CN106390934B - A kind of high-ratio surface dopamine silkworm excrement carbon composite and the preparation method and application thereof - Google Patents
A kind of high-ratio surface dopamine silkworm excrement carbon composite and the preparation method and application thereof Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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Abstract
The invention discloses a kind of high-ratio surface dopamine silkworm excrement carbon composites and the preparation method and application thereof.Faeces bombycis is first prepared into carbonization silkworm excrement under protective gas;Dopamine hydrochloride powder and carbonization silkworm excrement are mixed again, ZnCl is added2Solution is placed in high speed machine ball mill oscillation activated grafting and reacts to obtain dopamine/ZnCl2/ silkworm excrement slurry, slurry is directly dried and obtains composite material crude product;Composite material crude product is carried out to activation reaming reaction under protective gas again, high-ratio surface dopamine silkworm excrement carbon composite is obtained after then cleaning, be centrifuged and drying again.The material can be applied to pesticide and delay controlled release aspect.The present invention carries out Dopamine hydrochloride and silkworm excrement to be grafted compound and activator ZnCl using high speed machine oscillation2Mixing and primary activation, significantly promoted two kinds of materials grafting recombination reaction speed and activator silkworm excrement composite material surface dispersion degree, obtained carbon composite specific surface area with higher and polar group containing N, can there is higher adsorption capacity and preferable slow-releasing and controlled-releasing action to pesticide.
Description
Technical field
The invention belongs to carbon composite technical fields, and in particular to dopamine silkworm excrement composite material and preparation method with
Using.
Background technique
Pesticide can efficiently control the harm of disease, worm, grass and other harmful organisms to crops, it is as chemical prevention
Important means, play irreplaceable role in agricultural production.However, pesticide only a small amount of in specific time can arrive
Up to crop target site, and most of pesticide is directly released into natural environment and causes pesticide utilization efficiency low.This part is not
The pesticide for playing drug effect can cause Practice for Pesticide Residue in Agricultural Products exceeded, injury and environmental pollution to non-target organism etc. many negative
Face problem.The utilization efficiency and Targeting delivery function for how effectively improving pesticide are urgently to be resolved main of current pesticide field
One of problem.
Slow controlled-release technology is that one kind can be such that pesticide activity component slowly releases within given time by physically or chemically means
It is put in target site, and drug concentration is made to maintain the novel medicine feeding technology of effective concentration or more in a long time, and it is biological
Porous charcoal is one of the main representative that can be applied to slow controlled-release technology.Silkworm excrement is the main waste of silkworm industry, is passed through in rural area
Chang Suiyi discarding lead to environmental pollution, from Electron microscope from known to its with natural three-dimensional drape structure and phosphorus content height,
High-ratio surface multiporous biological charcoal, and its surface N (O) group also rich in can be obtained through high temperature cabonization and activation.DOPA
Amine is also a kind of phosphorus content height and nitrogenous biomolecule, is widely present in marine mussel surface layer, is marine mussel processing institute
The carbon source material of a kind of by-product and sustainable (renewable) acquisition of the mankind that obtain.
In conventional pesticide molecule mostly containing polar group (carboxyl, carbonyl, sulfur-bearing and containing cl radical etc.), and this portion
Polarity group is also the dominant reactive part in pesticide, these polar groups can be with N (O) group in silkworm excrement, dopamine
In conjunction with.If silkworm excrement, dopamine to be combined into new porous carbon material, while adjusting porous charcoal pore size and N (O) group contains
Amount can regulate and control the adsorption capacity of pesticide and Carbon Materials, reach the slow-releasing and controlled-releasing action to pesticide.
Summary of the invention
The invention proposes a kind of high-ratio surface dopamine silkworm excrement carbon composites and the preparation method and application thereof, using height
Fast mechanical oscillation method can make dopamine and silkworm excrement in dozens of minutes while quick graft reaction, by activator ZnCl2
Sufficiently with dopamine/silkworm excrement composite material mixes and primary activation, then by high-temperature activation counter-boring techniques high-ratio surface is formed, together
When achieve the purpose that regulate and control N (O) group content.Which not only improves the combined coefficienies of material, and can increase substantially compound
The yield of material realizes the purpose of slow controlled release.
The purpose of the present invention is achieved through the following technical solutions:
A kind of high-ratio surface dopamine silkworm excrement carbon composite, the three-dimensional apertures which is constituted with dopamine and charing silkworm excrement
Gap structure, Langmuir specific surface area are 1000-1400m2/ g, total pore volume is in 0.3-0.6cm3/ g, wherein micropore specific area
The 50~70% of total specific surface area and Kong Rong are accounted for Kong Rong.
The preparation method of high-ratio surface dopamine silkworm excrement composite material of the invention, includes the following steps:
(1) in N2, Faeces bombycis passed through into high temperature cabonization reaction preparation carbonization silkworm excrement in the protective gas such as Ar atmosphere;
(2) ZnCl for being 0.25~0.30g/mL by Dopamine hydrochloride powder, carbonization silkworm excrement and mass concentration2Solution is mixed
It closes, is placed in high speed machine oscillation ball mill sealing oscillation, speed control is in 1000~2000 turns/min, and the graft reaction time is 30
~60min obtains dopamine/ZnCl2/ silkworm excrement slurry, then slurry is directly dried obtain composite material crude product;
(3) composite material crude product acquired in step (2) is subjected to reaming reaction in protective gas, it is then clear again
High-ratio surface dopamine charcoal silkworm excrement carbon composite is obtained after washing, be centrifuged and drying.Cleaning uses dilute hydrochloric acid and deionized water
It rinses 1~3 time.
As the further preferred of scheme, the carburizing temperature of Faeces bombycis is at 500-1000 DEG C in step (1), the reaction time 2
~4h.
As the further preferred of scheme, Dopamine hydrochloride powder and the quality that mixes of carbonization silkworm excrement in the step (2)
Than for 1:(1~6).
As the further preferred of scheme, carbonization silkworm excrement and ZnCl in the step (2)2The plastid ratio of solution be 1:(4~
10)。
As the further preferred of scheme, the reaming reaction temperature is 500~700 DEG C, and the reaction time is 0.5~5h.
Optimum reaction condition is that reaming reaction temperature is 550~650 DEG C, and the reaction time is 2~3h.
High-ratio surface dopamine silkworm excrement carbon composite of the invention can be applicable to medicine sustained and controlled release aspect, especially pesticide
In terms of slow controlled release.
Product of the present invention, which is applied, delays controlled release field in pesticide, adsorbs anabasine pesticide Diacloden using the composite material,
Absorption carriage amount can reach 500mg/g or more, and can prepare and delay controlled release farm chemical carrier within the scope of 15~60 days effective time of sustained release
(using 90% Diacloden of total volume as endpoint calculation).
Compared with prior art, the present invention is advantageous in that:
1. mechanical energy produced by the present invention is vibrated using high speed machine can quickly cause between dopamine and carbonization silkworm excrement
Chemical reaction significantly promotes graft reaction speed of the dopamine on carbonization silkworm excrement and greatly shortens the reaction time, while again
It can be lost to avoid brought product is filtered.
2. compared to the hydro-thermal of existing composite material or solvent-thermal method etc., Mechanical Method synthetic method preparation of the present invention
Dopamine silkworm excrement activated carbon composite can greatly reduce the usage amount to solvent, can effectively reduce waste liquid discharging amount, make synthesis of the present invention
Process is more environmentally protective, and the harm to environment has been reduced or avoided.
3. the present invention, which prepares dopamine silkworm excrement activated carbon composite by Mechanical Method, can directly obtain composite material crude product, it is added simultaneously
ZnCl2Solution is soaked, first is that can be rotated by the quick of mechanical activation by ZnCl2It is sufficiently mixed with dopamine/silkworm excrement material
It closes;Second is that passing through the superelevation mechanical energy and temperature ZnCl that instant shock generates when mechanical activation2Composite material is carried out preliminary
Activation, while without further being separated to solution, the process of solution separation is eliminated, efficiency is improved.
4. the raw materials used in the present invention silkworm excrement has native three dimensional pleated structure and contains a large amount of carboxyls, hydroxyl and amino base
Group, can be grafted the micro scale channel formed after its carbonization treatment to form dopamine silkworm excrement carbon composite with dopamine, then lead to
Cross ZnCl2Activation can form high-ratio surface porous structure on the composite, can there is higher adsorption capacity to pesticide.
Composite material surface group containing N can have an important influence on the adsorption capacity between pesticide and composite material simultaneously, due to dopamine
It is high compound containing N, the graft reaction ratio by adjusting silkworm excrement and dopamine can control composite material surface group containing N
Quantity, and then regulate and control the adsorption capacity between pesticide and composite material, achieve the purpose that slow controlled release.
5. composite material prepared by the present invention is for adsorbing anabasine pesticide Diacloden, adsorbance can reach
500mg/g or more can prepare sustained-release pesticides of the slow-release time within the scope of 15~60 days by regulating and controlling dopamine graft ratio
Carrier (using 90% Diacloden of total volume as endpoint calculation).
Detailed description of the invention
Fig. 1 is Faeces bombycis electron-microscope scanning figure.
Fig. 2 is 1 high-ratio surface dopamine silkworm excrement carbon composite electron-microscope scanning figure of embodiment.
Fig. 3 difference slow-release material load capacity curve.
Fig. 4 difference slow-release material is sustained release profiles.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and examples, but the scope of protection of present invention is not
It is confined to the range of embodiment statement.
Embodiment 1
A kind of preparation method of high-ratio surface dopamine silkworm excrement composite material, includes the following steps,
(1) in N210.0g Faeces bombycis is raised to 500 DEG C with the heating rate of 5 DEG C/min in atmosphere, and is protected at 500 DEG C
Room temperature, preparation carbonization silkworm excrement are cooled to after holding 5.0h or more.
(2) Dopamine hydrochloride powder and 0.25g the carbonization silkworm excrement of 0.25g is placed in ball grinder, it is dense that 1.0mL mass is added
Degree is the ZnCl of 0.25g/L2Solution;Ball grinder sealing is placed in high speed machine oscillation ball mill to vibrate, revolving speed is 1000
Turn/min, the graft reaction time is 60min (being that atmospheric pressure sealed carries out in reaction process);By resulting dopamine/ZnCl2/ silkworm
The husky direct 80 DEG C of drying of composite mortar obtain composite material crude product;
(3) by composite material crude product acquired in step (2) in N2500 are raised in atmosphere with the heating rate of 5 DEG C/min
DEG C, and keep 5.0h to carry out reaming reaction at 500 DEG C and obtained solid is dissolved in 1mol/L's to be cooled to room temperature naturally
Cleaning dissolution unreacted ZnCl in HCl2, it reuses after deionized water is cleaned to pH ≈ 7 and is centrifuged, be placed in baking oven and be dried overnight,
High-ratio surface dopamine silkworm excrement carbon composite is obtained after drying.
Embodiment 2
(1) in N210.0g Faeces bombycis is raised to 600 DEG C with the heating rate of 5 DEG C/min in atmosphere, and is protected at 600 DEG C
Room temperature, preparation carbonization silkworm excrement are cooled to after holding 4.0h or more.
(2) Dopamine hydrochloride powder and 0.5g the carbonization silkworm excrement of 0.25g is placed in ball grinder, it is dense that 3.0mL mass is added
Degree is the ZnCl of 0.30g/L2Solution;Ball grinder sealing is placed in high speed machine oscillation ball mill to vibrate, revolving speed is 1050
Turn/min, the graft reaction time is 50min (being that atmospheric pressure sealed carries out in reaction process);By resulting dopamine/ZnCl2/ silkworm
The husky direct 80 DEG C of drying of composite mortar obtain composite material crude product.
(3) by composite material crude product acquired in step (2) in N2550 are raised in atmosphere with the heating rate of 5 DEG C/min
DEG C, and 4.0h is kept at 550 DEG C, to be cooled to room temperature naturally, obtained solid is dissolved in the HCl of 1mol/L and cleans dissolution
Unreacted ZnCl2, reuse after deionized water is cleaned to pH ≈ 7 and be centrifuged, be placed in baking oven and be dried overnight, high ratio is obtained after drying
Surface dopamine silkworm excrement carbon composite.
Embodiment 3
(1) in N210.0g Faeces bombycis is raised to 700 DEG C with the heating rate of 5 DEG C/min in atmosphere, and is protected at 600 DEG C
Room temperature, preparation carbonization silkworm excrement are cooled to after holding 3.0h or more.
(2) Dopamine hydrochloride powder and 0.75g the carbonization silkworm excrement of 0.25g is placed in ball grinder, it is dense that 5.5mL mass is added
Degree is the ZnCl of 0.25g/L2Solution;Ball grinder sealing is placed in high speed machine oscillation ball mill to vibrate, revolving speed is 1100
Turn/min, the graft reaction time is 45min (being that atmospheric pressure sealed carries out in reaction process);By resulting dopamine/ZnCl2/ silkworm
The husky direct 90 DEG C of drying of composite mortar obtain composite material crude product.
(3) by composite material crude product acquired in step (2) in N2600 are raised in atmosphere with the heating rate of 5 DEG C/min
DEG C, and 3.0h is kept at 600 DEG C, to be cooled to room temperature naturally, obtained solid is dissolved in the HCl of 1mol/L and cleans dissolution
Unreacted ZnCl2, reuse after deionized water is cleaned to pH ≈ 7 and be centrifuged, be placed in baking oven and be dried overnight, high ratio is obtained after drying
Surface dopamine silkworm excrement carbon composite.
Embodiment 4
(1) in N210.0g Faeces bombycis is raised to 600 DEG C with the heating rate of 5 DEG C/min in atmosphere, and is protected at 650 DEG C
Room temperature, preparation carbonization silkworm excrement are cooled to after holding 3.0h or more.
(2) Dopamine hydrochloride powder and 1.0g the carbonization silkworm excrement of 0.25g is placed in ball grinder, it is dense that 8.0mL mass is added
Degree is the ZnCl of 0.30g/L2Solution;Ball grinder sealing is placed in high speed machine oscillation ball mill to vibrate, revolving speed is 1100
Turn/min, the graft reaction time is 45min (being that atmospheric pressure sealed carries out in reaction process);By resulting dopamine/ZnCl2/ silkworm
The husky direct 80 DEG C of drying of composite mortar obtain composite material crude product.
(3) by composite material crude product acquired in step (2) in N2600 are raised in atmosphere with the heating rate of 5 DEG C/min
DEG C, and 2.0h is kept at 600 DEG C, to be cooled to room temperature naturally, obtained solid is dissolved in the HCl of 1mol/L and cleans dissolution
Unreacted ZnCl2, reuse after deionized water is cleaned to pH ≈ 7 and be centrifuged, be placed in baking oven and be dried overnight, high ratio is obtained after drying
Surface dopamine silkworm excrement carbon composite.
Embodiment 5
(1) in N210.0g Faeces bombycis is raised to 900 DEG C with the heating rate of 5 DEG C/min in atmosphere, and is protected at 900 DEG C
Room temperature, preparation carbonization silkworm excrement are cooled to after holding 2.0h or more.
(2) Dopamine hydrochloride powder and 1.25g the carbonization silkworm excrement of 0.25g is placed in ball grinder, 11.0mL mass is added
Concentration is the ZnCl of 0.25g/L2Solution;Ball grinder sealing is placed in high speed machine oscillation ball mill to vibrate, revolving speed is
1150 turns/min, the graft reaction time is 40min (being that atmospheric pressure sealed carries out in reaction process);By resulting dopamine/
ZnCl2The direct 85 DEG C of drying of/silkworm excrement composite mortar obtain composite material crude product.
(3) by composite material crude product acquired in step (2) in N2650 are raised in atmosphere with the heating rate of 5 DEG C/min
DEG C, and 1.0h is kept at 650 DEG C, to be cooled to room temperature naturally, obtained solid is dissolved in the HCl of 1mol/L and cleans dissolution
Unreacted ZnCl2, reuse after deionized water is cleaned to pH ≈ 7 and be centrifuged, be placed in baking oven and be dried overnight, high ratio is obtained after drying
Surface dopamine silkworm excrement carbon composite.
Embodiment 6
(1) in N210.0g Faeces bombycis is raised to 1000 DEG C with the heating rate of 5 DEG C/min in atmosphere, and at 1000 DEG C
Room temperature, preparation carbonization silkworm excrement are cooled to after keeping 0.5h or more.
(2) Dopamine hydrochloride powder and 1.5g the carbonization silkworm excrement of 0.25g is placed in ball grinder, it is dense that 15.0mL mass is added
Degree is the ZnCl of 0.25g/L2Solution;Ball grinder sealing is placed in high speed machine oscillation ball mill to vibrate, revolving speed is 1200
Turn/min, the graft reaction time is 30min (being that atmospheric pressure sealed carries out in reaction process);By resulting dopamine/ZnCl2/ silkworm
The husky direct 85 DEG C of drying of composite mortar obtain composite material crude product.
(3) by composite material crude product acquired in step (2) in N2700 are raised in atmosphere with the heating rate of 5 DEG C/min
DEG C, and 0.5h is kept at 700 DEG C, to be cooled to room temperature naturally, obtained solid is dissolved in the HCl of 1mol/L and cleans dissolution
Unreacted ZnCl2, reuse after deionized water is cleaned to pH ≈ 7 and be centrifuged, be placed in baking oven and be dried overnight, high ratio is obtained after drying
Surface dopamine silkworm excrement carbon composite.
Material properties test:
(1) electron microscope of high-ratio surface dopamine silkworm excrement carbon composite
Using Japanese Hitachi S-3400N type low power scanning electron microscope to 1 institute of Faeces bombycis and the embodiment of the present invention
Dopamine silkworm excrement carbon composite obtained carries out the characterization of material surface pattern, as shown in Figure 1 and Figure 2.
Fig. 1 is Faeces bombycis electron-microscope scanning figure, embodies Faeces bombycis tridimensional network.Fig. 2 is high-ratio surface dopamine charcoal
Silkworm excrement carbon composite electron-microscope scanning figure, it can be seen that after DOPA amine polymer and grafting and activating is added by mechanical activation,
A large amount of dopamine beads are formed on carbonization silkworm excrement, form dopamine silkworm excrement carbon composite.
(2) pore structure study of dopamine silkworm excrement carbon composite
Using the 3-Flex specific surface pore-size distribution instrument of Micro company of U.S. production to dopamine silkworm prepared by the present invention
The pore structure of husky carbon composite is measured, and the results are shown in Table 1.
The specific surface area and pore-size distribution of the resulting dopamine silkworm excrement carbon composite of 1. 6 kinds of embodiments of table.
Smicro, VtAnd VmicroRespectively indicate specific surface area provided by micropore, Kong Rong provided by total pore volume and micropore.
According to 1 column data of table it is found that the Langmuir of dopamine silkworm excrement carbon composite prepared by six kinds of embodiments
Specific surface area is in 1000-1400m2/ g, total pore volume is about in 0.3-0.6cm3/ g or more, wherein micropore specific area and Kong Rong are accounted for
The 50~70% of total specific surface area and Kong Rong.This explanation, in the embodiment of the present invention coverage area, prepares obtained DOPA
Amine silkworm excrement carbon composite is a kind of porous carbon material with high specific surface area.
(3) dopamine silkworm excrement carbon composite sustained release performance is analyzed
It is gentle that pesticide Diacloden absorption carriage amount is carried out to dopamine silkworm excrement carbon composite prepared by case study on implementation 2,4,6
Tracing analysis is released, wherein the adsorption conditions of carbon composite are that 50mg composite slow release material is put into 50mL0.8g/L Diacloden solution
Middle oscillation absorption, vibrates 200 revs/min of revolving speed by 30 DEG C of bath temperature;The sustained release condition of carbon composite is multiple after 50mg is adsorbed
It closes slow-release material to be put into 120mL deionized water, changes water 100mL daily, 30 DEG C of bath temperature, vibrate 200 revs/min of revolving speed,
Experimental result difference is as shown in Figure 3, Figure 4.From figure 3, it can be seen that 3 kinds of slow-release materials are in absorption 48 hours back loadings of Diacloden
Amount all reaches 500mg/g or more, and without apparent difference between three kinds of materials, illustrates such material with different sustained releases
Similar adsorption effect is able to maintain while effect.From fig. 4, it can be seen that being released respectively in completion in 15 days, 30 days and 60 days or so
Journey (using 90% Diacloden of total volume as endpoint calculation) is let off, the requirement of different times pesticide slow-release is able to satisfy.
The above embodiment of the present invention is only intended to clearly illustrate examples made by the present invention, and is not to of the invention
The restriction of embodiment.For those of ordinary skill in the art, other can also be made on the basis of the above description
Various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all in spirit of the invention
With any modifications, equivalent replacements, and improvements made within principle etc., the protection scope of the claims in the present invention should be included in
Within.
Claims (7)
1. a kind of application of high-ratio surface dopamine silkworm excrement carbon composite, it is characterised in that: it is in terms of pesticide delays controlled release
Using;The three dimensional pore structures that the material is constituted with dopamine and charing silkworm excrement, Langmuir specific surface area are 1000-1400
m2/ g, total pore volume is in 0.3-0.6 cm3/ g, wherein micropore specific area and Kong Rong account for the 50 ~ 70% of total specific surface area and Kong Rong;
The preparation method of the material includes the following steps,
(1) Faeces bombycis is reacted into preparation carbonization silkworm excrement by high temperature cabonization in protective gas;
(2) Dopamine hydrochloride powder and carbonization silkworm excrement are mixed, ZnCl is added2Solution is placed on high speed machine oscillation ball milling secret
Envelope oscillation, speed control, in 30 ~ 60 min, obtain dopamine/ZnCl in 1000 ~ 2000 turns/min, graft reaction time2/
Then slurry is directly dried and obtains composite material crude product by silkworm excrement slurry;
(3) composite material crude product acquired in step (2) is subjected in protective gas reaming reaction, then cleans, is centrifuged again
And high-ratio surface dopamine silkworm excrement carbon composite is obtained after drying.
2. the application of high-ratio surface dopamine silkworm excrement carbon composite according to claim 1, it is characterised in that: the step
Suddenly the mass ratio that Dopamine hydrochloride powder is mixed with carbonization silkworm excrement in (2) is 1:6 ~ 1.
3. the application of high-ratio surface dopamine silkworm excrement carbon composite according to claim 1, it is characterised in that: the step
Suddenly carbonization silkworm excrement and ZnCl in (2)2The plastid ratio of solution is 1:4 ~ 10.
4. the application of high-ratio surface dopamine silkworm excrement carbon composite according to claim 1, it is characterised in that: the step
Suddenly ZnCl in (2)2Concentration of polymer solution is 0.25 ~ 0.30g/mL.
5. the application of high-ratio surface dopamine silkworm excrement carbon composite according to claim 1, it is characterised in that: the expansion
Hole reaction temperature is 500 ~ 700 oC, and the reaction time is 0.5 ~ 5 h.
6. the application of high-ratio surface dopamine silkworm excrement carbon composite according to claim 1, it is characterised in that: the expansion
Hole reaction temperature is 550 ~ 650 oC, and the reaction time is 2 ~ 3 h.
7. the application of high-ratio surface dopamine silkworm excrement carbon composite according to claim 1, it is characterised in that: step
(1) carburizing temperature of Faeces bombycis is in 500-1000 oC, 2 ~ 4 h of reaction time in.
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Application Number | Priority Date | Filing Date | Title |
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CN103482624A (en) * | 2013-09-26 | 2014-01-01 | 福建农林大学 | Preparation method for active carbon with photocatalysis function |
CN104150479A (en) * | 2014-07-17 | 2014-11-19 | 大连理工大学 | Preparation method of doped high-specific-surface-area activated carbon |
CN104386685A (en) * | 2014-10-22 | 2015-03-04 | 北京化工大学 | Method for preparing nitrogen-doped active carbon from nitrogen-enriched biomass raw material |
CN104689857A (en) * | 2015-03-26 | 2015-06-10 | 中国科学院青岛生物能源与过程研究所 | Preparing method for nitrogen-doped porous carbon material, catalyst comprising material and application of material |
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CN103482624A (en) * | 2013-09-26 | 2014-01-01 | 福建农林大学 | Preparation method for active carbon with photocatalysis function |
CN104150479A (en) * | 2014-07-17 | 2014-11-19 | 大连理工大学 | Preparation method of doped high-specific-surface-area activated carbon |
CN104386685A (en) * | 2014-10-22 | 2015-03-04 | 北京化工大学 | Method for preparing nitrogen-doped active carbon from nitrogen-enriched biomass raw material |
CN104689857A (en) * | 2015-03-26 | 2015-06-10 | 中国科学院青岛生物能源与过程研究所 | Preparing method for nitrogen-doped porous carbon material, catalyst comprising material and application of material |
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