g particle diameter is that 1～2 μ m tourmaline powder adds the 200ml deionized water and obtains suspension, leave standstill 24h after.Get supernatant liquor, add also abundant stirring of 17g neopelex and obtain B component, wherein the weight ratio of tourmaline particle, deionized water and neopelex is 5: 10: 13.Complex solution A is joined in the B solution, and the volume ratio of solution B and solution A is 1: 2, stirs 3h down at 30 ℃, obtains suspension.Add the 0.1g citric acid, the concentration of citric acid is 0.07mol/l, is warming up to 90 ℃, keeps temperature 3h to obtain nano silver colloidal sol component C, and the lip-deep silver ammino ion of modification this moment micron order tourmaline is reduced into Nano Silver, its particle diameter of Nano Silver 20～50nm.In C, add a certain amount of deionized water, the volume ratio of C component and deionized water is 1: 200, suspends, and leaves standstill, and gets supernatant liquor, obtains multifunctional nano silver solution, and wherein the concentration of Nano Silver is 1000ppm.
Case study on implementation 2
Silver nitrate 9g is dissolved in the 500ml deionized water, and dripping the disappearance of 7.5% ammoniacal liquor to deposition becomes complex solution, and the concentration of silver nitrate is about 0.1mol/l among the gained complex solution A, and the concentration of ammonia is 0.8mol/l.With the 7g particle diameter is that 1～2 μ m tourmaline powder adds the 150ml triethanolamine and obtains suspension, leave standstill 18h after.Get supernatant liquor, add also abundant stirring of 9g SDS and obtain B component, wherein the weight ratio of tourmaline particle, triethanolamine and neopelex is 7: 6: 11.Complex solution A is joined in the B solution, and the volume ratio of solution B and solution A is 1: 4, stirs 6h down at 45 ℃, obtains suspension.Add the 0.2g natrium citricum, the concentration of natrium citricum is 0.16mol/l, is warming up to 75 ℃, keeps temperature 2h to obtain nano silver colloidal sol component C, and the lip-deep silver ammino ion of modification this moment micron order tourmaline is reduced into Nano Silver, Nano Silver particle diameter 20～90nm.The volume ratio that in C, adds a certain amount of deionized water C component and deionized water is 1: 100, suspends, and leaves standstill, and gets supernatant liquor, obtains multifunctional nano silver solution, and wherein the concentration of Nano Silver is 700ppm.
Case study on implementation 3
Silver nitrate 12g is dissolved in the 500ml deionized water, drips 20% ammoniacal liquor to deposition and disappear and to become the concentration of silver nitrate among the complex solution gained complex solution A and be about 0.2mol/l, the concentration of ammonia is 0.95mol/l.With the 9g particle diameter is that 0.2～1 μ m tourmaline powder adds after the 150ml tween obtains suspension and leave standstill 24h.Get supernatant liquor, add also abundant stirring of 6g SDS and obtain B component, wherein the weight ratio of tourmaline particle, tween and lauryl sodium sulfate is 7: 7: 10.Complex solution A is joined in the B solution, and the volume ratio of solution B and solution A is 1: 6, stirs 4h down at 20 ℃, obtains suspension.Add potassium borohydride 0.15g; The concentration of potassium borohydride is 0.56mol/l, is warming up to 70 ℃, keeps temperature 2h to obtain nano silver colloidal sol component C; The lip-deep silver ammino ion of modification this moment micron order tourmaline is reduced into Nano Silver, Nano Silver particle diameter 50～100nm.In C, add a certain amount of deionized water, the volume ratio of C component and deionized water is 1: 100, and suspension is left standstill, and gets supernatant liquor, obtain multifunctional nano silver solution wherein the concentration of Nano Silver be 1600ppm.
Case study on implementation 4
Silver nitrate 20g is dissolved in the 500ml deionized water, and Dropwise 5 % ammoniacal liquor disappears to deposition becomes complex solution, and the concentration of silver nitrate is 0.3mol/l among the gained complex solution A, and the concentration of ammonia is 1mol/l.With the 9g particle diameter is that 0.2～1 μ m tourmaline powder adds the 150ml deionized water and obtains suspension, leave standstill 8h after.Get supernatant liquor, add also abundant stirring of 15g neopelex and obtain B component, wherein the weight ratio of tourmaline particle, deionized water and neopelex is 9: 10: 16.Complex solution A is joined in the B solution, and the volume ratio of solution B and solution A is 9: 1, stirs 4h down at 40 ℃, obtains suspension.Add the 0.15g sodium sulfite, the concentration of sodium sulfite is 0.76mol/l, is warming up to 80 ℃, keeps temperature 7h to obtain nano silver colloidal sol component C, and the lip-deep silver ammino ion of modification this moment micron order tourmaline is reduced into Nano Silver, its particle diameter 30～80nm.In C, add a certain amount of deionized water, the volume ratio of C component and deionized water is 1: 70, suspends, and leaves standstill, and gets supernatant liquor, obtains multifunctional nano silver solution, and wherein the concentration of Nano Silver is 500ppm.
Case study on implementation 1～4 remembered respectively be A1～A4, white cotton is immersed in the above-mentioned solution dry naturally behind the 1h.Carry out the bactericidal property test, method of testing all adopts the textile industry standard FZ/T3023 of the People's Republic of China (PRC)～2006.Above-mentioned national FZ/T3023～2006 standards that all reach.This solution also has characteristics such as the anion of release, good water imbibition in addition.
Claims (3)
1. the preparation method of a multifunctional nano silver solution is characterized in that:
(a) take by weighing solid nitric acid silver 5～25g and be dissolved in the deionized water, drip 1～30% ammoniacal liquor and disappear to deposition, the gained complex solution is labeled as component A, and wherein silver nitrate concentration is 0.01～0.3mol/l, and the concentration of ammonia is 0.2～1mol/l;
(b) select the micron order tourmaline powder for use, particle diameter adds dispersant at 0.2～2 μ m; Obtain suspension, leave standstill 5～24h after, get supernatant liquor; Add surface modifier; Make its micron tourmaline surface connect hydrophilic radical, obtain B component solution, wherein the weight ratio of tourmaline particle, dispersant and surface modifier is 4.3～9: 5～10: 10～20; Said dispersant is deionized water, triethanolamine or tween; Said surface modifier is neopelex or SDS;
(c) complex solution A is joined in the B solution, the volume ratio of solution B and solution A is 1: 1.4～1: 10, under 20～45 ℃, stirs 1～6h, makes silver ammino ion be adsorbed on the tourmaline surface, obtains suspension;
(d) suspension that step (c) is obtained adds reducing agent, and its concentration is 0.04～1mol/l; Under 70～90 ℃; Continue 2～7h and obtain nano silver colloidal sol C, the lip-deep silver ammino ion of modification this moment micron order tourmaline is reduced into Nano Silver, its particle diameter 20～100nm;
(e) in nano silver colloidal sol C component, add a certain amount of deionized water, the volume ratio of C component and deionized water is 1: 70～1: 200, suspends, and leaves standstill, and gets supernatant liquor, thereby obtains multifunctional nano silver solution.
2. according to the preparation method of the said multifunctional nano silver solution of claim 1, it is characterized in that: the concentration of Nano Silver is at 500～2000ppm in the Nano silver solution that obtains.
3. the preparation method of multifunctional nano silver solution according to claim 1, it is characterized in that: reducing agent is citric acid, potassium borohydride, sodium sulfite or natrium citricum.
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| JP5344099B2 (en) * | 2011-06-16 | 2013-11-20 | 住友金属鉱山株式会社 | Silver powder and method for producing the same |
| CN103722181B (en) * | 2014-01-21 | 2016-01-20 | 江苏欧耐尔新型材料有限公司 | Liquid phase reduction uses dispersant to prepare the method for nano-silver powder |
| CN105108169A (en) * | 2015-09-09 | 2015-12-02 | 深圳市芭田生态工程股份有限公司 | Antibacterial agent used for fertilizer and application thereof |
| CN106149351B (en) * | 2016-07-15 | 2018-08-24 | 浙江健盛集团江山针织有限公司 | Oxidation-reduction method prepares the method and its anti-bacterial fibre of multivalent state silver system anti-bacterial fibre |
| CN111387585A (en) * | 2020-02-18 | 2020-07-10 | 安徽姆大陆科技发展有限公司 | Medical mask containing last-in silver/negative oxygen ions and production method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1470682A (en) * | 2002-07-26 | 2004-01-28 | 上海弘康科技发展有限公司 | Method for preparing fiber with negative ion far infrared antibacterial health-care function and product thereof |
| CN1653907A (en) * | 2005-01-27 | 2005-08-17 | 浙江大学 | Method for preparing nanometer silver solution and nanometer silver powder by using high polymer as stabilizer |
| CN1765369A (en) * | 2004-10-25 | 2006-05-03 | 陈添水 | Nano silver gel and its use |
| CN1888158A (en) * | 2005-06-30 | 2007-01-03 | 上海弘康科技发展有限公司 | Far infrared antiseptic health care fiber with anion and producing method thereof |
| CN101722313A (en) * | 2009-12-16 | 2010-06-09 | 蒋伟平 | Nanometer silver solution, method for preparing same and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470682A (en) * | 2002-07-26 | 2004-01-28 | 上海弘康科技发展有限公司 | Method for preparing fiber with negative ion far infrared antibacterial health-care function and product thereof |
| CN1765369A (en) * | 2004-10-25 | 2006-05-03 | 陈添水 | Nano silver gel and its use |
| CN1653907A (en) * | 2005-01-27 | 2005-08-17 | 浙江大学 | Method for preparing nanometer silver solution and nanometer silver powder by using high polymer as stabilizer |
| CN1888158A (en) * | 2005-06-30 | 2007-01-03 | 上海弘康科技发展有限公司 | Far infrared antiseptic health care fiber with anion and producing method thereof |
| CN101722313A (en) * | 2009-12-16 | 2010-06-09 | 蒋伟平 | Nanometer silver solution, method for preparing same and application thereof |
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Effective date of registration: 20160316 Address after: 133700 Jilin city in Dunhua Province, South Ring Road No. 121 Dade Park building eleven No. 1105 hit off Patentee after: Dunhua city picometers drug development limited liability company Address before: 150030 No. 1, Jinxing street, Xiangfang District, Harbin District, Heilongjiang Patentee before: Harbin Deyi Pharmaceutical Co., Ltd. |
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