CN105127447B - Plant reduction method joint magnetic field prepares nano material and reaction twice laid method - Google Patents
Plant reduction method joint magnetic field prepares nano material and reaction twice laid method Download PDFInfo
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- CN105127447B CN105127447B CN201510603570.4A CN201510603570A CN105127447B CN 105127447 B CN105127447 B CN 105127447B CN 201510603570 A CN201510603570 A CN 201510603570A CN 105127447 B CN105127447 B CN 105127447B
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Abstract
Biological reducing method in the prior art is directed to prepare metal, particularly prepare the problem of nano metal material is present, nano material and reaction twice laid method are prepared the invention provides a kind of plant reduction method joint magnetic field, belongs to the green preparing technical field of nano material.Its method is：Particle diameter is taken to be mixed for micron-sized plant powder with metal salt solution, 24~30h is reacted in magnetic field intensity H is 20mT~1T steady magnetic field or alternating magnetic field, or, placed in magnetic field intensity 1T ＜ H≤12T steady magnetic field after 10~60min, 24~30h is reacted again, then separating nanomaterials product and reaction discarded object；The discarded object of reaction is subjected to fermentation process again, the biogas or ethanol of generation can as the energy, ferment the biogas slurry produced or residue etc. can as anti-appliable plant fertilizer nutrient.This method can improve efficiency, operability and the stability that plant reduction method prepares nano material, and reaction waste, which can ferment, produces biogas or ethanol, is the environment-friendly preparation method of environmental protection.
Description
Technical field
The invention belongs to the green preparing technical field of nano material, more particularly to a kind of plant reduction method joint magnetic field system
Standby nano material and reaction twice laid method.
Background technology
The material of nanoscale is in the handover region of atom and macro object, is imitated with surface-interface effect, small size
Should, quantum size effect and macro quanta tunnel effect, and unusual mechanics, electricity, magnetics, optics, calorifics and change can be produced
Etc. characteristic.So as to have important answer in the fields such as national defence, electronics, chemical industry, metallurgy, aviation, light industry, medicine, nuclear technology
With value, increasingly it is valued by people.The nano materials such as particularly common gold, silver, palladium, it is catalyzed, sterilized, electricity Gong electricity
Son characteristic be widely used in fields such as environmental protection, medical treatment, stability and high efficiency prepare different shape, species metal nano material general
Promote every profession and trade development.
A kind of current biological reducing method, principle of reaction thinks ,-the C- in the polyhydroxy based biological molecule such as reduced sugar, flavones
OH reacts with metal ion, generates nano metal, and the hydroxyl of these biomolecule may be oxidized to carbonyl, explanation after the reaction
Polyhydroxy based biological molecule plays a leading role to metal reduction；It is another to think that protein reacts in reduction process and metal ion
Leading role.
But, it is slow that current biological reducing method also has a reaction speed, and more can not handle etc. of discarded object is asked after reaction
Topic.
Electrochemical reaction is redox reaction, and the transmission and transfer of electronics, and ion are there is during the course of the reaction
Movement.Thus ionization ion can change movement locus in the presence of Lorentz force, increase diffusivity, change electrochemistry
Reaction.Because magnetic field has obvious effect to chemical reaction, and magnetic field can produce obvious effect to hydroxyl and metal ion,
And plant reduction process nature is chemical reaction, and plant reduction reaction is exactly mainly the effect of organic group such as hydroxyl, so,
In theory, magnetic field has facilitation to plant reduction reaction.But, it there is no prepared for plant reduction method joint magnetic field at present
Metal material, the particularly research to preparing nano material.
The content of the invention
Plant reduction method in the prior art is directed to prepare metal, particularly prepare the problem of nano metal material is present,
Nano material and reaction twice laid method are prepared the invention provides a kind of plant reduction method joint magnetic field.This method can be improved
Plant reduction method prepares efficiency, operability and the stability of nano material, and reaction waste can be used for fermentation to produce biogas or second
Alcohol, is the environment-friendly preparation method of environmental protection.
A kind of plant reduction method joint magnetic field prepares nano material and reaction twice laid method, comprises the following steps：
(1) particle diameter is taken to be mixed with metal salt solution for micron-sized plant powder, at 10~50 DEG C, mixing speed 100~
150rmin-1Under conditions of, 24~30h is reacted in magnetic field intensity H is 20mT~1T steady magnetic field or alternating magnetic field, is obtained
Nano metal product, then separation product and reaction discarded object；
Or, take particle diameter to be mixed for micron-sized plant powder with metal salt solution, magnetic field intensity 1T ＜ H≤12T's
Placed in steady magnetic field after 10~60min, in the absence of a magnetic field, in 10~50 DEG C, 100~150rmin of mixing speed-1
Under conditions of, then 24~30h is reacted, nano metal product is obtained, then separation product and reaction discarded object；
Wherein, described metal salt is Ag, Au, Pt or Pd nitrate or hydrochloride；
The addition ratio of metal ion is 1g in described plant powder and metal salt：(0.0167-0.5)mmol；
Preferably, described metal salt solution concentration is 1-5mmol/L；
Described plant powder is the cauline leaf the like waste of crops；Or, described plant powder is fruit tree, views and admires tree
Or the leaf of shade tree；
The particle size range of described micron order plant powder is 1~999 micron；
The yield of above-mentioned reaction is higher than 90%；
(2) discarded object of reaction is subjected to fermentation process, the biogas or ethanol of generation can be as the energy, in step (1)
Used in reaction, for heating, provide electromagnetic field, the stirring offer energy；The biogas slurry produced of fermenting or residue can plant as reaction
The fertilizer nutrient of thing growth.
Compared with prior art, advantage of the invention is that：
1st, the present invention applies a magnetic field when plant reduction reacts, and substantially increases plant reduction method and prepares nano material
Efficiency, operability and stability, the yield of reaction is higher than 90%.
2nd, generation Lorentz force is moved in magnetic field by powered reactant or product and promotes that equally there is ferromagnetism, suitable
The plant reduction process of the metal ions such as the Au of magnetic or diamagnetic characteristic, Pt, Pd, Ag, improves reaction rate and yield and colloidal sol
Stability.
3. metal nanoparticle pattern can be controlled by magnetic field, subsphaeroidal, wire is prepared, bar-shaped and flake nano material
Material, and specific plant is easily formed the nano material of given shape and orientation during the course of the reaction during plant reduction,
This method is conducive to the pattern of further reinforced metal nano-particle product using both controls simultaneously.
4th, the present invention is effectively utilized reaction discarded object, has accomplished the nano metal material preparation method of environmental protection.
Brief description of the drawings
The graph of a relation in reaction product absorbance and reaction time in Fig. 1, embodiment 1 and comparative example 1；
Fig. 2, embodiment 4 prepare Nano Silver schematic device；
Wherein, 1, AgNO3Solution, 2, plant powder charge door, 3, pump and pre-mix reservoir, 4, snakelike reaction tube, 5, nanometer
Silver sol collects container；
The partial enlarged drawing of snakelike reaction tube in Fig. 3, Fig. 2 schematic device；
Wherein, 6, permanent magnet, and permanent magnet can substitute with electromagnetic field.
Embodiment
Following reaction raw materials are purchased in market.
Embodiment 1
The dry powder that crushing is made 500 ± 50 microns is carried out from fragrant camphor tree cured leaf, the composition of fragrant camphor tree leaf is as shown in table 1；
Take the fragrant camphor tree leaf dry powder of 0.1g to be mixed with 50mL concentration for 1.0mM silver nitrate solution, react enterprising in shaking bath
OK, reaction condition is 30 DEG C of reaction temperature, rotating speed 120rmin-1, alternating magnetic field magnetic field intensity 20-30mT, when react 24h when,
Ag+Percent reduction is 99.01%, and after reaction 130h, separation product and residue obtain nanometer Ag 5.30mg, and yield is 99.06%；
Silver nano-grain granularity 45-70nm, it is subsphaeroidal.
Raffinate and residue after reaction can be used for ferment preparation of sludge gas and fertilizer, and biogas can be used for generating electricity and heat production,
The energy is provided for above-mentioned reaction, fertilizer is used to improve fragrant camphor tree crop yield, so as to form the circulation technology of efficient green.
The fragrant camphor tree leaf polyol content of table 1
Comparative example 1
From fragrant camphor tree cured leaf dry powder same as Example 1, the fragrant camphor tree leaf dry powder of 0.1g and nitre of the 50mL concentration for 1.0mM are taken
Sour silver solution mixing, reaction is carried out on shaking bath, and reaction temperature is 30 DEG C, rotating speed is 120rmin-1, when reacting 24h
Ag+Percent reduction is 54.01%, and after reaction 130h, separation product and residue obtain nanometer Ag 3.60mg, and yield is 67.38%.
(result such as Fig. 1) is had found by the contrast of embodiment 1 and the reaction result of comparative example 1：Apply the reaction ratio behind magnetic field
Comparative example 1 is shortened using nanometer Ag output increased, saturation time in the case of same materials concentration and consumption；In fragrant camphor tree leaf addition
In the case of 0.1g, the effect in magnetic field is fairly obvious, and not only saturation time shortens 5 times, i.e., without absorbance knot after magnetic field conditions 130h
Fruit just shows stable saturation, and has 23h of the magnetic field reaction in figure to stablize saturation, and the reaction time greatly shortens, saturation production
Amount improves 2-3 times, and whole structure improves 15 times, and the output increased after saturation illustrates that magnetic field has and promotes AgNO3With plant into
Divide the effect of reaction, its saturation is unable to reach by improving fragrant camphor tree leaf consumption, and this process is by being fixed on container
Interior permanent magnet is provided, and extra energy is not consumed, the consumption for not having any matter and energy relative to the technique without magnetic field,
It is potentiality very huge technique but yield and efficiency are then greatly improved.
Embodiment 2
Maize straw is taken to be carried out crushing the dry powder for being made 1~10 micron, maize straw composition is as shown in table 2；
Take 0.5g maize straws dry powder to be mixed with 50mL concentration for 1.0mM silver nitrate solution, react on shaking bath
Carry out, reaction temperature be 30 DEG C, rotating speed be 120rmin-1, magnetic field intensity for 0.2-0.3T alternating magnetic field in, react 30h,
Separation product and residue, obtain 5.29mg nanometer Ags, and yield is 99.01%, silver nano-grain granularity 50-80nm, subsphaeroidal.
It can be fermented using the residue after reaction, as ruminant domestic animal feed, animal waste can be with compost fermentation
The biogas of acquisition；Or directly provide the energy, the biogas slurry of generation using the residue fermentation Biogas after reaction for above-mentioned reaction
For corn planting, the benign technique of environmental protection is formed.
The maize straw polyol content of table 2
Embodiment 3
Take 0.5g fragrant camphor tree leaf dry powder same as Example 1 and HAuCl of the 50mL concentration for 2.5mM4Solution is mixed, in magnetic
Field intensity places 30min for 1.5-2T steady magnetic field, is then departed from magnetic field and moves on on shaking bath, is in reaction temperature
10 DEG C, rotating speed be 150rmin-1Under the conditions of, 30h, separation product and residue are reacted, 9.80mg nanometers of Au are obtained, yield is
99.49%；Gold nano grain granularity 10-30nm, it is subsphaeroidal.
Residue after reaction can be used for ferment preparation of sludge gas and fertilizer, and biogas can be used for generating electricity and heat production, be above-mentioned
Reaction provides the energy, and fertilizer is used to improve fragrant camphor tree crop yield, so as to form the circulation technology of efficient green.
Embodiment 4
Take 3.0g maize straw dry powder same as Example 2 and HAuCl of the 50mL concentration for 1.0mM4Solution is mixed, instead
Answer device as shown in Figures 2 and 3, reaction is carried out on shaking bath, reaction temperature be 30 DEG C, shaking speed be 100rmin-1, magnetic field intensity under 0.5-1T steady magnetic field condition, to react 28h, separation product and residue obtain 9.79mg nanometer Au, receipts
Rate is 99.39%；Gold nano grain granularity 10-30nm, it is subsphaeroidal.
Then the stalk residue after reaction is used for reduced sugar, Feed Manufacturing.
Embodiment 5
The 1g safflower dry powder that granularity is 100 ± 10 microns is taken, is mixed with 50mL concentration for 1.0mM silver nitrate solution,
Magnetic field intensity is then departed from magnetic field and is transferred on shaking bath, anti-to place 10min in 11~12T steady magnetic field
To answer temperature be 10 DEG C, rotating speed is 150rmin-1Under the conditions of react 24h, separation product and residue, obtain 5.31mg nanometer Ags, yield
For 99.26%；Silver nano-grain granularity 45-70nm, it is subsphaeroidal.
Residue after reaction can be used for ferment preparation of sludge gas and fertilizer, and biogas can be used for generating electricity and heat production, be above-mentioned
Reaction provides the energy, and fertilizer is used to improve crop yield, so as to form the circulation technology of efficient green.
Embodiment 6
The 6g persimmon leaf dry powder that granularity is 50 ± 10 microns is taken, with the H that 40mL concentration is 5.0mM2PtCl6Mixing, in magnetic
Field intensity is then departed from magnetic field and is transferred on shaking bath to place 1h in 5~6T steady magnetic field, is 40 in reaction temperature
DEG C, rotating speed be 120rmin-1Under the conditions of react 26h, separation product and residue, obtain 30.42mg Pt nano particles, yield is
82.06%；Pt nanoparticle granularity 45-70nm, it is subsphaeroidal.
Residue after reaction can be used for ferment preparation of sludge gas and fertilizer, and biogas can be used for generating electricity and heat production, be above-mentioned
Reaction provides the energy, and fertilizer is used to improve crop yield, so as to form the circulation technology of efficient green.
Embodiment 7
The 2g sea-buckthorn leaf dried powders that granularity is 800~900 microns are taken, are 3.0mM PdCl with 50ml concentration2Solution is mixed, instead
Should be carried out on shaking bath, reaction temperature be 50 DEG C, rotating speed be 120rmin-1, 0.5~0.8T of magnetic field intensity steady magnetic
In, 24h, separation product and residue are reacted, 14.32mg nano Pd particles are obtained, yield is 90.06%；Palladium nano-particles granularity 2-
12nm, it is subsphaeroidal.
Residue after reaction can be used for ferment preparation of sludge gas and fertilizer, and biogas can be used for generating electricity and heat production, be above-mentioned
Reaction provides the energy, and fertilizer is used to improve crop yield, so as to form the circulation technology of efficient green.
Claims (6)
1. a kind of plant reduction method joint magnetic field prepares nano material and reaction twice laid method, it is characterised in that including such as
Lower step：
(1) particle diameter is taken to be mixed for micron-sized plant powder with metal salt solution, in the steady magnetic that magnetic field intensity H is 20mT~1T
24~30h is reacted in field or alternating magnetic field, nano metal product is obtained, then separation product and reaction discarded object；
Or, take particle diameter to be mixed for micron-sized plant powder with metal salt solution, in magnetic field intensity 1T ＜ H≤12T steady
Placed in magnetic field after 10~60min, under no magnetic field conditions, then react 24~30h, obtain nano metal product, Ran Houfen
From product and reaction discarded object；
(2) discarded object of reaction is subjected to fermentation process, the biogas or ethanol of generation are as the energy, in the reaction of step (1)
Use；Ferment produce biogas slurry or residue as reaction plant growth fertilizer nutrient；
(3) metal salt described in is Ag, Au, Pt or Pd nitrate or hydrochloride.
2. a kind of plant reduction method joint magnetic field according to claim 1 prepares nano material and reaction twice laid side
Method, it is characterised in that the addition ratio of metal ion is 1g in the plant powder and metal salt described in step (1)：
(0.0167-0.5)mmol。
3. a kind of plant reduction method joint magnetic field according to claim 1 prepares nano material and reaction twice laid side
Method, it is characterised in that the metal salt solution concentration described in step (1) is 1-5mmol/L.
4. a kind of plant reduction method joint magnetic field according to claim 1 prepares nano material and reaction twice laid side
Method, it is characterised in that the plant powder described in step (1) is the cauline leaf discarded object of crops.
5. a kind of plant reduction method joint magnetic field according to claim 1 prepares nano material and reaction twice laid side
Method, it is characterised in that the plant powder described in step (1) is fruit tree, views and admires the leaf of tree or shade tree.
6. a kind of plant reduction method joint magnetic field according to claim 1 prepares nano material and reaction twice laid side
Method, it is characterised in that the reaction temperature reacted described in step (1) is 10~50 DEG C, mixing speed is 100~150rmin-1。
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| CN101138792A (en) * | 2007-10-15 | 2008-03-12 | 吉林大学 | Novel process for preparing simple substance Fe nanometer particles at normal temperature and pressure in liquid phase original station |
| JP2010109184A (en) * | 2008-10-30 | 2010-05-13 | Toyota Motor Corp | MANUFACTURING METHOD OF Fe/FePd NANO COMPOSITE MAGNET |
| CN101912976A (en) * | 2010-08-24 | 2010-12-15 | 厦门大学 | Method for preparing silver nano granules by reducing plant extract |
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN103449623A (en) * | 2013-08-30 | 2013-12-18 | 武汉市硕隽科技有限公司 | Method for preparing metal nanometer material by recovering from industrial waste water |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101138792A (en) * | 2007-10-15 | 2008-03-12 | 吉林大学 | Novel process for preparing simple substance Fe nanometer particles at normal temperature and pressure in liquid phase original station |
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| JP2010109184A (en) * | 2008-10-30 | 2010-05-13 | Toyota Motor Corp | MANUFACTURING METHOD OF Fe/FePd NANO COMPOSITE MAGNET |
| CN101912976A (en) * | 2010-08-24 | 2010-12-15 | 厦门大学 | Method for preparing silver nano granules by reducing plant extract |
| CN103449623A (en) * | 2013-08-30 | 2013-12-18 | 武汉市硕隽科技有限公司 | Method for preparing metal nanometer material by recovering from industrial waste water |
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