CN101999409A - Nano silver-zinc complex antibacterial disinfectant and preparation method thereof - Google Patents
Nano silver-zinc complex antibacterial disinfectant and preparation method thereof Download PDFInfo
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- CN101999409A CN101999409A CN2010102977732A CN201010297773A CN101999409A CN 101999409 A CN101999409 A CN 101999409A CN 2010102977732 A CN2010102977732 A CN 2010102977732A CN 201010297773 A CN201010297773 A CN 201010297773A CN 101999409 A CN101999409 A CN 101999409A
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Abstract
The invention discloses a nano silver-zinc complex antibacterial disinfectant and a preparation method thereof. The nano silver-zinc complex antibacterial disinfectant is prepared from the following components in percentage by weight: 0.008-0.49 percent of silver salt, 0.002-0.25 percent of reducing agent, 0.01-2.0 percent of zinc-contained nano carrier and 97.26-99.98 percent of water. The nano silver-zinc complex antibacterial disinfectant of the invention has high stability, high concentration of nano silver-zinc complex particles, small average particle diameter, neutral pH value and high antibacterial disinfecting performance.
Description
Technical field
The present invention relates to a kind of antimicrobial fluid and preparation method thereof, especially relate to a kind of Nano Silver zinc complex sterilizing disinfectant and preparation method thereof.
Background technology
Environment for human survival exists the microorganism of various harmful healths, and to the mankind's life generation harmful effect, studying various anti-biotic materials has become current heat subject.Anti-biotic material refers under the prerequisite that does not change original material traditional performance, safety and processing characteristics, gives material good antibacterial effect.The antibacterial ability of silver is very strong and have the bactericidal effect of wide spectrum, can not produce toxin in the human body accumulation again, just be used as the antibacterial activity material a long time ago.The nanometer-level silver particle has higher surface energy and more contact area, has higher antibacterial activity, and bacterium just loses activity 6 seconds after contacting with Nano Silver.The antibiotic and sterilizing ability of zinc is also very outstanding, and is the necessary element of human body.
In the third phase in 2005 " Jilin Normal University's journal " " synthesis characterization of dispersed nano silver sol and property research thereof ", a kind of synthetic method of nano silver colloidal sol is disclosed, this method is soluble in water sodium borohydride and trisodium citrate, under stirring fast, add liquor argenti nitratis ophthalmicus, obtain the Nano silver solution of pale brown look, obtain nano silver colloidal sol through centrifugal, washing, ultrasonic circulation again.Adopt the nano silver colloidal sol complex process of the method preparation, concentration of silver ions is low, and poor stability lost efficacy gradually with regard to producing more black precipitate after 3 months.
Chinese patent ZL200410069105.9 discloses a kind of preparation method of nano silver colloid aqueous solution; this method adopts double injecting control technology; under the stirring of agitator; silver-colored ammonia spirit and two simultaneously injection of the reductant aqueous solution are contained in the reaction system of the protectant aqueous solution; through the ultrafiltration desalination, obtain the nano silver colloid aqueous solution of average grain diameter less than 50nm.The equipment cost height of this method, complex process, it is the agitator of ZL01278630.6 that its agitator adopts the patent No., double injecting control technology adopts the double injecting control technology that adopts in the emulsion preparation in the U.S. Pat 4439215, and will be through complicated ultra-filtration process and desalination processes, will be by the ultrafiltration post under sizable pressure, and the Nano Silver average grain diameter that obtains at last is less than 50nm, do not reach the 20nm of industry acquiescence far away, and particle size distribution range broad, particle size is very inhomogeneous, and activity is lower, uses to be subjected to significant limitation.
Chinese patent ZL200510036375.4 discloses a kind of liquid nanometer simple substance silver antibacterial agent and preparation method, the employing running water has been proposed, silver sulfate, silver complexing agent and Nano Silver generate the method that agent prepares nano-silver water solution, the Nano silver solution cost of this method preparation is low, the concentration of silver ions height, but the production equipment poor-performing that uses, the highest 600～the 800r/min that only reaches of mixing speed, therefore, the flow of wanting strict restriction Nano Silver to generate agent only is 0.5～1.0L/min, otherwise can cause product cut size excessive even precipitate, but the speed and the scale of suitability for industrialized production so, have just seriously been limited.Simultaneously, this method causes the pH value of Nano silver solution very low owing to used acid silver-colored complexing agent, is acid, and this has just caused product to have corrosivity, excitant, thereby has limited the product range of application greatly.
Summary of the invention
For addressing the above problem, the purpose of this invention is to provide a kind of good stability, concentration height, average grain diameter is little, pH value is neutral Nano Silver zinc complex sterilizing disinfectant and preparation method thereof.
For achieving the above object, the present invention adopts following technical scheme:
A kind of Nano Silver zinc complex sterilizing disinfectant, its by silver salt, reductant, contain the zinc nano-carrier and water formulated, the weight percent content of each component is: silver salt 0.008～0.49%, reductant 0.002～0.25%, contain zinc nano-carrier 0.01～2.0%, water 97.26～99.98%.
Described Nano Silver zinc complex sterilizing disinfectant, the percentage by weight of its Nano Silver zinc complex in Nano Silver zinc complex sterilizing disinfectant is 0.01～0.7%.
Described Nano Silver zinc complex sterilizing disinfectant, its Nano Silver zinc complex average particle size≤20nm.
Further, described Nano Silver zinc complex sterilizing disinfectant, its Nano Silver zinc complex average particle size≤18.6nm.
Described Nano Silver zinc complex sterilizing disinfectant, its silver salt are one or more the combination in silver nitrate, silver sulfate, the silver orthophosphate; Wherein, silver sulfate, silver orthophosphate need routinely that collocation method is configured to silver ammino solution, are that the mass ratio of 25% ammoniacal liquor is 1: 0.6～3.8 formation silver ammino solutions by silver salt and weight percent concentration.
Described Nano Silver zinc complex sterilizing disinfectant, its reductant are one or more the combination in sodium borohydride, potassium borohydride, trisodium citrate, hydrazine hydrate, the hydrogen peroxide.
Described Nano Silver zinc complex sterilizing disinfectant, it contains the zinc nano-carrier is LYZS-2 type water-soluble granular shape white powder.
Described Nano Silver zinc complex sterilizing disinfectant, described water are the running water of placing under deionized water or the room temperature 16～36 hours.
A kind of equipment for preparing Nano Silver zinc complex sterilizing disinfectant, it comprises reactor, batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine, reactor top is provided with charging aperture, the bottom is provided with discharging opening, discharging opening is equipped with the discharging valve, the batch (-type) high-shear emulsion machine is installed in reactor top, the emulsifying head of batch (-type) high-shear emulsion machine stretches into reactor inside, the pipeline high-shear emulsion machine is installed in the reactor outside, pipeline high-shear emulsion machine discharging opening is connected with reactor by pipeline, and charging aperture is connected with the discharging opening of reactor by pipeline.
A kind of preparation method of Nano Silver zinc complex sterilizing disinfectant, it comprises following concrete steps:
(1), in reactor, add under the deionized water of mass percent 15～70% or the room temperature and place 16～36 hours running water, the water of residual mass percentage is used for configuration and contains the zinc nano-carrier aqueous solution, silver salt solution, the reductant aqueous solution; Add and contain the zinc nano-carrier aqueous solution, the mass ratio that contains zinc nano-carrier and water is 1: 40～130; Under the mixed at high speed of batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine was sheared, dispersion and emulsion 6～20 minutes, fluid temperature remained on 5～25 ℃;
(2), in reactor, add silver salt solution, the mass ratio of silver salt and water is 1: 30～110, continues dispersion and emulsion 40～90 minutes;
(3), the speed of the reductant aqueous solution with 1.5～9.5kg/min is sprayed in the reactor, the mass ratio of reductant and water is 1: 50～250, continues dispersion and emulsion 30～60 minutes, can obtain Nano Silver zinc complex sterilizing disinfectant.
Among the preparation method of above-mentioned Nano Silver zinc complex sterilizing disinfectant, the speed of agitator of described batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine is 2000～3000rpm.
The available model of described batch (-type) high-shear emulsion machine has: GRW-401, GRW-405, GRW-410, GRW-415, GRW-425, GRW-430, GRW-405/3, GRW-410/3, GRW-415/3, GRW-425/3 or GRW-430/3.
The available model of described pipeline high-shear emulsion machine has: SA90, SA100, SA120, SA140, SA160, SA180 or SA200.
The batch (-type) high-shear emulsion machine of using among the present invention and the operation principle of pipeline high-shear emulsion machine are basic identical, the rotor and the close-fitting stator that all are high-speed motion suck material in the working cavity, make material bear strong mixing and shearing, reach the purpose of mixing, emulsification, dispersion, homogeneous.
The pipeline high-shear emulsion machine is the hgh-performance emulsified equipment that is used for continuity production or the meticulous material of circulation production processing, one or more sets commentaries on classics, stator structure is housed in its working cavity, thereby makes emulsifying effectiveness obtain the lifting of homogeneous.In addition, the pipeline high-shear emulsion machine has good conveying function, can realize continuous production, and can automation control, it is big to have treating capacity, and quick, efficient, energy-conservation, no dead angle, material 100% are by shearing, simple and easy to use, be fit to advantages such as the continuous production of industrialization.Above-mentioned advantage is most important for the high Nano Silver zinc complex sterilizing disinfectant of preparation stability.
It is the product of being produced by business ethics letter nano material Co., Ltd in the Luoyang that LYZS-2 type in the Nano Silver zinc complex sterilizing disinfectant of the present invention contains the zinc nano-carrier, is the water-soluble granular shape product that is exclusively used in the preparation nano material.
Because adopt aforesaid technical scheme, the present invention has following superiority:
The present invention has adopted batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine, and the LYZS-2 type contains the zinc nano-carrier, Nano Silver silver zinc complex particle concentration height in the Nano Silver zinc complex sterilizing disinfectant of preparation, particle diameter is little, pH value is 7.0 ± 1, good stability, room temperature following stabilization time 〉=2 years, the antibiotic and sterilizing performance is good.
Nano Silver zinc complex sterilizing disinfectant of the present invention can form the antibiotic and sterilizing material with the fabric strong bonded, fabric can be the cloth that processes of cotton, hair, chemical fibre, blending, line, and knit goods and bonded fabric product, is preferably clothing, mouth mask, isolation clothes, wet tissue, sheet; Can be used for making disinfectant, shampoo; Can be used for the sterilization of environment such as compartment, breed factory, medicine equipment, hospital ward, toilet.
Description of drawings
Fig. 1 is the structural representation of equipment of the Nano Silver zinc complex sterilizing disinfectant of preparation;
Fig. 2 is the transmission electron microscope photo of Nano Silver zinc complex particle of the present invention;
Among the figure: 1-batch (-type) high-shear emulsion machine; The 2-charging aperture; The 3-reactor; The 4-discharge pipe; 5-pipeline high-shear emulsion machine; The 6-feed pipe; The 7-discharging opening; 8-discharging valve.
Embodiment
Can be described in further detail the present invention with reference to following examples; But following examples only are illustrations, and the present invention is not limited to these embodiment.
As shown in Figure 1, the equipment of described preparation Nano Silver zinc complex sterilizing disinfectant, it comprises reactor 3, batch (-type) high-shear emulsion machine 1 and pipeline high-shear emulsion machine 5, reactor 3 tops are provided with charging aperture 2, the bottom is provided with discharging opening 7, discharging opening 7 is equipped with discharging valve 8, batch (-type) high-shear emulsion machine 1 is installed in reactor 3 tops, the emulsifying head of batch (-type) high-shear emulsion machine stretches into reactor inside, pipeline high-shear emulsion machine 5 is installed in reactor 3 outsides, pipeline high-shear emulsion machine 5 discharging openings are connected with reactor 3 tops by discharge pipe 4, and charging aperture is connected with the discharging opening 7 of reactor 3 by feed pipe 6.
Form pipeline/batch (-type) high shear combination mulser by GRW-401 type batch (-type) high-shear emulsion machine and SA90 type pipeline high-shear emulsion machine; Add the running water that 300kg places 24h from charging aperture 2, add again with 1.2kg LYZS-2 type and contain the 100kg aqueous solution of zinc nano-carrier preparation in reactor, start batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine, mulser rotating speed 2500rpm, 20 ℃ of reaction temperatures, dispersion and emulsion 8 minutes; Add the 120kg aqueous solution again, continued dispersion and emulsion 45 minutes with the preparation of 1.58kg silver nitrate; Get sodium borohydride 0.55kg, be dissolved in the 60kg deionized water, be made into the aqueous solution of reductant, speed with 8.1kg/min sprays into the reactor from charging aperture 2, continued emulsion reaction after having annotated again 40 minutes, and promptly obtained average grain diameter and be 0.19% Nano Silver zinc complex sterilizing disinfectant less than 18.6nm, stability 〉=two year, pH value 7.2, Nano Silver zinc complex percentage by weight.
Form pipeline/batch (-type) high shear combination mulser by GRW-405/3 type batch (-type) high-shear emulsion machine and SA100 type pipeline high-shear emulsion machine; Add the 150kg deionized water from charging aperture 2, add again contain the preparation of zinc nano-carrier with 3.5kg LYZS-2 type aqueous solution 300kg in reactor, startup batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine, mulser rotating speed 3000rpm, 15 ℃ of reaction temperatures, dispersion and emulsion 10 minutes; Add again with the 2.79kg silver orthophosphate and add the silver-colored ammonia spirit 110kg that 5kg 25% ammoniacal liquor and deionized water are made into, continuation dispersion and emulsion 50 minutes; Get potassium borohydride 0.5kg and trisodium citrate 0.6kg, be dissolved in the 245kg deionized water, be made into the aqueous solution of reductant, speed with 3.3kg/min sprays into the reactor from charging aperture 2, continued emulsion reaction after having annotated again 60 minutes, and promptly obtained average grain diameter and be 0.26% Nano Silver zinc complex sterilizing disinfectant less than 17.2nm, stability 〉=two year, pH value 7.6, Nano Silver zinc complex percentage by weight.
Form pipeline/batch (-type) high shear combination mulser by GRW-401 type batch (-type) high-shear emulsion machine and SA90 type pipeline high-shear emulsion machine; Add the 250kg deionized water from charging aperture 2, add again contain the preparation of zinc nano-carrier with 1.6kg LYZS-2 type the 180kg aqueous solution in reactor, startup batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine, mulser rotating speed 2300rpm, 25 ℃ of reaction temperatures, dispersion and emulsion 15 minutes; Add the 100kg silver ammonia spirit that adds 3kg 25% ammoniacal liquor and deionized water preparation with the 1.1kg silver sulfate again, continued dispersion and emulsion 60 minutes; Get sodium borohydride 0.3kg and potassium borohydride 0.35kg, be dissolved in the 80kg deionized water, be made into the aqueous solution of reductant, speed with 8.1kg/min sprays into the reactor from charging aperture 2, continued emulsion reaction after having annotated again 50 minutes, and promptly obtained average grain diameter and be 0.14% Nano Silver zinc complex sterilizing disinfectant less than 18nm, stability 〉=two year, pH value 6.8, Nano Silver zinc complex percentage by weight.
The antibacterial tests of comparative example Nano Silver zinc complex of the present invention sterilizing disinfectant
The antibacterial effect of Nano Silver zinc complex sterilizing disinfectant of the present invention and lavo-ofloxacin, amphomoronal compares, and the results are shown in Table 1, table 2.
Table 1 Nano Silver zinc complex sterilizing disinfectant, lavo-ofloxacin are to the MIC (mg/%) of part bacterium
By table 1 as seen, compare with lavo-ofloxacin, Nano Silver zinc complex sterilizing disinfectant all has significantly antibacterial, bactericidal effect to the clinical separation of bacterial of 78 strains, and especially gram-positive bacteria such as Staphylococcus epidermidis, bacillus cereus have stronger antibacterial action, the MIC of Staphylococcus epidermidis
50, the MIC of Staphylococcus epidermidis and bacillus cereus
90Be starkly lower than lavo-ofloxacin.Annotate: MIC
50, MIC
90Be worth more for a short time, antibacterial action is strong more.
Table 2 Nano Silver zinc complex sterilizing disinfectant, amphomoronal are to the MIC (mg/%) of part fungi
By table 2 as seen, compare with amphomoronal, Nano Silver zinc complex sterilizing disinfectant all has stronger antibacterial, bactericidal action, its MIC to the clinical separation fungi of 41 strains
50, MIC
90Be starkly lower than amphomoronal.Annotate: MIC
50, MIC
90Be worth more for a short time, antibacterial action is strong more.
Claims (10)
1. Nano Silver zinc complex sterilizing disinfectant, it is characterized in that: its by silver salt, reductant, contain the zinc nano-carrier and water formulated, the weight percent content of each component is: silver salt 0.008～0.49%, reductant 0.002～0.25%, contain zinc nano-carrier 0.01～2.0%, water 97.26～99.98%.
2. Nano Silver zinc complex sterilizing disinfectant according to claim 1 is characterized in that: the percentage by weight of its Nano Silver zinc complex in Nano Silver zinc complex sterilizing disinfectant is 0.01～0.7%.
3. Nano Silver zinc complex sterilizing disinfectant according to claim 1 is characterized in that: its Nano Silver zinc complex average particle size≤20nm.
4. Nano Silver zinc complex sterilizing disinfectant according to claim 1 is characterized in that: its silver salt is one or more the combination in silver nitrate, silver sulfate, the silver orthophosphate.
5. Nano Silver zinc complex sterilizing disinfectant according to claim 1 is characterized in that: its reductant is one or more the combination in sodium borohydride, potassium borohydride, trisodium citrate, hydrazine hydrate, the hydrogen peroxide.
6. Nano Silver zinc complex sterilizing disinfectant according to claim 1 is characterized in that: it contains the zinc nano-carrier is LYZS-2 type water-soluble granular shape white powder.
7. Nano Silver zinc complex sterilizing disinfectant according to claim 1 is characterized in that: its water is the running water of placing under deionized water or the room temperature 16～36 hours.
8. equipment for preparing the described Nano Silver zinc complex of claim 1 sterilizing disinfectant, it is characterized in that: it comprises reactor (3), batch (-type) high-shear emulsion machine (1) and pipeline high-shear emulsion machine (5), reactor top is provided with charging aperture (2), the bottom is provided with discharging opening (7), discharging opening is equipped with discharging valve (8), the batch (-type) high-shear emulsion machine is installed in reactor top, the emulsifying head of batch (-type) high-shear emulsion machine stretches into reactor inside, the pipeline high-shear emulsion machine is installed in the reactor outside, pipeline high-shear emulsion machine discharging opening is connected with reactor by discharge pipe (4), and charging aperture is connected with the discharging opening of reactor by feed pipe (6).
9. the preparation method of the described Nano Silver zinc complex of claim 1 sterilizing disinfectant, it is characterized in that: it comprises following concrete steps:
(1), in reactor, add under the deionized water of mass percent 15～70% or the room temperature and place 16～36 hours running water, the water of residual mass percentage is used for configuration and contains the zinc nano-carrier aqueous solution, silver salt solution, the reductant aqueous solution; Add and contain the zinc nano-carrier aqueous solution, the mass ratio that contains zinc nano-carrier and water is 1: 40～130; Under the mixed at high speed of batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine was sheared, dispersion and emulsion 6～20 minutes, fluid temperature remained on 5～25 ℃;
(2), in reactor, add silver salt solution, the mass ratio of silver salt and water is 1: 30～110, continues dispersion and emulsion 40～90 minutes;
(3), the speed of the reductant aqueous solution with 1.5～9.5kg/min is sprayed in the reactor, the mass ratio of reductant and water is 1: 50～250, continues dispersion and emulsion 30～60 minutes, can obtain Nano Silver zinc complex sterilizing disinfectant.
10. the preparation method of Nano Silver zinc complex sterilizing disinfectant according to claim 9 is characterized in that: the speed of agitator of its batch (-type) high-shear emulsion machine and pipeline high-shear emulsion machine is 2000～3000rpm.
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| CN104140133A (en) * | 2014-07-27 | 2014-11-12 | 惠州市银嘉环保科技有限公司 | Antibacterial oil absorption compound kieselguhr and application thereof |
| CN104743686A (en) * | 2015-04-08 | 2015-07-01 | 华东理工大学 | Novel renewable fish tank sterilizing and oxygen-releasing bag |
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| CN108849939A (en) * | 2018-07-31 | 2018-11-23 | 广东省农业科学院植物保护研究所 | Lavo-ofloxacin hydrochloride is preparing the application in the pesticidal preparations for preventing and treating tobacco bacterial wilt |
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| CN108849939A (en) * | 2018-07-31 | 2018-11-23 | 广东省农业科学院植物保护研究所 | Lavo-ofloxacin hydrochloride is preparing the application in the pesticidal preparations for preventing and treating tobacco bacterial wilt |
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Application publication date: 20110406 |