CN102583304A - Method for preparing carbon microsphere by utilizing waste cotton fibre - Google Patents

Method for preparing carbon microsphere by utilizing waste cotton fibre Download PDF

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Publication number
CN102583304A
CN102583304A CN2011104615868A CN201110461586A CN102583304A CN 102583304 A CN102583304 A CN 102583304A CN 2011104615868 A CN2011104615868 A CN 2011104615868A CN 201110461586 A CN201110461586 A CN 201110461586A CN 102583304 A CN102583304 A CN 102583304A
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carbosphere
cotton fiber
waste cotton
deionized water
beaker
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CN102583304B (en
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戴晋明
史晟
高立斌
侯文生
牛梅
王淑花
蔡智锋
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Taiyuan University of Technology
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Taiyuan University of Technology
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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

A kind of method for preparing carbosphere with waste cotton fiber
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 many types, and carbosphere is one of a kind of widely used, important carbon material, and carbosphere has good chemicalstability, 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, and making its surface contain a large amount of reactive groups could be applied at value segment.
Along with the raising of social development and living standards of the people, global annual depleted cotton textiles 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 staple of cotton fibre is a 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 to 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 that waste cotton fiber utilizes again, and improves the chemical physics performance of carbosphere.
Technical scheme
The chemical substance material that the present invention uses is: waste cotton fiber, absolute ethyl alcohol, sodium hydroxide, V-Brite B, linear alkylbenzene sulphonic acid, fatty alcohol-ether sodium sulfate, deionized water, its combination consumption is following: with gram, milliliter is measure unit
Waste cotton fiber: (C 6H 10O 5) nN=6000~15000 molecular structural formulas:
Figure BSA00000652706600021
10g±0.01g
Absolute ethyl alcohol: CH 3CH 2OH 1000ml ± 10ml
Deionized water: H 2O 6000ml ± 10ml
Sodium hydroxide: NaOH 0.5g ± 0.001g
V-Brite B: Na 2S 2O 41g ± 0.001g
Linear alkylbenzene sulphonic acid: C 18H 29O 3SNa 1g ± 0.001g
Polyoxyethylenated alcohol sodium sulfate: C 13H 27O (CH 2CH 2O) 2SO 3Na 0.5g ± 0.001g
The preparation method is following
(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
Waste cotton fiber: solid-state solid carbon amount: 44.44%
Absolute ethyl alcohol: liquid liquid 99.5%
Deionized water: liquid liquid 99.9%
Sodium hydroxide: solid powder 99.9%
V-Brite B: solid powder 99.9%
The liquid viscous liquid 99.9% of LABS
Polyoxyethylenated alcohol sodium sulfate liquid gel shape lotion 99.9%
(2) washing waste cotton fiber
1. getting waste cotton fiber 10g ± 0.01g places in the washer; In washer, add deionized water 300ml, LABS 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, in beaker, adds deionized water 500ml, 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
The waste cotton fiber and the deionized water 200ml that 1. will cut behind the bar place in the beaker;
2. in beaker, add sodium hydroxide 0.4g and stir, 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, retained the waste cotton fiber after fading, the cotton fibre after will fading then moves in another beaker; Add deionized water 300ml, once more 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, then beaker is placed in the tank of ultrasonic disperser, and fixing;
2. in the tank of ultrasonic disperser, add deionized water 1500ml, deionized water is wanted 9/10 of submergence beaker volume;
3. open ultrasonic generator, UW voltage 220V, power 100W, 65HZ, and constant, under 25 ℃ of temperature, under the UW effect, waste cotton fiber mixes with water, and is dispersed in the water liquid, and ultrasonic dispersing time 120min becomes dispersion liquid;
(7) in reaction kettle, preparation carbosphere under HTHP
It is in reaction kettle that waste cotton fiber prepares carbosphere, under the condition of 260 ℃ ± 1 ℃ of temperature, pressure 4.1MPa, carries out;
1. open reaction kettle, the waste cotton fiber+deionized water dispersion liquid that soaks after disperseing is moved in the reaction kettle, the axe lid is built in the insulation of reaction kettle indirect heating, makes reaction kettle be in sealed state;
2. open the reaction kettle 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 reaction kettle;
The agitator speed 200r/min of the waste cotton fiber+deionized water dispersion liquid in the reaction kettle, heating, pressurization, churning time are 480min;
3. cooling
Close electric heater, close whisking appliance 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 reaction kettle, 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 reactive group on the carbosphere surface that is shaped, and reaction formula is following:
Cellulose hydrolysis is a monose:
Figure BSA00000652706600051
In the formula:
Figure BSA00000652706600052
cellulose hydrolysis product glucose
Glucose generates isometry product fructose:
Figure BSA00000652706600053
In the formula:
The isomers fructose of
Figure BSA00000652706600061
glucose
The gluconate dehydratase cracking:
Figure BSA00000652706600062
In the formula:
The hydrolysate 5-hydroxymethylfurfural of
Figure BSA00000652706600063
glucose
The hydrolysate furans of
Figure BSA00000652706600064
glucose
The hydrolysate 1 of
Figure BSA00000652706600065
glucose sugar; 2, the 4-pyrogallol
CH 3CHO: the hydrolysate acetaldehyde of glucose
Oxyhydroquinone and furans generation dehydration reaction:
Figure BSA00000652706600066
In the formula:
Figure BSA00000652706600071
1; 2, the carbosphere intermediate product that generates after 4-pyrogallol and the furans dehydration reaction
5-hydroxymethylfurfural, oxyhydroquinone and furans generation aldol reaction:
Figure BSA00000652706600072
In the formula:
5-hydroxymethylfurfural, 1; 2, generate the carbosphere intermediate product behind 4-pyrogallol and the furans generation aldol reaction;
Intermediate product further reacts:
Figure BSA00000652706600074
Figure BSA00000652706600081
In the formula:
Figure BSA00000652706600082
waste cotton fiber carbosphere
(8) standing demix is moved into waste cotton fiber carbosphere reaction solution in the beaker, standing demix, and time 60min outwells supernatant, retains the waste cotton fiber carbosphere;
(9) washing
1. the waste cotton fiber carbosphere is placed beaker, add absolute ethyl 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 a 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 reactive group are detected, analyze, characterize;
The appearance structure of use emission scan electron microscopic observation carbosphere;
Analyze the surface composition of carbosphere with IR;
With X-ray diffractometer the structure and the composition of product are analyzed;
Conclusion: through 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; Being to be raw material with the waste cotton fiber, is reaction medium with the deionized water, is clean-out system with absolute ethyl alcohol and deionized water; With V-Brite B and sodium hydroxide is decolourant; With LABS and polyoxyethylenated alcohol sodium sulfate is washing composition, through wash, sterilize, cut bar, fade, immersion, dispersion, the pressurization of reaction kettle internal heating are stirred, again through the product washing, dry, process the carbosphere that the surface contains reactive group after grinding, this preparing method's technology is advanced; Do not use acid base catalysator; Can not cause environmental pollution, the product physical and chemical performance is stable, and carbosphere need not modification can be at its surperficial directly multiple group of grafting; Processing functional fibre with trevira, polyphenylene sulfide fibre, polypropylene fibre section blend, is the very good method for preparing active-carbon-microball with waste cotton fiber.
Description of drawings
Fig. 1 reaction kettle 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 ir spectra comparison diagram of waste cotton fiber and cotton fibre carbosphere
Shown in the figure, list of numerals is following:
1, magnetic stirring apparatus, 2, the reaction kettle standing bolt, 3, the reaction kettle top cover, 4, the insulation zone of heating, 5, reaction kettle; 6, cotton fibre+deionized water dispersion liquid, 7, lead, 8, the pressurization motor, 9, tensimeter; 10, TM, 11, electric control box, 12, the mixing speed image display, 13, the temperature in the kettle image display; 14, stir switch, 15, power switch, 16, temperature regulator, 17, the mixing speed modulator.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified:
Shown in Figure 1, for reaction kettle prepares the state graph of cotton fibre carbosphere, each location, annexation want correct, according to quantity proportioning, operation according to the order of sequence.
The value of the chemical substance that preparation is used is to confirm by the scope that is provided with in advance, is measure unit with gram, milliliter.
Waste cotton fiber prepares carbosphere to carry out in reaction kettle; Under high temperature, high pressure, stirring condition, accomplish; Reaction kettle 5 is a round shape; Reaction kettle 5 is outside for being incubated zone of heating 4; Putting waste cotton fiber+deionized water dispersion liquids 6 in the reaction kettle 5, is kettle cover 3 and by bolt 2 fixing seals on the top of reaction kettle 5, on kettle cover 3, is provided with whisking appliance 1, TM 10, pressurization motor 8, tensimeter 9; Right side at reaction kettle 6 connects electric control box 11 through lead 7, on electric control box 11, is provided with and stirs revolution image display 12, temperature in the kettle image display 13, stirs switch 14, power switch 15, temperature regulator 16, mixing speed modulator 17.
Fig. 2 is a cotton fibre carbosphere shape appearance figure, from figure, can see that carbosphere is irregular sphere, and particle diameter≤100nm because of 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 a 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, and 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 receives strict control, can improve through thermal treatment.
Shown in Figure 4, be waste cotton fiber and cotton fibre carbosphere ir spectra comparison diagram, can know among the figure: b curve function carbosphere has rich functional groups, and shows that the cellulosic reaction of hydrothermal carbonization is the process of dehydration and 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 possibly be present in 3000~3700cm -1Between, this scope is O-H stretching vibration in hydroxyl or the carboxyl, 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-O stretching vibration and O-H flexural vibration in hydroxyl, ester, the ether; At 1000~1460cm -1With 3000~3700cm -1Between, product is compared with unprocessed waste cotton fiber a, and vibration intensity has obvious decline, and explaining 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, absolute ethyl alcohol, sodium hydroxide, V-Brite B, LABS, polyoxyethylenated alcohol sodium sulfate, its combination consumption is following: with gram, milliliter is measure unit
Waste cotton fiber: (C 6H 10O 5) nN=6000~15000 molecular structural formulas:
Figure FSA00000652706500011
10g±0.01g
Absolute ethyl alcohol: CH 3CH 2OH 1000ml ± 10ml
Deionized water: H 2O 6000ml ± 10ml
Sodium hydroxide: NaOH 0.5g ± 0.001g
V-Brite B: Na 2S 2O 41g ± 0.001g
Linear alkylbenzene sulphonic acid: C 18H 29O 3SNa 1g ± 0.001g
Polyoxyethylenated alcohol sodium sulfate: C 13H 27O (CH 2CH 2O) 2SO 3Na 0.5g ± 0.001g
The preparation method is following
(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
Waste cotton fiber: solid-state solid carbon amount: 44.44%
Absolute ethyl alcohol: liquid liquid 99.5%
Deionized water: liquid liquid 99.9%
Sodium hydroxide: solid powder 99.9%
V-Brite B: solid powder 99.9%
The liquid viscous liquid 99.9% of LABS
Polyoxyethylenated alcohol sodium sulfate liquid gel shape lotion 99.9%
(2) washing waste cotton fiber
1. getting waste cotton fiber 10g ± 0.01g places in the washer; In washer, add deionized water 300ml, LABS 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, in beaker, adds deionized water 500ml, 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
The waste cotton fiber and the deionized water 200ml that 1. will cut behind the bar place in the beaker;
2. in beaker, add sodium hydroxide 0.4g and stir, 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, retained the waste cotton fiber after fading, the cotton fibre after will fading then moves in another beaker; Add deionized water 300ml, once more 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, then beaker is placed in the tank of ultrasonic disperser, and fixing;
2. in the tank of ultrasonic disperser, add deionized water 1500ml, deionized water is wanted 9/10 of submergence beaker volume;
3. open ultrasonic generator, UW voltage 220V, power 100W, 65HZ, and constant, under 25 ℃ of temperature, under the UW effect, waste cotton fiber mixes with water, and is dispersed in the water liquid, and ultrasonic dispersing time 120min becomes dispersion liquid;
(7) in reaction kettle, preparation carbosphere under HTHP
It is in reaction kettle that waste cotton fiber prepares carbosphere, under the condition of 260 ℃ ± 1 ℃ of temperature, pressure 4.1MPa, carries out;
1. open reaction kettle, the waste cotton fiber+deionized water dispersion liquid that soaks after disperseing is moved in the reaction kettle, the axe lid is built in the insulation of reaction kettle indirect heating, makes reaction kettle be in sealed state;
2. open the reaction kettle 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 reaction kettle;
The agitator speed 200r/min of the waste cotton fiber+deionized water dispersion liquid in the reaction kettle, heating, pressurization, churning time are 480min;
3. cooling
Close electric heater, close whisking appliance 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 reaction kettle, 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 reactive group on the carbosphere surface that is shaped, and reaction formula is following:
Cellulose hydrolysis is a monose:
Figure FSA00000652706500041
In the formula:
Figure FSA00000652706500042
cellulose hydrolysis product glucose
Glucose generates isometry product fructose:
Figure FSA00000652706500043
In the formula:
The isomers fructose of
Figure FSA00000652706500051
glucose
The gluconate dehydratase cracking:
In the formula:
The hydrolysate 5-hydroxymethylfurfural of
Figure FSA00000652706500053
glucose
The hydrolysate furans of
Figure FSA00000652706500054
glucose
The hydrolysate 1 of
Figure FSA00000652706500055
glucose sugar; 2, the 4-pyrogallol
CH 3CHO: the hydrolysate acetaldehyde of glucose
Oxyhydroquinone and furans generation dehydration reaction:
In the formula:
Figure FSA00000652706500061
1; 2, the carbosphere intermediate product that generates after 4-pyrogallol and the furans dehydration reaction
5-hydroxymethylfurfural, oxyhydroquinone and furans generation aldol reaction:
Figure FSA00000652706500062
In the formula:
Figure FSA00000652706500063
5-hydroxymethylfurfural, 1; 2, generate the carbosphere intermediate product behind 4-pyrogallol and the furans generation aldol reaction;
Intermediate product further reacts:
Figure FSA00000652706500064
Figure FSA00000652706500071
In the formula:
Figure FSA00000652706500072
waste cotton fiber carbosphere
(8) standing demix is moved into waste cotton fiber carbosphere reaction solution in the beaker, standing demix, and time 60min outwells supernatant, retains the waste cotton fiber carbosphere;
(9) washing
1. the waste cotton fiber carbosphere is placed beaker, add absolute ethyl 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 a 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 reactive group are detected, analyze, characterize;
The appearance structure of use emission scan electron microscopic observation carbosphere;
Analyze the surface composition of carbosphere with IR;
With X-ray diffractometer the structure and the composition of product are analyzed;
Conclusion: through 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 reaction kettle, carry out; Completion under the reaction conditions of high temperature, high pressure, stirring; Reaction kettle (5) is a round shape, and reaction kettle (5) is outside for being incubated zone of heating (4), puts cotton fibre+deionized water dispersion liquid in the reaction kettle (6); Be kettle cover (3) and on the top of reaction kettle (5), on kettle cover (3), be provided with whisking appliance (1), TM (2), pressurization motor (8), tensimeter (9) by bolt (2) fixing seal; Right side at reaction kettle (6) connects electric control box (11) through lead (7), on electric control box (11), is provided with and stirs revolution image display (12), temperature in the kettle image display (13), stirs switch (14), power switch (15), temperature regulator (16), mixing speed modulator (17).
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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
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
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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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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
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
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
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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