CN103817754A - Nano-silver floor - Google Patents
Nano-silver floor Download PDFInfo
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- CN103817754A CN103817754A CN201410106776.1A CN201410106776A CN103817754A CN 103817754 A CN103817754 A CN 103817754A CN 201410106776 A CN201410106776 A CN 201410106776A CN 103817754 A CN103817754 A CN 103817754A
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Abstract
The invention relates to the field of nano materials and in particular relates to a nano-silver floor. The nano-silver floor is characterized by sending a technical wood floor into a vacuum tank containing a nano-silver water solution; then carrying out pressure treatment; finally carrying out microwave treatment, and then taking out and treating the floor, wherein the nano-silver water solution is formed by taking deionized water as a solvent and nano-silver as a solute, dissolving nano-silver into the deionized water, dissolving an acrylic resin as a complexing agent and stabilizing agent into the deionized water, and then simultaneously adding a dispersing agent and a first reducing agent; the concentration of nano-silver is 50-150ppm, and the mass content of the acrylic resin in the solution is 1-10%; the nano-silver is prepared by the following steps of adding a sodium dodecyl sulfate solution to a silver nitrate water solution to obtain mixed liquor, adding crown ether and second reducing agents containing alkali metals to the mixed liquor, and controlling the pH value to be 8-9, thus obtaining the nano-silver, wherein the mole ratio of sodium dodecyl sulfate to silver nitrate is (2-3):1. The nano-silver floor has good stability and dispersibility and can fully resist moulds.
Description
Technical field
The present invention relates to field of nanometer material technology, relate in particular to a kind of Nano Silver floor.
Background technology
Metal nano material is an important branch of nano material, and it wherein obtains maximum concerns because of the wide application prospect of Nano Silver take noble metal gold, silver, copper as representative.Nano Silver can be used in a lot of aspects: in chemical fibre, add a small amount of Nano Silver, can improve some performance of chemical fibre product, and make it have very strong sterilizing ability; The appropriate Nano Silver that adulterates in silicon oxide film, can make the glass that plates this film have certain Photoluminescence.Therefore Nano 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, becomes and has the functional material theoretical research of property and the important topic of application and development.
Since the preparation of Nano Silver and improvement technology are initial from nano anti-biotic material, just become the focus of researcher and developers' extensive concern.The preparation of Nano Silver is divided into Physical and chemical method.Chemical method has sol-gal process, galvanoplastic, oxidation-reduction method and vacuum vapour deposition etc.The I of silver-colored particle prepared by chemical method reaches several nanometers, simple to operate, easily controls.Shortcoming is that the silver-colored particle obtaining is difficult for shifting and assembling, and easily comprises impurity, and easily assembles.Physical is mainly vacuum evaporation, sputter plating and ion plating etc.Wherein chemical reduction method obtains fine application because required experiment condition is simple, energy-conservation.
CN200958280Y (2007-10-10) discloses a kind of floor of containing Nano Silver, but this use is nano silver colloidal sol, fails to give full play to the antimildew and antibacterial effect of Nano Silver.
Summary of the invention
The first object of the present invention be to provide a kind of can effectively resist mould Nano Silver floor.
The first technical purpose of the present invention is achieved by the following technical programs:
A kind of Nano Silver floor, it is that floor is sent in the vacuum tank that contains nano-silver water solution, is evacuated to vacuum for-0.05MPa～-0.01MPa and keeps 15-20min; Then the processing of exerting pressure, applies pressure to 0.2-0.5MPa and keeps 18-28min; Finally carry out microwave treatment, microwave frequency is 400MHz～650MHz, and microwave treatment time is 1～3min, then takes out post processing; Described floor is the floor that Recombinant Wood is made; Described Recombinant Wood is glued board, thick china, solid wooden compound floor or Recombinant Wood section;
Described nano-silver water solution is take deionized water as solvent, dissolves in deionized water, take acrylic resin as complexing agent, stabilizing agent adds dispersant and the first reducing agent and form solution after dissolving in deionized water simultaneously take Nano Silver as solute;
Described dispersant is triethanolamine, and described the first reducing agent is the hydrazine hydrate aqueous solution;
The concentration of described Nano Silver is 50-150ppm, and the mass content of described acrylic resin in solution is 1-10%;
Described Nano Silver is prepared from according to following steps:
(1) sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtain mixed liquor, the mol ratio of described dodecyl sodium sulfate and silver nitrate is 2-3:1;
(2) in described mixed liquor, add crown ether and contain alkali-metal the second reducing agent, controlling pH value is 8-9, obtains Nano Silver.
Advantage of the present invention is:
Crown ether have hydrophobic external skeletal and hydrophilic can with the inner chamber of metal ion Cheng Jian, can form stable complex with alkali metal ion.Simultaneously; the present invention is engaged in follow-up reduction reaction and adds and contain alkali-metal reducing agent; add after above-mentioned reducing agent, crown ether and alkali metal ion form stable complex, make on the one hand free in reaction system or exposed reduction anion have higher reactivity; Meanwhile, after alkali metal and crown ether generation ligand complex, alkali metal cation is coated in inner chamber by crown ether, just pulls open thus the distance between positive and negative charge in Nano Silver system, make Nano Silver can stable dispersion in the aqueous solution, be difficult for reuniting;
2. combination and the Nano Silver solute of dispersant, the first reducing agent and the stabilizing agent by specific components and proportioning are mixed with nano-silver water solution, in depositing, can not occur to reunite and particle is grown up, and can be not oxidized, stability and good dispersion;
3. be prepared into the required Nano Silver of the preparation of nano silver aqueous solution by specific method, nano-Ag particles is more even, stable good with dispersive property, has further improved the stability on final required Nano Silver floor.
As preferably, the mol ratio of described crown ether and silver nitrate is 1-2:1; The described mol ratio that contains alkali-metal reducing agent and silver nitrate is 0.5-1:1.
As preferably, the mass content of described dispersant in solution is 1-3%; The content of described the first reducing agent in solution is 0.2-0.4%.
As preferably, described in to contain alkali-metal the second reducing agent be one or more in sodium borohydride, potassium borohydride, sodium metaphosphate or natrium citricum.
As preferably, described step (2) adds crown ether and contains before alkali-metal the second reducing agent in described mixed liquor, and described mixed liquor is heated to 45-55 ℃.
First heating adds crown ether again and contains alkali-metal the second reducing agent, can increase the reactivity of reduction anion that dissociate or exposed in reaction system, promote that alkali metal reacts with crown ether generation ligand complex, further pull open the distance between positive and negative charge in Nano Silver system, make Nano Silver can stable dispersion in the aqueous solution, be difficult for reuniting.
More preferably, described step (2) is heated to 70-85 ℃ after adding crown ether in described mixed liquor and containing alkali-metal the second reducing agent, continues to stir 5-8min.
After adding crown ether in described mixed liquor and containing alkali-metal the second reducing agent, continue heating, can further increase the reactivity of reduction anion that dissociate or exposed in reaction system, promote that alkali metal reacts with crown ether generation ligand complex, further pull open the distance between positive and negative charge in Nano Silver system, make Nano Silver can stable dispersion in the aqueous solution, be difficult for reuniting.
As preferably, described step (2) is carried out under microwave vacuum condition, is specifically evacuated to vacuum for-0.02MPa～-0.001MPa, then carries out microwave treatment, and microwave frequency is 100MHz～230MHz, and microwave treatment time is 3～7s.
Adopt microwave to react and can greatly accelerate reaction rate, Reaction time shorten, further improves the stability of nano-silver water solution.
As preferably, described Nano Silver preparation also comprises step (3) ultrafiltration desalination and dry.
Ultrafiltration, except the inorganic salts or the organic salt that generate in dereaction, finally obtains the Nano Silver that particle size range is 20-60nm.
As preferably, described crown ether be bicyclohexane also-18-hat-6.
As preferably, described post processing is dry or hot pressing; Described hot pressing pressure is 0.5-1.4MPa, and hot pressing time is 1-5min.
In sum, the present invention has following beneficial effect: nano-silver water solution stability of the present invention and good dispersion; Can make Nano Silver more effectively infiltrate in wood floor board, fully resist because of the invasion and attack of moisture-induced mould to Recombinant Wood.
The specific embodiment
embodiment mono-
The preparation of Nano Silver:
Sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtains mixed liquor, and the mol ratio of dodecyl sodium sulfate and silver nitrate is 2:1;
Mixed liquor is heated to 45 ℃, under stirring to add in mixed liquor bicyclohexane also-18-hat-6 and sodium borohydride, be heated to 70 ℃, continue to stir 5min; Bicyclohexane also-18-hat-6 is 1:1 with the mol ratio of silver nitrate; The mol ratio of sodium borohydride and silver nitrate is 0.5:1, and controlling pH value is 8, obtains Nano Silver.
The preparation of nano-silver water solution:
Take deionized water as solvent, dissolve in deionized water take Nano Silver as solute, take acrylic resin as complexing agent with stabilizing agent adds dispersant after dissolving in deionized water and the first reducing agent forms solution simultaneously;
Dispersant is triethanolamine, and the mass content in solution is 1%; The first reducing agent is the hydrazine hydrate aqueous solution; Content in solution is 0.2%;
The concentration of Nano Silver is 50ppm, and the mass content of acrylic resin in solution is 1%.
Using method by nano-silver water solution for the preparation of wood floor board:
Using method is that Recombinant Wood is sent in the vacuum tank that contains nano-silver water solution, is evacuated to vacuum for-0.05MPaMPa and keeps 15min; Then the processing of exerting pressure, applies pressure to 0.2MPa and keeps 18min; Finally carry out microwave treatment, microwave frequency is 300MHz, and microwave treatment time is 1min, then takes out dry; Recombinant Wood can be glued board, thick china, solid wooden compound floor or Recombinant Wood section.
The Recombinant Wood that the present embodiment obtains reaches the highest 0 grade of JISZ 2911 standards after testing, decorates popularity bacillus in room, food Trichoderma, stain fungus etc. and has stronger killing action.
embodiment bis-
The preparation of Nano Silver:
Sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtains mixed liquor, and the mol ratio of dodecyl sodium sulfate and silver nitrate is 3:1;
Mixed liquor is heated to 55 ℃, under stirring to add in mixed liquor bicyclohexane also-18-hat-6 and potassium borohydride, be heated to 85 ℃, continue to stir 8min; Bicyclohexane also-18-hat-6 is 1-2:1 with the mol ratio of silver nitrate; The mol ratio of potassium borohydride and silver nitrate is 0.5-1:1, and controlling pH value is 8-9, obtains Nano Silver.
The preparation of nano-silver water solution:
Take deionized water as solvent, dissolve in deionized water take Nano Silver as solute, take acrylic resin as complexing agent with stabilizing agent adds dispersant after dissolving in deionized water and reducing agent forms solution simultaneously;
Dispersant is triethanolamine, and the mass content in solution is 1-3%; The first reducing agent is the hydrazine hydrate aqueous solution; Content in solution is 0.2-0.4%;
The concentration of Nano Silver is 50-150ppm, and the mass content of acrylic resin in solution is 1-10%.
Using method by nano-silver water solution for the preparation of wood floor board (Recombinant Wood can be glued board, thick china, solid wooden compound floor or Recombinant Wood section):
Using method is that Recombinant Wood is sent in the vacuum tank that contains nano-silver water solution, is evacuated to vacuum for-0.05MPa～-0.01MPa and keeps 15-20min; Then the processing of exerting pressure, applies pressure to 0.2-0.5MPa and keeps 18-28min; Finally carry out microwave treatment, microwave frequency is 300MHz～950MHz, and microwave treatment time is 1～3min, then takes out hot pressing, and hot pressing pressure is 0.5-0.8MPa, and hot pressing time is 1-2min.
The Recombinant Wood that the present embodiment obtains reaches the highest 0 grade of JISZ 2911 standards after testing, decorates popularity bacillus in room, food Trichoderma, stain fungus etc. and has stronger killing action.
embodiment tri-
The preparation of Nano Silver:
Sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtains mixed liquor, and the mol ratio of dodecyl sodium sulfate and silver nitrate is 2.5:1;
Mixed liquor is heated to 50 ℃, under stirring to add in mixed liquor bicyclohexane also-18-hat-6 and sodium metaphosphate, be heated to 75 ℃, continue to stir 6min; Bicyclohexane also-18-hat-6 is 1.5:1 with the mol ratio of silver nitrate; The mol ratio of sodium metaphosphate and silver nitrate is 0.8:1, and controlling pH value is 8.5, obtains Nano Silver.
The preparation of nano-silver water solution:
Take deionized water as solvent, dissolve in deionized water take Nano Silver as solute, take acrylic resin as complexing agent with stabilizing agent adds dispersant after dissolving in deionized water and reducing agent forms solution simultaneously;
Dispersant is triethanolamine, and the mass content in solution is 2%; The first reducing agent is the hydrazine hydrate aqueous solution; Content in solution is 0.3%;
The concentration of Nano Silver is 100ppm, and the mass content of acrylic resin in solution is 8%.
The using method on the floor that nano-silver water solution is made for Recombinant Wood (can be glued board, thick china, solid wooden compound floor or Recombinant Wood section):
Using method is that Recombinant Wood is sent in the vacuum tank that contains nano-silver water solution, is evacuated to vacuum for-0.03MPa and keeps 18min; Then the processing of exerting pressure, applies pressure to 0.3MPa and keeps 23min; Finally carry out microwave treatment, microwave frequency is 550MHz, and microwave treatment time is 2min, then takes out hot pressing, and hot pressing pressure is 0.8-1.1MPa, and hot pressing time is 2-3min.
The Recombinant Wood that the present embodiment obtains reaches the highest 0 grade of JISZ 2911 standards after testing, decorates popularity bacillus in room, food Trichoderma, stain fungus etc. and has stronger killing action.
embodiment tetra-
The preparation of Nano Silver:
Sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtains mixed liquor, and the mol ratio of dodecyl sodium sulfate and silver nitrate is 2:1;
To add in mixed liquor bicyclohexane also-18-hat-6 and natrium citricum, bicyclohexane also-18-hat-6 is 1:1 with the mol ratio of silver nitrate; The mol ratio of natrium citricum and silver nitrate is 0.5:1, controlling pH value is 8, put into microwave vacuum tank processes under microwave vacuum condition, specifically being evacuated to vacuum is-0.02MPa, carry out microwave treatment, microwave frequency is 100MHz again, and microwave treatment time is 3s, then ultrafiltration desalination dry, finally obtains the Nano Silver that particle size range is 20-60nm.
The preparation of nano-silver water solution and using method thereof are with embodiment mono-.
Using method by nano-silver water solution for wood floor board:
Recombinant Wood can be glued board, thick china, solid wooden compound floor or Recombinant Wood section; Using method is that Recombinant Wood is sent in the vacuum tank that contains nano-silver water solution, is evacuated to vacuum for-0.03MPa and keeps 18min; Then the processing of exerting pressure, applies pressure to 0.3MPa and keeps 23min; Finally carry out microwave treatment, microwave frequency is 550MHz, and microwave treatment time is 2min, then takes out hot pressing, and hot pressing pressure is 1.1-1.4MPa, and hot pressing time is 3-5min.
embodiment five
The preparation of Nano Silver:
Sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtains mixed liquor, and the mol ratio of dodecyl sodium sulfate and silver nitrate is 3:1;
To add in mixed liquor bicyclohexane also-18-hat-6 and 1:1 combines in molar ratio sodium borohydride and potassium borohydride, bicyclohexane also-mol ratio of 18-hat-6 and silver nitrate is 1-2:1; The mol ratio of sodium borohydride and potassium borohydride and silver nitrate is 1:1, controlling pH value is 9, put into microwave vacuum tank processes under microwave vacuum condition, specifically being evacuated to vacuum is-0.001MPa, carry out microwave treatment, microwave frequency is 230MHz again, and microwave treatment time is 7s, then ultrafiltration desalination dry, finally obtains the Nano Silver that particle size range is 20-60nm.
The preparation of nano-silver water solution and using method thereof are with embodiment bis-.
embodiment six
The preparation of Nano Silver:
Sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtains mixed liquor, and the mol ratio of dodecyl sodium sulfate and silver nitrate is 2.5:1;
To add in mixed liquor bicyclohexane also-18-hat-6 and 1:1 combines in molar ratio potassium borohydride and sodium metaphosphate, bicyclohexane also-mol ratio of 18-hat-6 and silver nitrate is 1.5:1; The mol ratio of potassium borohydride and sodium metaphosphate and silver nitrate is 0.8:1, controlling pH value is 8.5, put into microwave vacuum tank processes under microwave vacuum condition, specifically being evacuated to vacuum is-0.01MPa, carry out microwave treatment, microwave frequency is 130MHz again, and microwave treatment time is 5s, then ultrafiltration desalination dry, finally obtains the Nano Silver that particle size range is 20-60nm.
The preparation of nano-silver water solution and using method thereof are with embodiment tri-.
comparing embodiment one
The preparation of Nano Silver:
Sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtains mixed liquor, and the mol ratio of dodecyl sodium sulfate and silver nitrate is 1:1;
Under stirring, in mixed liquor, add sodium borohydride, continue to stir 5min; The mol ratio of sodium borohydride and silver nitrate is 2:1, and controlling pH value is 10, obtains Nano Silver.
The preparation of nano-silver water solution:
Take water as solvent, dissolve in water take Nano Silver as solute, take acrylic resin as complexing agent and stabilizing agent add dispersant triethanolamine after dissolving in water simultaneously and form solution;
The mass content of triethanolamine in solution is 1%; Content in solution is 0.2%;
The concentration of Nano Silver is 40ppm, and the mass content of acrylic resin in solution is 0.5%.
Embodiment 1-6 and comparative example are left standstill, the dispersity of observing respectively the Nano Silver of nano-silver water solution system after 1 month and 6 months, observed result is in table 1.
The dispersity of Nano Silver in table 1 nano-silver water solution system
This specific embodiment is only explanation of the invention; it is not limitation of the present invention; those skilled in the art are reading after this description and can make to the present embodiment the modification that there is no creative contribution as required, but as long as within the scope of claim of the present invention, are all subject to the protection of Patent Law.
Claims (10)
1. a Nano Silver floor, is characterized in that:
Floor is sent in the vacuum tank that contains nano-silver water solution, be evacuated to vacuum for-0.05MPa～-0.01MPa and keep 15-20min; Then the processing of exerting pressure, applies pressure to 0.2-0.5MPa and keeps 18-28min; Finally carry out microwave treatment, microwave frequency is 400MHz～650MHz, and microwave treatment time is 1～3min, then takes out post processing; Described floor is the floor that Recombinant Wood is made; Described Recombinant Wood is glued board, thick china, solid wooden compound floor or Recombinant Wood section;
Described nano-silver water solution is take deionized water as solvent, dissolves in deionized water, take acrylic resin as complexing agent, stabilizing agent adds dispersant and the first reducing agent and form solution after dissolving in deionized water simultaneously take Nano Silver as solute;
Described dispersant is triethanolamine, and described the first reducing agent is the hydrazine hydrate aqueous solution;
The concentration of described Nano Silver is 50-150ppm, and the mass content of described acrylic resin in solution is 1-10%;
Described Nano Silver is prepared from according to following steps:
(1) sodium dodecyl sulfate solution is added in silver nitrate aqueous solution and obtain mixed liquor, the mol ratio of described dodecyl sodium sulfate and silver nitrate is 2-3:1;
(2) in described mixed liquor, add crown ether and contain alkali-metal the second reducing agent, controlling pH value is 8-9, obtains Nano Silver.
2. a kind of Nano Silver according to claim 1 floor, is characterized in that: the mol ratio of described crown ether and silver nitrate is 1-2:1; The described mol ratio that contains alkali-metal reducing agent and silver nitrate is 0.5-1:1.
3. a kind of Nano Silver according to claim 1 floor, is characterized in that: the mass content of described dispersant in solution is 1-3%; The content of described the first reducing agent in solution is 0.2-0.4%.
4. a kind of Nano Silver according to claim 1 floor, is characterized in that: described in to contain alkali-metal the second reducing agent be one or more in sodium borohydride, potassium borohydride, sodium metaphosphate or natrium citricum.
5. according to a kind of Nano Silver floor described in claim 1-4 any one, it is characterized in that: described step (2) adds crown ether and contains before alkali-metal the second reducing agent in described mixed liquor, and described mixed liquor is heated to 45-55 ℃.
6. a kind of Nano Silver according to claim 5 floor, is characterized in that: described step (2) is heated to 70-85 ℃ after adding crown ether in described mixed liquor and containing alkali-metal the second reducing agent, continues to stir 5-8min.
7. a kind of Nano Silver according to claim 6 floor, it is characterized in that: described step (2) is carried out under microwave vacuum condition, specifically being evacuated to vacuum is-0.02MPa～-0.001MPa, carry out again microwave treatment, microwave frequency is 100MHz～230MHz, and microwave treatment time is 3～7s.
8. a kind of Nano Silver according to claim 7 floor, is characterized in that: described crown ether be bicyclohexane also-18-hat-6.
9. a kind of Nano Silver according to claim 8 floor, is characterized in that: described Nano Silver preparation also comprises step (3) ultrafiltration desalination and dry.
10. a kind of Nano Silver according to claim 9 floor, for the using method of Recombinant Wood, is characterized in that: described post processing is dry or hot pressing; Described hot pressing pressure is 0.5-1.4MPa, and hot pressing time is 1-5min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104963478A (en) * | 2015-07-15 | 2015-10-07 | 德华兔宝宝装饰新材股份有限公司 | Photocatalyst environment-friendly floor and production process thereof |
| CN106977969A (en) * | 2017-04-17 | 2017-07-25 | 广东善健健康产业有限公司 | Antibacterial and mouldproof wood-fibred chopping block and preparation method thereof |
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