CN104986752A - Preparation method and application of carbon aerogel - Google Patents
Preparation method and application of carbon aerogel Download PDFInfo
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- CN104986752A CN104986752A CN201510344508.8A CN201510344508A CN104986752A CN 104986752 A CN104986752 A CN 104986752A CN 201510344508 A CN201510344508 A CN 201510344508A CN 104986752 A CN104986752 A CN 104986752A
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Abstract
The invention relates to a preparation method and application of carbon aerogel and belongs to the technical field of carbon aerogel preparation. Serving as a nano-carbon fertilizer synergist, the carbon aerogel is applied to the aspect of plant growth regulation. The preparation method comprises the specific preparation process that a carbohydrate, a high polymer and an organic solvent are arranged in an airtight container to perform reaction at the temperature of 150-250 DEG C and are dried to obtain the carbon aerogel. The preparation method does not need a catalyzer in the carbon aerogel preparing process, and the duct blockage situations caused by uneven catalyzer distribution and residues are decreased. In addition, the preparation method has the advantages of being simple, low in cost and the like. The carbon aerogel prepared by means of the preparation method is high in purity, low in density and high in porosity, the carbon aerogel serving as the nano-carbon fertilizer synergist can promote plant growth, and the fertilizer application amount can be decreased.
Description
Technical field
The present invention relates to a kind of carbon aerogels preparation method and as the application of nano-sized carbon fertilizer synergist in coordinate plant growth, belong to carbon aerogels preparing technical field.
Background technology
Carbon aerogels is a kind of how empty amorphous condensed state material be made up of high-polymer molecular, has the pore size that high-ratio surface sum is controlled, can be used as sorbent material and be applied in the aspect such as sewage disposal, sea water desaltination.In addition, carbon aerogels has the performances such as density is low, excellent conductivity, has broad application prospects in new forms of energy battery and ultracapacitor.
The method that tradition prepares carbon aerogels is catalyzer mainly with sodium carbonate, through a series of processes such as sol-gel, drying, carbonizations, forms the carbon materials of porous amorphous structure.Studies have reported that employing magnesium salts is catalyzer recently, obtained the carbon aerogels of spheroidal particle structure.It is that the carbon aerogels TEM figure that catalyzer obtains presents big area worm-eaten form that meter second place etc. have studied with magnesium hydroxide, is that the carbon aerogels that catalyzer obtains presents continuously granular with magnesium acetate.He Rui etc. using ammoniacal liquor as the catalyzer of Resorcinol and formaldehyde reaction, through preparation of sol-gel organic aerogel, drier through normal temperature and pressure, that high temperature cabonization forms continuous particulate shape carbon aerogels.Visible, the structure of raw material to carbon aerogels has a certain impact.
Summary of the invention
The object of the present invention is to provide a kind of carbon aerogels preparation method and as the application of nano-sized carbon fertilizer synergist in coordinate plant growth.
Implementation procedure of the present invention is as follows:
A kind of preparation method of carbon aerogels: in encloses container, by saccharide compound, superpolymer and organic solvent after 150 ~ 250 DEG C of reactions, drying obtains carbon aerogels, described saccharide compound is selected from monose or disaccharides, and described superpolymer is selected from polyvinylpyrrolidone, polyacrylic acid, polyacrylamide, polyoxyethylene glycol, polyvinyl alcohol.
Described saccharide compound is selected from glucose, fructose, semi-lactosi, sucrose, maltose, lactose.
Described organic solvent is selected from formic acid, acetic acid, propionic acid, methyl alcohol, ethanol, ethylene glycol, Virahol, butanols, acetonitrile, methylene dichloride, chloroform, N, dinethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide (DMSO), thionyl chloride, N-Methyl pyrrolidone.
The mass ratio of saccharide compound, superpolymer and organic solvent is 1:1:5 ~ 1:0.1:0.5, and temperature of reaction is 160 ~ 200 DEG C.
The drying of above-mentioned carbon aerogels adopts lyophilize or CO 2 supercritical drying.
Above-mentioned carbon aerogels can further under an inert atmosphere through 300 ~ 1200 DEG C of calcination processing.
The carbon aerogels that above-mentioned preparation method obtains can be used as nano-sized carbon fertilizer synergist and is applied to coordinate plant growth aspect.
Advantage of the present invention and positively effect: (1) the present invention prepares carbon aerogels without the need to adding catalyzer, decrease the uneven and residual duct blocking caused of catalyst distribution; (2) the inventive method is simple to operate, cost is low, and the carbon aerogels purity prepared is high, and density is low, porosity is high; (3) carbon aerogels prepared of the inventive method can not only Promoting plant growth as nano-sized carbon fertilizer synergist, can also reduce rate of fertilizer.
Accompanying drawing explanation
The cylindric gel photograph of Fig. 1 prepared by embodiment 1,4,13;
The powder diagram of the carbon aerogels of Fig. 2 prepared by embodiment 1;
The infrared figure of the carbon aerogels of Fig. 3 prepared by embodiment 1;
The x-ray photoelectron spectroscopy figure of the carbon aerogels of Fig. 4 prepared by embodiment 1.
Embodiment
Embodiment 1
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL glacial acetic acid, react 8 hours at 200 DEG C, obtain cylindric gel after reaction terminates and see Fig. 1 (a), gel after lyophilize in a nitrogen atmosphere 1000 DEG C of calcinings within 3 hours, obtain carbon aerogels, its 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 ~ and 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, in figure, a is full spectrogram, b is carbon spectrum, prepared carbon aerogels is found out mainly containing C, N, O tri-kinds of elements from a figure, find out that C1s peak can be made up of at two sub-peaks of 285.5 eV, 288.1 eV combination from b figure, these two sub-peaks correspond to C-C and-COOH respectively.Can find out that prepared carbon aerogels is rich in the functional groups such as-OH ,-COOH from above-mentioned sign.
Embodiment 2
In closed reactor, add 1g fructose, 0.1g polyacrylic acid and 0.5mL formic acid, react 8 hours at 160 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after CO 2 supercritical drying.
Embodiment 3
In closed reactor, add 1g maltose, 0.1g polyacrylamide and 3mL ethylene glycol, at 200 DEG C react 8 hours, reaction terminate after obtain cylindric gel, gel after lyophilize in a nitrogen atmosphere 300 DEG C of calcinings within 4 hours, obtain carbon aerogels.
Embodiment 4
In closed reactor, add 1g lactose, 0.5g polyvinyl alcohol and 3mL ethanol, react 4 hours at 250 DEG C, obtain cylindric gel after reaction terminates and see Fig. 1 (b), gel obtains carbon aerogels after lyophilize.
Embodiment 5
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL butanols, react 8 hours at 200 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after lyophilize.
Embodiment 6
In closed reactor, add 1g semi-lactosi, 0.1g polyacrylic acid and 3mL propionic acid, react 8 hours at 180 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after lyophilize.
Embodiment 7
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL acetonitrile, at 200 DEG C react 8 hours, reaction terminate after obtain cylindric gel, gel after lyophilize in a nitrogen atmosphere 1200 DEG C of calcinings within 1 hour, obtain carbon aerogels.
Embodiment 8
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL methylene dichloride, react 8 hours at 200 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after lyophilize.
Embodiment 9
In closed reactor, add 1g sucrose, 0.1g polyvinylpyrrolidone (K30) and 3mL chloroform, react 8 hours at 200 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after lyophilize.
Embodiment 10
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL N, dinethylformamide, react 8 hours at 200 DEG C, reaction terminate after obtain cylindric gel, gel after lyophilize in a nitrogen atmosphere 800 DEG C of calcinings within 3 hours, obtain carbon aerogels.
Embodiment 11
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL N,N-dimethylacetamide, react 8 hours at 200 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after lyophilize.
Embodiment 12
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL dimethyl sulfoxide (DMSO), react 8 hours at 200 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after lyophilize.
Embodiment 13
In closed reactor, add 1g sucrose, 1g polyoxyethylene glycol (PEG-4000) and 2mL methyl alcohol, react 8 hours at 200 DEG C, obtain cylindric gel after reaction terminates and see Fig. 1 (c), gel obtains carbon aerogels after lyophilize.
Embodiment 14
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL thionyl chloride, at 200 DEG C react 8 hours, reaction terminate after obtain cylindric gel, gel after lyophilize in a nitrogen atmosphere 500 DEG C of calcinings within 2 hours, obtain carbon aerogels.
Embodiment 15
In closed reactor, add 1g glucose, 0.1g polyvinylpyrrolidone (K30) and 3mL N-Methyl pyrrolidone, react 8 hours at 200 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after lyophilize.
Embodiment 16
In closed reactor, add 1g glucose, 1g polyvinylpyrrolidone (K30) and 5mL Virahol, react 10 hours at 150 DEG C, obtain cylindric gel after reaction terminates, gel obtains carbon aerogels after lyophilize.
Embodiment 17 carbon aerogels is as the application of nano-sized carbon fertilizer synergist in coordinate plant growth
(1) nano-sized carbon working concentration indoor pot experiment
By the rate of fertilizer application of soybean every mu rate of fertilizer application conversion indoor pot, the massfraction then carbon aerogels prepared by embodiment 1 being mixed with carbon is respectively 0,0.5 ‰, 1 ‰, 3 ‰, the nano-sized carbon fertilizer synergist of 5 ‰, each process arranges 5 basins, the strain of every basin 5, cultivates 45 days.Test soybean whole plant biomass, statistical study.
Table 1 carbon aerogels is as the evaluating data table of nano-sized carbon fertilizer synergist coordinate plant growth
As can be seen from Table 1, carbon aerogels has the effect of Promoting plant growth as nano-sized carbon fertilizer synergist, but when nano-sized carbon concentration increases to 5 ‰, the growth velocity of large bean seedlings reduces on the contrary, illustrate the massfraction of carbon be 3 ‰ nano-sized carbon fertilizer synergist can remarkable Promoting plant growth.
(2) fertilizer decrement indoor pot experiment
Be suitable for based on adding proportion 3 ‰ by nano-sized carbon fertilizer synergist, the Term Fertilization of 100%, 70% be set and add the Term Fertilization process of nano-sized carbon fertilizer synergist 3 ‰, each process 5 basin, the strain of every basin 5, cultivate 45 days, test soybean whole plant biomass, statistical study.
Table 2 carbon aerogels is as the evaluating data table of nano-sized carbon fertilizer synergist coordinate plant growth
As can be seen from Table 2, compared with normally apply fertilizer (namely 100%), after increasing the fertile synergistic agent of 3 ‰ nano-sized carbon, the fresh weight of large bean seedlings adds 2.1g, when rate of fertilizer application is kept to 70%, add 3 ‰ nano-sized carbon fertilizer synergists in fertilizer after, the fresh weight 1.5g heavier than normal fertilising (namely 100%) of large bean seedlings, illustrates that carbon aerogels can reduce rate of fertilizer application as nano-sized carbon fertilizer synergist while Promoting plant growth.
Claims (8)
1. a preparation method for carbon aerogels, is characterized in that: in encloses container, and by saccharide compound, superpolymer and organic solvent after 150 ~ 250 DEG C of reactions, drying obtains carbon aerogels,
The mass ratio of described saccharide compound, superpolymer and organic solvent is 1:1:5 ~ 1:0.1:0.5; Described saccharide compound is selected from monose or disaccharides, and described superpolymer is selected from polyvinylpyrrolidone, polyacrylic acid, polyacrylamide, polyoxyethylene glycol, polyvinyl alcohol.
2. the preparation method of carbon aerogels according to claim 1, is characterized in that: described saccharide compound is selected from glucose, fructose, semi-lactosi, sucrose, maltose, lactose.
3. the preparation method of carbon aerogels according to claim 1, it is characterized in that: described organic solvent is selected from formic acid, acetic acid, propionic acid, methyl alcohol, ethanol, ethylene glycol, Virahol, butanols, acetonitrile, methylene dichloride, chloroform, N, dinethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide (DMSO), thionyl chloride, N-Methyl pyrrolidone.
4. the preparation method of carbon aerogels according to claim 1, is characterized in that: temperature of reaction is 160 ~ 200 DEG C.
5. the preparation method of carbon aerogels according to claim 1, is characterized in that: dry employing lyophilize or CO 2 supercritical drying.
6. the preparation method of carbon aerogels according to claim 1, is characterized in that: carbon aerogels is further under an inert atmosphere through 300 ~ 1200 DEG C of calcination processing.
7. the carbon aerogels for preparing of preparation method described in claim 1.
8. carbon aerogels described in claim 7 is as the application of nano-sized carbon fertilizer synergist in coordinate plant growth.
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Cited By (10)
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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 |
| CN106396842A (en) * | 2016-08-26 | 2017-02-15 | 和县常久农业发展有限公司 | Watermelon high efficiency fertilizer with added carbon aerogel carrying brassinolide 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 |
| 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 |
| CN106431605A (en) * | 2016-08-26 | 2017-02-22 | 和县常久农业发展有限公司 | Efficient fertilizer added with small molecule pigment carbon aerogel for watermelons and preparation method of fertilizer |
| 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 |
| 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 |
| 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 |
| 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 |
| CN108622871A (en) * | 2017-03-17 | 2018-10-09 | 南开大学 | It is a kind of to use polyaniline as the organic aerogel of crosslinking agent and the preparation method of charcoal-aero gel |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106396842A (en) * | 2016-08-26 | 2017-02-15 | 和县常久农业发展有限公司 | Watermelon high efficiency fertilizer with added carbon aerogel carrying brassinolide and preparation method thereof |
| CN106431605A (en) * | 2016-08-26 | 2017-02-22 | 和县常久农业发展有限公司 | Efficient fertilizer added with small molecule pigment carbon aerogel for watermelons and preparation method of fertilizer |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN108622871A (en) * | 2017-03-17 | 2018-10-09 | 南开大学 | It is a kind of to use polyaniline as the organic aerogel of crosslinking agent and the preparation method of charcoal-aero gel |
| 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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