CN104986752B - A kind of preparation method of carbon aerogels and application - Google Patents
A kind of preparation method of carbon aerogels and application Download PDFInfo
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Abstract
Application the present invention relates to a kind of preparation method of carbon aerogels and its as nano-sized carbon fertilizer synergist in terms of coordinate plant growth, belongs to carbon aerogels preparing technical field.Its specific preparation process is as follows：In closed container, by saccharide compound, high polymer and organic solvent after 150~250 DEG C of reactions, through being dried to obtain carbon aerogels.The method of the present invention, which prepares carbon aerogels, need not add in catalyst, and duct caused by reducing catalyst distribution unevenness and residual blocks；Have many advantages, such as that preparation method is simple, at low cost simultaneously.Carbon aerogels purity that the method for the present invention is prepared is high, density is low, porosity is high, can not only promote plant growth as nano-sized carbon fertilizer synergist, moreover it is possible to reduce rate of fertilizer.
Description
Technical field
Plant life is being adjusted the present invention relates to a kind of preparation method of carbon aerogels and its as nano-sized carbon fertilizer synergist
The application of long side belongs to carbon aerogels preparing technical field.
Background technology
Carbon aerogels are a kind of more empty amorphous condensed state materials being made of high-polymer molecular, have high-specific surface area and can
The pore size of control can be applied as adsorbent in sewage disposal, sea water desalination etc..In addition, carbon aerogels have density
The performances such as low, excellent conductivity have broad application prospects in terms of new energy battery and ultracapacitor.
Tradition prepares the method for carbon aerogels mostly using sodium carbonate as catalyst, through a system such as sol-gel, drying, carbonization
Row process forms the carbon materials of porous impalpable structure.Recently studies have reported that using the magnesium salts to obtain ball for catalyst
The carbon aerogels of shape grain structure.Meter second place etc. has studied to scheme to present by the carbon aerogels TEM that catalyst obtains of magnesium hydroxide
Large area worm-eaten form is presented continuous granular using magnesium acetate as the carbon aerogels that catalyst obtains.He Rui etc. is using ammonium hydroxide between
Benzenediol and the catalyst of formaldehyde reaction, organic aerogel is prepared through sol-gel, using normal temperature and pressure drying, pyrocarbon
Change the carbon aerogels for forming continuous particulate shape.As it can be seen that raw material has a certain impact to the structure of carbon aerogels.
The content of the invention
Exist it is an object of the invention to provide a kind of preparation method of carbon aerogels and its as nano-sized carbon fertilizer synergist
Application in terms of coordinate plant growth.
The realization process of the present invention is as follows：
A kind of preparation method of carbon aerogels：In closed container, saccharide compound, high polymer and organic solvent are existed
After 150~250 DEG C of reactions, through being dried to obtain carbon aerogels, the saccharide compound is selected from monose or disaccharides, and the height gathers
Object is selected from polyvinylpyrrolidone, polyacrylic acid, polyacrylamide, polyethylene glycol, polyvinyl alcohol.
The saccharide compound is selected from glucose, fructose, galactolipin, sucrose, maltose, lactose.
The organic solvent is selected from formic acid, acetic acid, propionic acid, methanol, ethyl alcohol, ethylene glycol, isopropanol, butanol, acetonitrile, two
Chloromethanes, chloroform, n,N-Dimethylformamide, n,N-dimethylacetamide, dimethyl sulfoxide (DMSO), thionyl chloride, N- methylpyrroles
Alkanone.
The mass ratio of saccharide compound, high polymer and organic solvent is 1：1：5~1：0.1：0.5, reaction temperature for 160~
200℃。
The dry of above-mentioned carbon aerogels is dried using freeze-drying or CO 2 supercritical.
Above-mentioned carbon aerogels can further pass through 300~1200 DEG C of calcination processings under an inert atmosphere.
The carbon aerogels that above-mentioned preparation method obtains can be used as nano-sized carbon fertilizer synergist to be applied to coordinate plant growth side
Face.
Advantages of the present invention and good effect：（1）The present invention, which prepares carbon aerogels, need not add in catalyst, reduce catalysis
Duct caused by agent is unevenly distributed and remains blocks；（2）The method of the present invention is easy to operate, at low cost, the carbon airsetting being prepared
Glue purity is high, and density is low, porosity is high；（3）The method of the present invention prepare carbon aerogels as nano-sized carbon fertilizer synergist not only
It can promote plant growth, moreover it is possible to reduce rate of fertilizer.
Description of the drawings
Fig. 1 is the cylindric gel photograph prepared by embodiment 1,4,13；
Fig. 2 is the powder diagram of the carbon aerogels prepared by embodiment 1；
Fig. 3 is the infrared figure of the carbon aerogels prepared by embodiment 1；
Fig. 4 is the x-ray photoelectron spectroscopy figure of the carbon aerogels prepared by embodiment 1.
Specific embodiment
Embodiment 1
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL glacial acetic acids,
When reaction 8 is small at 200 DEG C, cylindric gel is obtained after reaction and sees Fig. 1（a）, in nitrogen atmosphere after gel is freeze-dried
Lower 1000 DEG C of calcinings 3 obtain carbon aerogels when small, and powder diagram is shown in Fig. 2, it can thus be appreciated that prepared carbon aerogels is non-
Crystalline state；Its infared spectrum is shown in Fig. 3, in figure~3411.5cm-1For the peak of-OH ,~1660 cm-1For the peak of C=O and C=C ,~
1282.8 cm-1For the peak of C-OH；Its x-ray photoelectron spectroscopy figure is shown in Fig. 4, and a is full spectrogram in figure, and b is carbon spectrum, in terms of a figures
Go out prepared carbon aerogels and mainly contain tri- kinds of elements of C, N, O, from b figures find out C1s peaks be by combine can 285.5 eV,
Two sub- peak compositions of 288.1 eV, the two sub- peaks correspond to C-C and-COOH respectively.It can be seen that from above-mentioned characterization made
Standby carbon aerogels are rich in functional groups such as-OH ,-COOH.
Embodiment 2
In closed reactor, 1g fructose, 0.1g polyacrylic acid and 0.5mL formic acid are added in, it is small that 8 are reacted at 160 DEG C
When, cylindric gel is obtained after reaction, and gel obtains carbon aerogels after CO 2 supercritical is dried.
Embodiment 3
In closed reactor, 1g maltose, 0.1g polyacrylamides and 3mL ethylene glycol are added in, reacts 8 at 200 DEG C
Hour, cylindric gel is obtained after reaction, is obtained when 300 DEG C of calcinings 4 are small in a nitrogen atmosphere after gel is freeze-dried
Carbon aerogels.
Embodiment 4
In closed reactor, 1g lactose, 0.5g polyvinyl alcohol and 3mL ethyl alcohol are added in, when reaction 4 is small at 250 DEG C,
Cylindric gel is obtained after reaction sees Fig. 1（b）, carbon aerogels are obtained after gel is freeze-dried.
Embodiment 5
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL butanol, 200
When reaction 8 is small at DEG C, cylindric gel is obtained after reaction, carbon aerogels are obtained after gel is freeze-dried.
Embodiment 6
In closed reactor, 1g galactolipins, 0.1g polyacrylic acid and 3mL propionic acid are added in, it is small that 8 are reacted at 180 DEG C
When, cylindric gel is obtained after reaction, and carbon aerogels are obtained after gel is freeze-dried.
Embodiment 7
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL acetonitriles, 200
At DEG C reaction 8 it is small when, obtain cylindric gel after reaction, after gel is freeze-dried in a nitrogen atmosphere 1200 DEG C forge
Burn 1 it is small when obtain carbon aerogels.
Embodiment 8
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL dichloromethane,
When reaction 8 is small at 200 DEG C, cylindric gel is obtained after reaction, carbon aerogels are obtained after gel is freeze-dried.
Embodiment 9
In closed reactor, 1g sucrose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL chloroforms, at 200 DEG C
It is lower reaction 8 it is small when, obtain cylindric gel after reaction, carbon aerogels obtained after gel is freeze-dried.
Embodiment 10
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL N, N- dimethyl
Formamide when reaction 8 is small at 200 DEG C, obtains cylindric gel, in nitrogen gas after gel is freeze-dried after reaction
The lower 800 DEG C of calcinings 3 of atmosphere obtain carbon aerogels when small.
Embodiment 11
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL N, N- dimethyl
Acetamide when reaction 8 is small at 200 DEG C, obtains cylindric gel, carbon gas is obtained after gel is freeze-dried after reaction
Gel.
Embodiment 12
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL dimethyl sulfoxide (DMSO)s,
When reaction 8 is small at 200 DEG C, cylindric gel is obtained after reaction, carbon aerogels are obtained after gel is freeze-dried.
Embodiment 13
In closed reactor, 1g sucrose, 1g polyethylene glycol are added in（PEG-4000）With 2mL methanol, reacted at 200 DEG C
8 it is small when, obtain cylindric gel after reaction and see Fig. 1（c）, carbon aerogels are obtained after gel is freeze-dried.
Embodiment 14
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL thionyl chlorides,
When reaction 8 is small at 200 DEG C, cylindric gel is obtained after reaction, 500 DEG C in a nitrogen atmosphere after gel is freeze-dried
Calcine 2 it is small when obtain carbon aerogels.
Embodiment 15
In closed reactor, 1g glucose, 0.1g polyvinylpyrrolidones are added in（K30）With 3mL N- methylpyrroles
Alkanone when reaction 8 is small at 200 DEG C, obtains cylindric gel, carbon airsetting is obtained after gel is freeze-dried after reaction
Glue.
Embodiment 16
In closed reactor, 1g glucose, 1g polyvinylpyrrolidones are added in（K30）With 5mL isopropanols, 150
When reaction 10 is small at DEG C, cylindric gel is obtained after reaction, carbon aerogels are obtained after gel is freeze-dried.
Application of 17 carbon aerogels of embodiment as nano-sized carbon fertilizer synergist in terms of coordinate plant growth
（1）Nano-sized carbon concentration indoor pot experiment
By the dose of soybean dose conversion indoor pot per acre, the carbon aerogels for then preparing embodiment 1 are prepared
Mass fraction into carbon is respectively 0,0.5 ‰, 1 ‰, 3 ‰, 5 ‰ nano-sized carbon fertilizer synergist, and each processing sets 5 basins, often
5 plants of basin is cultivated 45 days.Test soybean whole plant biomass, statistical analysis.
Evaluating data table of 1 carbon aerogels of table as nano-sized carbon fertilizer synergist coordinate plant growth
As it can be seen from table 1 carbon aerogels play an important role of to promote plant growth as nano-sized carbon fertilizer synergist, still
When nanometer concentration of carbon increases to 5 ‰, the growth rate of big bean seedlings reduces instead, and the mass fraction for illustrating carbon is 3 ‰ nanometer
Carbon fertilizer synergist can remarkably promote plant growth.
（2）Fertilizer is reduced indoor pot experiment
By nano-sized carbon fertilizer synergist suitable for adding proportion 3 ‰ based on, set 100%, 70% fertilizer application and addition
The fertilizer application processing of nano-sized carbon fertilizer synergist 3 ‰, it is each to handle 5 basins, it per 5 plants of basin, cultivates 45 days, tests soybean whole plant
Biomass, statistical analysis.
Evaluating data table of 2 carbon aerogels of table as nano-sized carbon fertilizer synergist coordinate plant growth
From table 2 it can be seen that it applies fertilizer with normal（I.e. 100%）It compares, after increasing by 3 ‰ nano-sized carbon fertilizer synergist, big bean seedlings
Fresh weight adds 2.1g, when dose is kept to 70%, in fertilizer add in 3 ‰ nano-sized carbon fertilizer synergists after, big bean seedlings it is fresh
Again than normally applying fertilizer（I.e. 100%）Weight 1.5g illustrates that carbon aerogels are promoting the same of plant growth as nano-sized carbon fertilizer synergist
When can reduce dose.
Claims (3)
1. a kind of preparation method of carbon aerogels, it is characterised in that：In closed container, by saccharide compound, high polymer and have
Solvent is after 150~250 DEG C of reactions, after the drying of freeze-dried or CO 2 supercritical, under an inert atmosphere by 300
~1200 DEG C of calcination processings, obtain carbon aerogels,
The organic solvent is selected from formic acid, acetic acid, propionic acid, methanol, ethyl alcohol, ethylene glycol, isopropanol, butanol, acetonitrile, dichloromethane
Alkane, chloroform, n,N-Dimethylformamide, n,N-dimethylacetamide, dimethyl sulfoxide (DMSO), thionyl chloride, N-Methyl pyrrolidone；
The mass ratio of the saccharide compound, high polymer and organic solvent is 1：1：5~1：0.1：0.5；The carbohydrate chemical combination
Object be selected from monose or disaccharides, the high polymer be selected from polyvinylpyrrolidone, polyacrylic acid, polyacrylamide, polyethylene glycol,
Polyvinyl alcohol.
2. the preparation method of carbon aerogels according to claim 1, it is characterised in that：The saccharide compound is selected from grape
Sugar, fructose, galactolipin, sucrose, maltose, lactose.
3. the preparation method of carbon aerogels according to claim 1, it is characterised in that：Reaction temperature is 160~200 DEG C.
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| CN106365785A (en) * | 2016-08-26 | 2017-02-01 | 和县常久农业发展有限公司 | High-effective fertilizer for strawberries with addition of active functional bacteria carbon aerogel and preparation method thereof |
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| CN106565289A (en) * | 2016-11-01 | 2017-04-19 | 马鞍山科邦生态肥有限公司 | Efficient melon fertilizer in which photosynthetic induction factor nutrient carbon aerogel is added and preparing method |
| CN106565315A (en) * | 2016-11-01 | 2017-04-19 | 马鞍山科邦生态肥有限公司 | Efficient blueberry fertilizer with natural sterilizing carbon aerogel added and preparation method |
| CN106431703A (en) * | 2016-11-01 | 2017-02-22 | 马鞍山科邦生态肥有限公司 | High-efficiency apple fertilizer with addition of onion oil carbon aerogel and preparation method of fertilizer |
| CN106565369A (en) * | 2016-11-01 | 2017-04-19 | 马鞍山科邦生态肥有限公司 | Efficient muskmelon fertilizer with plant active extract carbon aerogel added and preparation method |
| CN106431768A (en) * | 2016-11-01 | 2017-02-22 | 马鞍山科邦生态肥有限公司 | Banana high-efficiency fertilizer with mouthfeel-improving carbon aerogel and preparation method thereof |
| CN106431704A (en) * | 2016-11-01 | 2017-02-22 | 马鞍山科邦生态肥有限公司 | Efficient lemon fruit fertilizer with addition of tea polyphenol carbon aerogel and preparation method of efficient lemon fruit fertilizer |
| CN108622871B (en) * | 2017-03-17 | 2021-05-07 | 南开大学 | Preparation method of carbon aerogel by using polyaniline as cross-linking agent |
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