CN102583304B - Method for preparing carbon microsphere by utilizing waste cotton fibre - Google Patents
Method for preparing carbon microsphere by utilizing waste cotton fibre Download PDFInfo
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- CN102583304B CN102583304B CN2011104615868A CN201110461586A CN102583304B CN 102583304 B CN102583304 B CN 102583304B CN 2011104615868 A CN2011104615868 A CN 2011104615868A CN 201110461586 A CN201110461586 A CN 201110461586A CN 102583304 B CN102583304 B CN 102583304B
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- PKDVWOVKDPEBQF-UHFFFAOYSA-N Cc(cc(cc1)OC)c1O Chemical compound Cc(cc(cc1)OC)c1O PKDVWOVKDPEBQF-UHFFFAOYSA-N 0.000 description 1
- BXNWEKMOICKDLV-UHFFFAOYSA-N OCC(C(C(C1OCCC1)O)O)O Chemical compound OCC(C(C(C1OCCC1)O)O)O BXNWEKMOICKDLV-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a method for preparing a carbon microsphere by utilizing waste cotton fibre. The waste cotton fibre is taken as raw material, deionized water is taken as reaction medium, and washing, disinfecting, cutting into strips, fading, soaking, dispersing, heating, pressurizing and stirring in a reactor, product washing, drying and grinding are carried out, thus the cotton fibre carbon microsphere the surface of which contains an active group is obtained. The technological process is advanced, no acid-base catalyst is used, no environmental pollution is produced, the cotton fibre carbon microsphere has stable physical and chemical performances, multiple groups can be directly grafted on the surface of the carbon microsphere without modification, and functional fiber can be prepared when the carbon microsphere is blended with polyester fibre, polyphenylene sulfide fibre and polypropylene fibre, thus the method provided by the invention is perfect for preparing the active carbon microsphere by utilizing the waste cotton fibre, and an advanced method is provided for recycling the waste cotton fibre.
Description
Technical field
The invention belongs to a kind of method, the preparation of genus carbon material and technical field of using for preparing carbosphere with waste cotton fiber.
Background technology
Carbon material has very high using value and all polymorphic types, and carbosphere is one of a kind of widely used, important carbon material, and carbosphere has good chemical stability, thermostability, absorption property and good conduction and thermal conductivity; Can be applicable to the numerous areas such as additive of li-ion electrode negative material, high strength carbon material, support of the catalyst, adsorbent, nano-device and functional fibre preparation.
The preparation of carbon current microballoon has several different methods, is raw material with pitch, coal, acetylene often, utilizes high-temperature roasting method, vapour deposition process, doped catalyst method to prepare the carbosphere of different size, structure, performance; The carbosphere that has can be hollow or solid construction, can be micron order or nano level, be applied in the different technologies field, but the carbosphere constituent of these method preparations is single, must carry out graft modification to the carbosphere surface, making its surface contain a large amount of active groups could be applied at value segment.
Along with the raising of social development and living standards of the people, the annual discarded cotton textiles in the whole world reach 1,000 ten thousand tons, seldom are used as recovery and recycling of used resources, are but directly buried or burn, and have caused the huge wasting of resources and environmental pollution; Recycling cotton fibre material is the task of top priority, and the main component of cotton fibre is Mierocrystalline cellulose, contains a large amount of carbons, is raw material with the waste cotton fiber, and the preparation carbosphere is the brand-new approach that a waste product utilizes.
Summary of the invention
Goal of the invention
The objective of the invention is at the background technology situation, is raw material with the waste cotton fiber, uses the hydro-thermal reaction method, and methyl, hydroxyl and carbonyl functional group's carbosphere is contained on the preparation surface, realizes the waste cotton fiber recycling, and improves the chemical physics performance of carbosphere.
Technical scheme
The chemical substance material that the present invention uses is: waste cotton fiber, dehydrated alcohol, sodium hydroxide, V-Brite B, linear alkylbenzene sulphonic acid, fatty alcohol-ether sodium sulfate, deionized water, its combination consumption is as follows: be measure unit with gram, milliliter
Waste cotton fiber: (C
6H
10O
5)
nN=6000~15000 molecular structural formulas:
The preparation method is as follows
(1) selected chemical substance material
The chemical substance material that the preparation carbosphere is used will carry out selected, and carries out quality purity control: quality percentage
(2) washing waste cotton fiber
1. getting waste cotton fiber 10g ± 0.01g places in the washer, in washer, add deionized water 300ml, linear alkyl benzene sulphonic acid 1g ± 0.001g, polyoxyethylenated alcohol sodium sulfate 0.4g ± 0.001g, sodium hydroxide 0.1g ± 0.001g, open the washer power supply, washing 30min;
2. the waste cotton fiber after will washing takes out, and puts into beaker, adds deionized water 500ml in beaker, stirs rinsing 5min with glass stick, and rinsing repeats 5 times;
3. the waste cotton fiber after the rinsing is placed in the loft drier, carries out drying treatment, 50 ℃ ± 2 ℃ of drying temperatures, time of drying 120min;
(3) sterilization
Waste cotton fiber after the washing is placed in the ultraviolet disinfection case and carries out disinfection voltage 220V, power 40W, disinfecting time 60min;
(4) cut bar
Waste cotton fiber after the sterilization is cut into strip, be of a size of 2 * 2mm;
(5) fade
Waste cotton fiber and the deionized water 200ml that 1. will cut behind the bar place in the beaker;
2. add sodium hydroxide 0.4g in the beaker and stir evenly, place water-bath to heat in beaker then, 75 ℃ ± 2 ℃ of Heating temperatures, and constant temperature insulation;
3. in beaker, add decolourant V-Brite B 1g ± 0.001g, stir and insulation 10min;
4. continue heating, insulation 30min faded waste cotton fiber when temperature rose to 95 ℃ in water-bath and the beaker;
5. the water liquid that fades in the beaker is outwelled, waste cotton fiber after retention is faded, cotton fibre after will fading then moves in another beaker, add deionized water 300ml, again beaker is placed in the water-bath, the water-bath kettle temperature rises to 85 ℃, constant temperature insulation 10min, stir with glass stick, with the chemical reagent of washing waste cotton fiber remained on surface, washing repeats 3 times;
6. the waste cotton fiber after will fading and wash places the loft drier inner drying, 50 ℃ ± 2 ℃ of drying temperatures, time of drying 120min;
(6) soak, disperse
1. get waste cotton fiber 2g and deionized water 500ml after fading, place in the beaker and seal, beaker is placed in the tank of ultrasonic disperser then, and fixing;
2. add deionized water 1500ml in the tank of ultrasonic disperser, deionized water is wanted 9/10 of submergence beaker volume;
3. open ultrasonic generator, ultrasonic wave voltage 220V, power 100W, 65HZ, and constant, under 25 ℃ of temperature, under the ultrasonic wave effect, waste cotton fiber mixes with water, and is dispersed in the water liquid, and ultrasonic dispersing time 120min becomes dispersion liquid;
(7) in reactor, under High Temperature High Pressure, prepare carbosphere
It is in reactor that waste cotton fiber prepares carbosphere, carries out under the condition of 260 ℃ ± 1 ℃ of temperature, pressure 4.1MPa;
1. open reactor, the waste cotton fiber deionized water dispersion liquid that soaks after disperseing is moved in the reactor, the axe lid is built in the insulation of reactor indirect heating, makes reactor be in sealed state;
2. open the reactor well heater, temperature rises to 100 ℃ by 25 ℃, and turn on agitator stirs, continue to be warming up to 260 ℃ ± 1 ℃ then after the constant temperature insulation, and open the pressurization motor, make that pressure rises to 4.1MPa in the reactor;
The agitator speed 200r/min of the waste cotton fiber deionized water dispersion liquid in the reactor, heating, pressurization, churning time are 480min;
3. cooling
Close electric heater, close agitator when reactor temperature is cooled to 100 ℃ naturally, stop to stir;
Close the pressurization motor, pressure drop is to 100KPa in the still;
Reactor temperature naturally cools to 25 ℃;
4. drive still, open reactor, take out the waste cotton fiber deionized water dispersion liquid in the still, that is: cotton fibre carbosphere reaction solution;
5. the chemical physics reaction takes place in waste cotton fiber deionized water dispersion liquid in heating, pressurization, whipping process, and generates active group on the carbosphere surface that is shaped, and reaction formula is as follows:
Cellulose hydrolysis is monose:
In the formula:
Glucose generates isometry product fructose:
In the formula:
The gluconate dehydratase cracking:
In the formula:
CH
3CHO: the hydrolysate acetaldehyde of glucose
Oxyhydroquinone and furans generation dehydration reaction:
In the formula:
The carbosphere intermediate product that generates after oxyhydroquinone and the furans dehydration reaction
5-hydroxymethylfurfural, oxyhydroquinone and furans generation aldol reaction:
In the formula:
Generate the carbosphere intermediate product behind 5-hydroxymethylfurfural, oxyhydroquinone and the furans generation aldol reaction;
Intermediate product further reacts:
In the formula:
(8) standing demix is moved into waste cotton fiber carbosphere reaction solution in the beaker, standing demix, and time 60min outwells supernatant liquor, retains the waste cotton fiber carbosphere;
(9) washing
1. the waste cotton fiber carbosphere is placed beaker, add dehydrated alcohol 200ml, vibration agitator treating 10min; Absolute ethanol washing repeats 3 times;
2. the waste cotton fiber carbosphere behind the absolute ethanol washing is placed another beaker, add deionized water 200ml, vibration agitator treating 10min; Deionized water wash repeats 3 times;
(10) suction filtration
Waste cotton fiber carbosphere after the washing is placed the B of filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, waste liquid is evacuated in the filter flask;
(11) vacuum-drying
The product filter cake is placed quartzy product boat, place the vacuum drying oven inner drying then, 120 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying, 240min was black powder after the drying, that is: the cotton fibre carbosphere;
(12) grind, sieve
Place agate mortar to grind dried black powder, sieve with 800 eye mesh screens, grind repeatedly, sieve repeatedly, the black powder after sieving is the cotton fibre carbosphere;
(13) detect, analyze, characterize
Pattern, the composition of the cotton fibre carbosphere of preparation, the chemical physics performance of active group are detected, analyze, characterize;
The appearance structure of use emission scan electron microscopic observation carbosphere;
Analyze the surface composition of carbosphere with infrared spectrometer;
With X-ray diffractometer structure and the composition of product are analyzed;
Conclusion: by the cotton fibre carbosphere of hydrothermal synthesis method preparation, product is the spherical graphite carbon structure of black, and a large amount of carbonyls, hydroxyl, methyl functional group, carbosphere diameter≤100nm are contained in the carbosphere surface;
(14) store
Cotton fibre carbosphere to preparation is stored in the water white Glass Containers, and clean environment is wanted waterproof, protection against the tide, anti-oxidation, fire prevention, the saline and alkaline erosion of acid-proof, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has tangible advance, be to be raw material with the waste cotton fiber, be reaction medium with the deionized water, be clean-out system with dehydrated alcohol and deionized water, be decolourant with V-Brite B and sodium hydroxide, be washing composition with linear alkyl benzene sulphonic acid and polyoxyethylenated alcohol sodium sulfate, through washing, sterilization, cut bar, fade, soak, disperse, the pressurization of reactor internal heating is stirred, wash through product again, dry, make the carbosphere that the surface contains active group after the grinding, this preparation method's technology advanced person, do not use acid base catalysator, can not cause environmental pollution, the product physical and chemical performance is stable, carbosphere need not modification can be at the direct multiple group of grafting in its surface, with trevira, polyphenylene sulfide fibre, functional fibre is made in polypropylene fibre section blend, is the very good method for preparing active-carbon-microball with waste cotton fiber.
Description of drawings
Fig. 1 reactor prepares the state graph of cotton fibre carbosphere
Fig. 2 cotton fibre carbosphere product shape appearance figure
Fig. 3 is the X-ray diffraction spectrum comparison diagram of waste cotton fiber and cotton fibre carbosphere
Fig. 4 is the infrared spectra comparison diagram of waste cotton fiber and cotton fibre carbosphere
Shown in the figure, list of numerals is as follows:
1, magnetic stirring apparatus, 2, the reactor standing bolt, 3, the reactor top cover, 4, insulation zone of heating, 5, reactor, 6, cotton fibre deionized water dispersion liquid, 7, lead, 8, the pressurization motor, 9, tensimeter, 10, thermometer, 11, electric control box, 12, the mixing speed display screen, 13, temperature in the kettle display screen, 14, stir switch, 15, power switch, 16, temperature regulator, 17, the mixing speed modulator.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, for reactor prepares the state graph of cotton fibre carbosphere, each position, it is correct that annexation is wanted, according to quantity proportioning, operation according to the order of sequence.
The value of the chemical substance that preparation is used is to determine by the scope that sets in advance, and is measure unit with gram, milliliter.
Waste cotton fiber prepares carbosphere to carry out in reactor; Under high temperature, high pressure, stirring condition, finish; Reactor 5 is round shape, reactor 5 is outside for being incubated zone of heating 4, putting waste cotton fiber deionized water dispersion liquids 6 in the reactor 5, is kettle cover 3 and by bolt 2 fixing seals on the top of reactor 5, is provided with agitator 1, thermometer 10, pressurization motor 8, tensimeter 9 at kettle cover 3; Right side at reactor 5 connects electric control box 11 by lead 7, is provided with at electric control box 11 and stirs revolution display screen 12, temperature in the kettle display screen 13, stirs switch 14, power switch 15, temperature regulator 16, mixing speed modulator 17.
Fig. 2 is cotton fibre carbosphere shape appearance figure, and as we can see from the figure, carbosphere is irregular sphere, and particle diameter≤100nm because not carrying out surface modification treatment, is aggregating state.
Shown in Figure 3, XRD spectrum comparison diagram for waste cotton fiber and cotton fibre carbosphere, curve a is waste cotton fiber, and wherein 101 and 002 characteristic diffraction peak causes that by cellulose macromolecule is transversely arranged 040 characteristic diffraction peak is caused by the Mierocrystalline cellulose vertical structure; Curve b is the XRD figure spectrum of function cotton fibre carbosphere, find that obviously 101 and 040 characteristic diffraction peak disappears, the gained sample is non-crystalline state, wherein 002 crystal face is the diffraction peak of carbon-coating structure in the aromatic series, the existence of roomy crystal face explanation product camber disordered structure, show that its degree of graphitization is lower, this is not cause owing to the forming core process of growth is subjected to strict control, can be improved by thermal treatment.
Shown in Figure 4, be waste cotton fiber and cotton fibre carbosphere infrared spectra comparison diagram, among the figure as can be known: b curve function carbosphere has rich functional groups, and shows that the cellulosic reaction of hydrothermal carbonization is dehydration and the process of aromizing, at 1620cm
-1The place corresponds to the vibration of gripping olefin skeletal altogether, 1437cm
-1Exist for the phenyl ring skeletal vibration, show that glucose has produced aromizing in hydrolytic process, from 3000-2815cm
-1Between absorption peak meet aliphatics C-H stretching vibration, these char-forming materials of deducibility also have aliphatic structure simultaneously; Oxygen-containing functional group may be present in 3000~3700cm
-1Between, this scope is O in hydroxyl or the carboxyl-H stretching vibration, finds that simultaneously carbonyl in the fiber (C=O) vibration absorption peak has moved to 1710cm
-1The place; In addition, at 1000~1460cm
-1Between be C in hydroxyl, ester, the ether-O stretching vibration and O-H flexural vibration; At 1000~1460cm
-1With 3000~3700cm
-1Between, product is compared with unprocessed waste cotton fiber a, and vibration intensity has obvious decline, and illustrating has the dehydration phenomenon to occur in hydro-thermal reaction, and carbonization formation carbon-carbon single bond and two keys, makes product partially carbonized, realizes the purpose of preparation carbosphere.
Claims (2)
1. method for preparing carbosphere with waste cotton fiber, it is characterized in that: the chemical substance material of use is: pure cotton fabric, deionized water, dehydrated alcohol, sodium hydroxide, V-Brite B, linear alkyl benzene sulphonic acid, polyoxyethylenated alcohol sodium sulfate, its combination consumption as follows: with the gram, the milliliter be measure unit
The preparation method is as follows
(1) selected chemical substance material
The chemical substance material that the preparation carbosphere is used will carry out selected, and carries out quality purity control: quality percentage
(2) washing waste cotton fiber
1. getting waste cotton fiber 10g ± 0.01g places in the washer, in washer, add deionized water 300ml, linear alkyl benzene sulphonic acid 1g ± 0.001g, polyoxyethylenated alcohol sodium sulfate 0.4g ± 0.001g, sodium hydroxide 0.1g ± 0.001g, open the washer power supply, washing 30min;
2. the waste cotton fiber after will washing takes out, and puts into beaker, adds deionized water 500ml in beaker, stirs rinsing 5min with glass stick, and rinsing repeats 5 times;
3. the waste cotton fiber after the rinsing is placed in the loft drier, carries out drying treatment, 50 ℃ ± 2 ℃ of drying temperatures, time of drying 120min;
(3) sterilization
Waste cotton fiber after the washing is placed in the ultraviolet disinfection case and carries out disinfection voltage 220V, power 40W, disinfecting time 60min;
(4) cut bar
Waste cotton fiber after the sterilization is cut into strip, be of a size of 2 * 2mm;
(5) fade
Waste cotton fiber and the deionized water 200ml that 1. will cut behind the bar place in the beaker;
2. add sodium hydroxide 0.4g in the beaker and stir evenly, place water-bath to heat in beaker then, 75 ℃ ± 2 ℃ of Heating temperatures, and constant temperature insulation;
3. in beaker, add decolourant V-Brite B 1g ± 0.001g, stir and insulation 10min;
4. continue heating, insulation 30min faded waste cotton fiber when temperature rose to 95 ℃ in water-bath and the beaker;
5. the water liquid that fades in the beaker is outwelled, waste cotton fiber after retention is faded, cotton fibre after will fading then moves in another beaker, add deionized water 300ml, again beaker is placed in the water-bath, the water-bath kettle temperature rises to 85 ℃, constant temperature insulation 10min, stir with glass stick, with the chemical reagent of washing waste cotton fiber remained on surface, washing repeats 3 times;
6. the waste cotton fiber after will fading and wash places the loft drier inner drying, 50 ℃ ± 2 ℃ of drying temperatures, time of drying 120min;
(6) soak, disperse
1. get waste cotton fiber 2g and deionized water 500ml after fading, place in the beaker and seal, beaker is placed in the tank of ultrasonic disperser then, and fixing;
2. add deionized water 1500ml in the tank of ultrasonic disperser, deionized water is wanted 9/10 of submergence beaker volume;
3. open ultrasonic generator, ultrasonic wave voltage 220V, power 100W, 65HZ, and constant, under 25 ℃ of temperature, under the ultrasonic wave effect, waste cotton fiber mixes with water, and is dispersed in the water liquid, and ultrasonic dispersing time 120min becomes dispersion liquid;
(7) in reactor, under High Temperature High Pressure, prepare carbosphere
It is in reactor that waste cotton fiber prepares carbosphere, carries out under the condition of 260 ℃ ± 1 ℃ of temperature, pressure 4.1MPa;
1. open reactor, the waste cotton fiber deionized water dispersion liquid that soaks after disperseing is moved in the reactor, the axe lid is built in the insulation of reactor indirect heating, makes reactor be in sealed state;
2. open the reactor well heater, temperature rises to 100 ℃ by 25 ℃, and turn on agitator stirs, continue to be warming up to 260 ℃ ± 1 ℃ then after the constant temperature insulation, and open the pressurization motor, make that pressure rises to 4.1MPa in the reactor;
The agitator speed 200r/min of the waste cotton fiber deionized water dispersion liquid in the reactor, heating, pressurization, churning time are 480min;
3. cooling
Close electric heater, close agitator when reactor temperature is cooled to 100 ℃ naturally, stop to stir;
Close the pressurization motor, pressure drop is to 100KPa in the still;
Reactor temperature naturally cools to 25 ℃;
4. drive still, open reactor, take out the waste cotton fiber deionized water dispersion liquid in the still, that is: cotton fibre carbosphere reaction solution;
5. the chemical physics reaction takes place in waste cotton fiber deionized water dispersion liquid in heating, pressurization, whipping process, and generates active group on the carbosphere surface that is shaped, and reaction formula is as follows:
Cellulose hydrolysis is monose:
In the formula:
Cellulose hydrolysis product glucose
Glucose generates isometry product fructose:
In the formula:
The gluconate dehydratase cracking:
In the formula:
The hydrolysate oxyhydroquinone of glucose sugar
CH
3CHO: the hydrolysate acetaldehyde of glucose
Oxyhydroquinone and furans generation dehydration reaction:
In the formula:
The carbosphere intermediate product that generates after oxyhydroquinone and the furans dehydration reaction
5-hydroxymethylfurfural, oxyhydroquinone and furans generation aldol reaction:
In the formula:
Generate the carbosphere intermediate product behind 5-hydroxymethylfurfural, oxyhydroquinone and the furans generation aldol reaction;
Intermediate product further reacts:
In the formula:
(8) standing demix is moved into waste cotton fiber carbosphere reaction solution in the beaker, standing demix, and time 60min outwells supernatant liquor, retains the waste cotton fiber carbosphere;
(9) washing
1. the waste cotton fiber carbosphere is placed beaker, add dehydrated alcohol 200ml, vibration agitator treating 10min; Absolute ethanol washing repeats 3 times;
2. the waste cotton fiber carbosphere behind the absolute ethanol washing is placed another beaker, add deionized water 200ml, vibration agitator treating 10min; Deionized water wash repeats 3 times;
(10) suction filtration
Waste cotton fiber carbosphere after the washing is placed the B of filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, waste liquid is evacuated in the filter flask;
(11) vacuum-drying
The product filter cake is placed quartzy product boat, place the vacuum drying oven inner drying then, 120 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying, 240min was black powder after the drying, that is: the cotton fibre carbosphere;
(12) grind, sieve
Place agate mortar to grind dried black powder, sieve with 800 eye mesh screens, grind repeatedly, sieve repeatedly, the black powder after sieving is the cotton fibre carbosphere;
(13) detect, analyze, characterize
Pattern, the composition of the cotton fibre carbosphere of preparation, the chemical physics performance of active group are detected, analyze, characterize;
The appearance structure of use emission scan electron microscopic observation carbosphere;
Analyze the surface composition of carbosphere with infrared spectrometer;
With X-ray diffractometer structure and the composition of product are analyzed;
Conclusion: by the cotton fibre carbosphere of hydrothermal synthesis method preparation, product is the spherical graphite carbon structure of black, and a large amount of carbonyls, hydroxyl, methyl functional group, carbosphere diameter≤100nm are contained in the carbosphere surface;
(14) store
Cotton fibre carbosphere to preparation is stored in the water white Glass Containers, and clean environment is wanted waterproof, protection against the tide, anti-oxidation, fire prevention, the saline and alkaline erosion of acid-proof, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
2. a kind of method for preparing carbosphere with waste cotton fiber according to claim 1, it is characterized in that: prepare carbosphere with waste cotton fiber and in reactor, carry out, at high temperature, high pressure, finishing under the reaction conditions that stirs, reactor (5) is round shape, reactor (5) is outside for being incubated zone of heating (4), put cotton fibre deionized water dispersion liquid (6) in the reactor (5), be kettle cover (3) and by bolt (2) fixing seal on the top of reactor (5), be provided with agitator (1) at kettle cover (3), thermometer (10), pressurization motor (8), tensimeter (9); Right side at reactor (5) connects electric control box (11) by lead (7), is provided with at electric control box (11) and stirs revolution display screen (12), temperature in the kettle display screen (13), stirs switch (14), power switch (15), temperature regulator (16), mixing speed modulator (17).
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CN103588190B (en) * | 2013-10-31 | 2016-04-06 | 中国科学院过程工程研究所 | A kind of method being prepared carbosphere by lignocellulose |
CN103949216A (en) * | 2014-05-13 | 2014-07-30 | 农业部环境保护科研监测所 | Preparation method of carbon material for adsorbing hydrophilic ionic liquid |
CN105272389A (en) * | 2015-06-04 | 2016-01-27 | 浙江科技学院 | Pig manure carbon-based fertilizer development method based on soil improvement |
CN105129794A (en) * | 2015-07-13 | 2015-12-09 | 安徽成方新材料科技有限公司 | Nano cotton adsorption-reinforced composite spherical activated carbon and preparation method thereof |
CN104986764A (en) * | 2015-07-13 | 2015-10-21 | 安徽成方新材料科技有限公司 | Green environment-friendly light-weight porous reinforced compound spherical active carbon and preparation method of active carbon |
CN105197915A (en) * | 2015-11-05 | 2015-12-30 | 山西瑞赛格纺织科技有限公司 | Method for rapidly preparing carbon material from waste polyester-cotton fabric |
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CN1454839A (en) * | 2002-04-30 | 2003-11-12 | 财团法人工业技术研究院 | Hollow nano carbon ball manufacturing method |
CN101927994A (en) * | 2010-01-08 | 2010-12-29 | 大连理工大学 | Method for preparing monodisperse nano hollow carbon sphere with controllable size and shape |
CN101993057A (en) * | 2009-08-27 | 2011-03-30 | 中国科学院金属研究所 | Method for preparing carbon hollow sphere |
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CN1454839A (en) * | 2002-04-30 | 2003-11-12 | 财团法人工业技术研究院 | Hollow nano carbon ball manufacturing method |
CN101993057A (en) * | 2009-08-27 | 2011-03-30 | 中国科学院金属研究所 | Method for preparing carbon hollow sphere |
CN101927994A (en) * | 2010-01-08 | 2010-12-29 | 大连理工大学 | Method for preparing monodisperse nano hollow carbon sphere with controllable size and shape |
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