CN103357890B - One kettle way prepares the cellulose hydrothermal synthesis method of high length-diameter ratio nano silver wire - Google Patents
One kettle way prepares the cellulose hydrothermal synthesis method of high length-diameter ratio nano silver wire Download PDFInfo
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- CN103357890B CN103357890B CN201310332124.5A CN201310332124A CN103357890B CN 103357890 B CN103357890 B CN 103357890B CN 201310332124 A CN201310332124 A CN 201310332124A CN 103357890 B CN103357890 B CN 103357890B
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Abstract
The invention discloses the cellulose hydrothermal synthesis method that one kettle way prepares high length-diameter ratio nano silver wire, join in polytetrafluoroethyllining lining by disposable to cellulose, silver sulfate, softex kw and deionized water, fully stir and make it to mix; Then liner loaded autoclave and put into baking oven or Muffle furnace, at 180 ~ 200 DEG C, heating 10 ~ 24h, taking out nature cooling; Cooled product carries out centrifugal or suction filtration separation, obtains high length-diameter ratio nano silver wire.The present invention utilizes reproducible biomass resource, simple to operate, one pot of generation, the nano silver wire average diameter obtained be 90 ~ 350nm, draw ratio more than 200, size uniformity, productive rate be high.
Description
Technical field
The invention belongs to one-dimensional metal technical field of nanometer material preparation, be specifically related to the cellulose hydrothermal synthesis method that one kettle way prepares high length-diameter ratio nano silver wire.
Background technology
Size uniformity, have compared with high length-diameter ratio nano silver wire material due to its have excellent heat conduction electrically, the characteristic such as light transmission, flexible resistance, catalysis characteristics, antibiotic property and surface plasma resonance effect and enjoy the concern of people.The preparation method of current nano silver wire mainly contains Physical and chemical method two kinds.Wherein Physical mainly comprises sublimation recrystallization method, ion sputtering process and mechanical milling method etc.; Chemical method mainly comprises light or thermal induction method, template, chemical vapor infiltration, chemical reduction method and microwave irradiation etc.Though these methods solve subproblem, also there are some drawbacks.Physical requires higher to instrument and equipment, and producing cost is expensive; Chemical method is versatile and flexible, but the problems such as higher, the made nano silver wire uniformity of ubiquity preparation process very complicated, cost is poor, productive rate is lower, and chemical method often needs to introduce more chemical reagent, this will inevitably bring certain problem of environmental pollution.
Cellulose is a kind of polysaccharide that distributed in nature is the widest, content is maximum, is renewable resource the abundantest on the earth.Cellulose series biomass mainly comprises discarded object and residue (as agricultural crop straw, husk, wheat bran, bagasse etc.), forest (cork and hardwood) and forestry processing waste, the careless class etc. of agricultural production.By hydro-thermal reaction system, the hydrolysis of lignocellulosic is combined with the reduction process of nano silver wire, utilize cellulosic hydrolysate (sugar and aldehyde) carry out reducing preparation size homogeneous, there is nano silver wire compared with high length-diameter ratio, yet there are no relevant report.
Summary of the invention
One kettle way is the object of the present invention is to provide to prepare the cellulose hydrothermal synthesis method of high length-diameter ratio nano silver wire, utilize reproducible biomass resource, simple to operate, one pot of generation, the nano silver wire average diameter obtained be 90 ~ 350nm, draw ratio more than 200, size uniformity, productive rate be high.
For achieving the above object, the present invention adopts following technical scheme:
The cellulose hydrothermal synthesis method that one kettle way prepares high length-diameter ratio nano silver wire comprises the following steps:
(1) by cellulose, silver sulfate, softex kw (CTAB) with deionized water is disposable joins in polytetrafluoroethyllining lining, fully stir and make it to mix;
(2) above-mentioned liner loaded autoclave and put into baking oven or Muffle furnace, at 180 ~ 200 DEG C, heating 10 ~ 24h, taking out nature cooling;
(3) above-mentioned cooled product is carried out centrifugal or suction filtration separation, obtain high length-diameter ratio nano silver wire.
Described cellulose is one or more in filter paper, agricultural crop straw, husk, wheat bran, bagasse.
The mass ratio of cellulose and silver sulfate is 5 ~ 30:1.
The mol ratio of CTAB and silver sulfate is 3 ~ 8:1.
The addition of deionized water is 50 ~ 65% of polytetrafluoroethyllining lining volume.
Obtained nano silver wire average diameter is that 90 ~ 350nm, draw ratio are more than 200.
Remarkable advantage of the present invention is: utilize reproducible biomass resource, simple to operate, one pot of generation, the nano silver wire average diameter obtained be 90 ~ 350nm, draw ratio more than 200, size uniformity, productive rate be high.
Accompanying drawing explanation
Fig. 1 is SEM (SEM) photo of nano silver wire prepared by embodiment 1.
Detailed description of the invention
Example is below to illustrate technical process feature of the present invention further and unrestricted the present invention.
EXAMPLE l
Measure 0.03g Ag
2sO
4, 0.40g filter paper (cellulose), 7mL CTAB solution (0.1mol/L) and 25ml deionized water add in 50mL polytetrafluoroethyllining lining, fully stir and make it to mix.Then liner loaded autoclave and put into baking oven or Muffle furnace, at 180 DEG C, heating 20h, then making it be cooled to room temperature; Carry out centrifugation to reacted product, with ESEM (SEM) observing response product, gained nano silver wire average diameter is that 100 ~ 250nm, draw ratio are more than 200.
Embodiment 2
Measure 0.035g Ag
2sO
4, 0.45g filter paper (cellulose), 8mL CTAB solution (0.1mol/L) and 25ml deionized water add in 50mL polytetrafluoroethyllining lining, fully stir and make it to mix.Then liner loaded autoclave and put into baking oven or Muffle furnace, at 190 DEG C, heating 20h, then making it be cooled to room temperature; Carry out centrifugation to reacted product, with ESEM (SEM) observing response product, gained nano silver wire average diameter is that 100 ~ 200nm, draw ratio are more than 200.
Embodiment 3
Measure 0.035g Ag
2sO
4, 0.40g soya bean shell (cellulose), 9mL CTAB solution (0.1mol/L) and 25ml deionized water add in 50mL polytetrafluoroethyllining lining, fully stir and make it to mix.Then liner loaded autoclave and put into baking oven or Muffle furnace, at 180 DEG C, heating 20h, then making it be cooled to room temperature; Carry out centrifugation to reacted product, with ESEM (SEM) observing response product, gained nano silver wire average diameter is that 110 ~ 250nm, draw ratio are more than 200.
Embodiment 4
Measure 0.03g Ag
2sO
4, 0.40g soya bean shell (cellulose), 6mL CTAB solution (0.1mol/L) and 25ml deionized water add in 50mL polytetrafluoroethyllining lining, fully stir and make it to mix.Then liner loaded autoclave and put into baking oven or Muffle furnace, at 200 DEG C, heating 20h, then making it be cooled to room temperature; Carry out centrifugation to reacted product, with ESEM (SEM) observing response product, gained nano silver wire average diameter is that 110 ~ 300nm, draw ratio are more than 200.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. one kettle way prepares the cellulose hydrothermal synthesis method of high length-diameter ratio nano silver wire, it is characterized in that: comprise the following steps:
(1) join in polytetrafluoroethyllining lining by disposable to cellulose, silver sulfate, softex kw and deionized water, fully stir and make it to mix;
(2) above-mentioned liner loaded autoclave and put into baking oven or Muffle furnace, at 180 ~ 200 DEG C, heating 10 ~ 24h, taking out nature cooling;
(3) above-mentioned cooled product is carried out centrifugal or suction filtration separation, obtain high length-diameter ratio nano silver wire;
The mass ratio of cellulose and silver sulfate is 5 ~ 30:1;
The mol ratio of softex kw and silver sulfate is 3 ~ 8:1.
2. one kettle way according to claim 1 prepares the cellulose hydrothermal synthesis method of high length-diameter ratio nano silver wire, it is characterized in that: described cellulose is one or more in filter paper, agricultural crop straw, husk, wheat bran, bagasse.
3. one kettle way according to claim 1 prepares the cellulose hydrothermal synthesis method of high length-diameter ratio nano silver wire, it is characterized in that: the addition of deionized water is 50 ~ 65% of polytetrafluoroethyllining lining volume.
4. one kettle way according to claim 1 prepares the cellulose hydrothermal synthesis method of high length-diameter ratio nano silver wire, it is characterized in that: obtained nano silver wire average diameter is that 90 ~ 350nm, draw ratio are more than 200.
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CN103646868B (en) * | 2013-11-06 | 2016-05-25 | 南阳理工学院 | Hydro-thermal-vapor etch legal system is for the method for porous silicon |
CN104646682B (en) * | 2015-02-10 | 2017-01-18 | 上海理工大学 | Method for preparing gold nanoparticles by using sugarcane extracting solution |
CN104625087A (en) * | 2015-02-28 | 2015-05-20 | 济宁利特纳米技术有限责任公司 | Method for hydrothermally manufacturing silver nanowires |
TWI695848B (en) | 2015-03-03 | 2020-06-11 | 德商巴斯夫歐洲公司 | Silver nanowire synthesis with (meth) acrylate based capping agents |
CN110653379A (en) * | 2018-06-28 | 2020-01-07 | 宁波山功新材料科技有限公司 | Preparation method of degradable metal nanowires |
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CN102303124A (en) * | 2011-08-24 | 2012-01-04 | 浙江科创新材料科技有限公司 | Method for preparing length-diameter-ratio nano-silver wire by pH-value regulation solvothermal method |
CN102677454A (en) * | 2012-06-06 | 2012-09-19 | 山东大学 | Method for loading silver nano-particles on cellulose-containing material |
CN102775643A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Preparation method for nano-sliver/cellulose nanocrystalline composite particle |
CN102837003A (en) * | 2012-09-07 | 2012-12-26 | 中国科学院深圳先进技术研究院 | Nano silver particles with multilevel structure and preparation method thereof |
CN103203467A (en) * | 2013-04-17 | 2013-07-17 | 苏州冷石纳米材料科技有限公司 | Method for preparing silver nanowires |
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US7922787B2 (en) * | 2008-02-02 | 2011-04-12 | Seashell Technology, Llc | Methods for the production of silver nanowires |
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CN102303124A (en) * | 2011-08-24 | 2012-01-04 | 浙江科创新材料科技有限公司 | Method for preparing length-diameter-ratio nano-silver wire by pH-value regulation solvothermal method |
CN102677454A (en) * | 2012-06-06 | 2012-09-19 | 山东大学 | Method for loading silver nano-particles on cellulose-containing material |
CN102775643A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Preparation method for nano-sliver/cellulose nanocrystalline composite particle |
CN102837003A (en) * | 2012-09-07 | 2012-12-26 | 中国科学院深圳先进技术研究院 | Nano silver particles with multilevel structure and preparation method thereof |
CN103203467A (en) * | 2013-04-17 | 2013-07-17 | 苏州冷石纳米材料科技有限公司 | Method for preparing silver nanowires |
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