CN102633249A - Method for rapidly preparing carbon microspheres by using cotton cellulose - Google Patents
Method for rapidly preparing carbon microspheres by using cotton cellulose Download PDFInfo
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- CN102633249A CN102633249A CN2012100921996A CN201210092199A CN102633249A CN 102633249 A CN102633249 A CN 102633249A CN 2012100921996 A CN2012100921996 A CN 2012100921996A CN 201210092199 A CN201210092199 A CN 201210092199A CN 102633249 A CN102633249 A CN 102633249A
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Abstract
The invention relates to a method for rapidly preparing carbon microspheres by using cotton cellulose. The method provided by the invention has the following steps of: using the cotton cellulose as a raw material; carrying out a hydrolysis reaction and a carbonization reaction by controlling a heating temperature, time and a reactant concentration in a reaction kettle through a hydrothermal synthesis method; and finally, preparing the carbon microspheres at a temperature of 300 DEG C and a pressure intensity of 10 MPa. The preparation method has the advantages of advanced process, fast speed, fewer used equipment, abundant raw material resources, low price and less energy requested by a carbonization process, and is a very ideal method for rapidly preparing the carbon microspheres by using the cotton cellulose. The preparation method provides a wide prospect for a high value-added carbon material for the plant cellulose.
Description
Technical field
The present invention relates to a kind ofly prepare the method for carbosphere fast, belong to the preparation of macromolecule carbon material and the technical field of application with gossypin.
Background technology
Carbosphere is one of important carbon material, and it has high chemicalstability, thermostability, and favorable conductive, heat conductivility are widely used in electrode materials, sorbent material, fuel cell, catalyzer and support of the catalyst; The preparation method of carbosphere has arc discharge method, chemical Vapor deposition process, laser evaporation method, catalytic pyrolysis method; These preparing methods mostly need high-energy, LP and expensive plant and instrument; And the present carbon source that adopts is extracted from coal ore and in the petroleum product mostly; Staple is alkene, the refinery coke of alkynes compounds, pitch coke, coal tar, and these petrochemical industry by products are nonrenewable resource, and these resources reduce just gradually.
Gossypin is the abundantest in the world natural organic matter, accounts for more than 50% of vegitabilia's carbon content, and gossypin is elementary composition by carbon, hydrogen, three kinds of oxygen; Carbon content is up to more than 44.44%; The gossypin aboundresources, except the cotton macrofiber is used as the textile raw material, other tankage that can not be used to weave, linters, cotton seed and cotton stalk; Their content of cellulose is also very high, all can do carbon source and use; In addition, the whole world can produce the biomass residue of hundreds billion of tons rich cellulose every year, and they all are the very high organic cpds of carbon elements, for producing of carbon material provides very advantageous conditions.
Summary of the invention
Goal of the invention:
The objective of the invention is the situation to background technology, the employing gossypin is a carbon source, and in autoclave, under 300 ℃ of temperature, degradable carbon is combined to carbosphere fast, to improve the preparation efficiency and the quality of carbosphere.
Technical scheme
The chemical substance material that the present invention uses is: gossypin, ethanol, hydrochloric acid, deionized water, the accurate consumption of its combination matching is: with gram, milliliter is measure unit
The preparation method is following:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out the control of quality purity, concentration:
(2) pulverize, clean
Place kibbler to pulverize gossypin, sieve with 60 eye mesh screens then, crushing screening carries out repeatedly, and after sieving, gossypin becomes fine powder, fine powder particle diameter≤0.25mm;
(3) cleaning reaction still
In reaction kettle, inject hydrochloric acid 100mL, scrub 10min, inject deionized water 150mL then, scrub 10min, dry then with hairbrush;
(4) preparation aqueous hydrochloric acid
Measure hydrochloric acid 21.1mL ± 0.01mL, deionized water 250mL ± 1mL, add in the beaker, stir 5min, it is mixed, become: the aqueous hydrochloric acid of 0.5mol/L with whisking appliance;
(5) configuration gossypin hydrochloric acid soln
Take by weighing gossypin 10.0g ± 0.01g, measure aqueous hydrochloric acid 250mL ± 1mL of 0.5mol/L;
Place beaker, stir with whisking appliance, stir speed (S.S.) 400r/min, churning time 2min stirs the back and becomes mashed prod;
(6) preparation carbosphere
Prepare carbosphere with gossypin and in autoclave, carry out, under heating, pressurization, degraded, carburizing reagent, accomplish;
1. mashed prod is added in the autoclave, seal with kettle cover then;
2. open the reaction kettle well heater;
Temperature of reaction kettle is begun to heat up by 20 ℃ of normal temperature, 5 ℃/min of heat-up rate, and the TRT is 24min ± 2min; When temperature rises to 140 ℃ ± 3 ℃, gas evaporation in insulation, the constant temperature 150min ± 2min, reaction kettle; Pressure is 0.5MPa in the reaction kettle, and gossypin carries out DeR;
3. continue then to heat up, 5 ℃/min of heat-up rate, TRT 32min ± 2min, when temperature rose to 300 ℃ ± 3 ℃, pressure was 10MPa in insulation, the constant temperature 420min ± 2min, still;
The gossypin carbonization, modality generates carbosphere;
Gossypin carries out DeR under the state that 140 ℃ ± 3 ℃, hydrochloric acid exist, when temperature rose to 300 ℃, gossypin generation pyrolysis and carburizing reagent formed the physical chemistry transformation of gossypin-degraded-carbonization, the generation carbosphere;
The generative process of carbosphere:
I gossypin hydrolytic deterioration
In reaction kettle, under 140 ℃ ± 3 ℃, 0.5MPa state, issue unboiled water in the hydrogen ion effect and separate degraded, be transformed into oligose, glucose; The hydrolytic deterioration reaction equation is following:
In the formula:
C
6H
12O
6---glucose
(C
6H
10O
5)
m---oligose, m=2-3
H
2O---water vapour
The II carbonization
Under 300 ℃ ± 3 ℃, the HTHP of 10MP, oligose, glucose pyrolysis, dehydration, the CH that pyrolysis produces
4, CO, and organic molecule in high temperature and high pressure environment, be transformed into carboxyl or carbonyl, be present in carbon surface, form the agraphitic carbon microballoon, the carburizing reagent equation is following:
In the formula:
C---carbon
H
2---hydrogen
CO---carbon monoxide
CO
2---carbonic acid gas
C
5H
4O
2---alditol
CH
3COOH---acetate
H
2O---water vapour
(7) product cooling
The off-response kettle heater stops heating, and carbosphere cools to 20 ℃ ± 3 ℃ of normal temperature with the furnace in the still;
(8) deionized water wash
Carbosphere in the reaction kettle is moved in the beaker, add deionized water 250mL,, become: cleaning mixture with whisking appliance agitator treating 10min;
(9) spinning
Cleaning mixture is moved in the centrifuge tube, is spinning on the whizzer of 4000r/min at rotating speed, removes supernatant, retains black precipitate;
(10) ethanol supersound washing
Black precipitate is placed beaker, add ethanol 250mL, place then in the ultrasonic cleaning machine, carry out supersound washing 20min, become: alcohol mixeding liquid;
(11) suction filtration
Alcohol mixeding liquid is placed the B on the filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, washings is evacuated in the filter flask;
Washing with alcohol, suction filtration repeat 5 times;
(12) vacuum-drying
The product filter cake is placed quartz container, places vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 80Pa, time of drying 360min;
Get end product after the drying: black powder carbosphere;
(13) detect, analyze, characterize
Pattern, color and luster, composition, the chemical physics performance of carbosphere to preparation detects, analyzes and characterize;
1. carry out IR spectroscopy with infrared absorption spectrometer;
2. carry out the product morphology analysis with ESEM;
3. with X-ray diffractometer product is carried out structure detection, analysis;
Conclusion: carbosphere is the black powder, powder granule diameter≤1um; Hydroxyl, carbonyl and carboxyl functional group are contained in the carbosphere surface of hydrothermal carbonization preparation;
(14) product stores
Carbosphere to preparation is stored in the brown transparent Glass Containers, and airtight lucifuge stores, and storing temp is 20 ℃ ± 3 ℃, and relative humidity≤10% is stored in drying, cool place, the clean environment.
Beneficial effect
The present invention compares with background technology has tangible advance, is to be carbon source with the gossypin, utilizes hydrothermal synthesis method, in reaction kettle, through pressure, reactant concn in regulation and control reaction times, temperature, the still, obtains the surface and contains the carbosphere that enriches functional group; Can use in catalysis, absorption, separation, field of functional materials, this fast preparation method technology is advanced, and use equipment is few; Rapid and simple; Easy to operate, raw material sources are abundant, and are cheap; The required little energy of carbonization process, this method are that plant class material changes into the high added value carbon material and opened up bright prospects.
Description of drawings
Fig. 1 prepares the carbosphere state graph for reaction kettle
Fig. 2 is reactor temperature and time coordinate graph of a relation
Fig. 3 amplifies 10,000 times of shape appearance figures for the carbosphere field emission scanning electron microscope
Fig. 4 is the carbosphere infrared spectrogram
Fig. 5 is the carbosphere X ray diffracting spectrum
Shown in the figure, list of numerals is following:
1, reaction kettle, 2, sealing cover, 3, whisking appliance, 4, thermopair, 5, sealing-ring; 6, tensimeter, 7, water vapour, 8, hydrating solution, 9, the reaction kettle supervisory control desk, 10, image display; 11, power switch, 12, the electrically heated modulator, 13, the whisking appliance modulator, 14, PL; 15, gasket, 16, gasket, 17, holding bolt, 18, the reaction kettle heated seats.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified:
Shown in Figure 1, for reaction kettle prepares the carbosphere state graph, 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.
Prepare carbosphere with gossypin and in reaction kettle, carry out, in heating, pressurization, hydrolysis, carbonation reaction, accomplish; Reaction kettle is a round shape, makes with stainless material, and the top of reaction kettle 1 is sealing cover 2, and by sealing-ring 5 sealings, whisking appliance 3 and gasket 16, thermopair 4 and gasket 15 is set on sealing cover 2, and stretches in the reaction kettle 1; The bottom is that hydrating solution 8, top are water vapour 7 in the reaction kettle 1; Reaction kettle 1 places on the reaction kettle heated seats 18, and reaction kettle heated seats 18 places on the reaction kettle supervisory control desk 9, and reaction kettle supervisory control desk 9 is provided with image display 10, power switch 11, electrically heated modulator 12, whisking appliance modulator 13, PL 14.
Shown in Figure 2, be reactor temperature and time coordinate graph of a relation, Heating temperature begins to heat up by 20 ℃, i.e. the A point; 5 ℃/min of heat-up rate, when temperature rises to 140 ℃ ± 3 ℃, i.e. B point, constant temperature, insulation 150min ± 2min; Be the B-C section, the reaction that is hydrolyzed continues to rise to 300 ℃ ± 3 ℃ with 5 ℃/min speed, i.e. the D point then; At this temperature constant temperature, insulation 420min ± 2min, promptly the D-E section carries out carburizing reagent, and the gossypin modality is a carbosphere; Stop heating then, make it naturally cool to 20 ℃, i.e. F point, Heating temperature was directly proportional with the time.
Shown in Figure 3, for the carbosphere field emission scanning electron microscope amplifies 10,000 times of shape appearance figures, carbosphere is the black circular granular among the figure, be irregular push away long-pending.
Shown in Figure 4, be the carbosphere infrared spectrogram, can know among the figure: 3100cm
-1The absorption peak at place is hydroxyl-OH charateristic avsorption band, 1710cm
-1Peak, wave number place is the vibration absorption peak of carboxyl-COOH, 1620cm
-1The absorption peak at place is a carbonyl C=O charateristic avsorption band.
Shown in Figure 5, be product carbosphere X ray diffracting spectrum, ordinate zou is a diffraction intensity, X-coordinate is diffraction angle 2 θ, can know among the figure: the peak among the figure is the characteristic peak of agraphitic carbon, 2 θ=25.4 °, correspondence belongs to C (002).
Claims (3)
1. one kind prepares the method for carbosphere fast with gossypin, and it is characterized in that: the chemical substance material of use is: gossypin, ethanol, hydrochloric acid, deionized water, the accurate consumption of its combination matching is: with gram, milliliter is measure unit
The preparation method is following:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out the control of quality purity, concentration:
(2) pulverize, clean
Place kibbler to pulverize gossypin, sieve with 60 eye mesh screens then, crushing screening carries out repeatedly, and after sieving, gossypin becomes fine powder, fine powder particle diameter≤0.25mm;
(3) cleaning reaction still
In reaction kettle, inject hydrochloric acid 100mL, scrub 10min, inject deionized water 150mL then, scrub 10min, dry then with hairbrush;
(4) preparation aqueous hydrochloric acid
Measure hydrochloric acid 21.1mL ± 0.01mL, deionized water 250mL ± 1mL, add in the beaker, stir 5min, it is mixed, become: the aqueous hydrochloric acid of 0.5mol/L with whisking appliance;
(5) configuration gossypin hydrochloric acid soln
Take by weighing gossypin 10.0g ± 0.01g, measure aqueous hydrochloric acid 250mL ± 1mL of 0.5mol/L;
Place beaker, stir with whisking appliance, stir speed (S.S.) 400r/min, churning time 2min stirs the back and becomes mashed prod;
(6) preparation carbosphere
Prepare carbosphere with gossypin and in autoclave, carry out, under heating, pressurization, degraded, carburizing reagent, accomplish;
1. mashed prod is added in the autoclave, seal with kettle cover then;
2. open the reaction kettle well heater;
Temperature of reaction kettle is begun to heat up by 20 ℃ of normal temperature, 5 ℃/min of heat-up rate, and the TRT is 24min ± 2min; When temperature rises to 140 ℃ ± 3 ℃, gas evaporation in insulation, the constant temperature 150min ± 2min, reaction kettle; Pressure is 0.5MPa in the reaction kettle, and gossypin carries out DeR;
3. continue then to heat up, 5 ℃/min of heat-up rate, TRT 32min ± 2min, when temperature rose to 300 ℃ ± 3 ℃, pressure was 10MPa in insulation, the constant temperature 420min ± 2min, still;
The gossypin carbonization, modality generates carbosphere;
Gossypin carries out DeR under the state that 140 ℃ ± 3 ℃, hydrochloric acid exist, when temperature rises to 300 ℃, and gossypin generation pyrolysis and carburizing reagent, the physical chemistry that forms gossypin-degraded-carbonization changes, the generation carbosphere;
The generative process of carbosphere:
I gossypin hydrolytic deterioration
In reaction kettle, under 140 ℃ ± 3 ℃, 0.5MPa state, issue unboiled water in the hydrogen ion effect and separate degraded, be transformed into oligose, glucose; The hydrolytic deterioration reaction equation is following:
In the formula:
C
6H
12O
6---glucose
(C
6H
10O
5)
m---oligose, m=2-3
H
2O---water vapour
The II carbonization
Under 300 ℃ ± 3 ℃, the HTHP of 10MP, oligose, glucose pyrolysis, dehydration, the CH that pyrolysis produces
4, CO, and organic molecule in high temperature and high pressure environment, be transformed into carboxyl or carbonyl, be present in carbon surface, form the agraphitic carbon microballoon, the carburizing reagent equation is following:
In the formula:
C---carbon
H
2---hydrogen
CO---carbon monoxide
CO
2---carbonic acid gas
C
5H
4O
2---alditol
CH
3COOH---acetate
H
2O---water vapour
(7) product cooling
The off-response kettle heater stops heating, and carbosphere cools to 20 ℃ ± 3 ℃ of normal temperature with the furnace in the still;
(8) deionized water wash
Carbosphere in the reaction kettle is moved in the beaker, add deionized water 250mL,, become: cleaning mixture with whisking appliance agitator treating 10min;
(9) spinning
Cleaning mixture is moved in the centrifuge tube, is spinning on the whizzer of 4000r/min at rotating speed, removes supernatant, retains black precipitate;
(10) ethanol supersound washing
Black precipitate is placed beaker, add ethanol 250mL, place then in the ultrasonic cleaning machine, carry out supersound washing 20min, become: alcohol mixeding liquid;
(11) suction filtration
Alcohol mixeding liquid is placed the B on the filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, washings is evacuated in the filter flask;
Washing with alcohol, suction filtration repeat 5 times;
(12) vacuum-drying
The product filter cake is placed quartz container, places vacuum drying oven to carry out drying then, 80 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 80Pa, time of drying 360min;
Get end product after the drying: black powder carbosphere;
(13) detect, analyze, characterize
Pattern, color and luster, composition, the chemical physics performance of carbosphere to preparation detects, analyzes and characterize;
1. carry out IR spectroscopy with infrared absorption spectrometer;
2. carry out the product morphology analysis with ESEM;
3. with X-ray diffractometer product is carried out structure detection, analysis;
Conclusion: carbosphere is the black powder, powder granule diameter≤1um; Hydroxyl, carbonyl and carboxyl functional group are contained in the carbosphere surface of hydrothermal carbonization preparation;
(14) product stores
Carbosphere to preparation is stored in the brown transparent Glass Containers, and airtight lucifuge stores, and storing temp is 20 ℃ ± 3 ℃, and relative humidity≤10% is stored in drying, cool place, the clean environment.
2. according to claim 1ly a kind ofly prepare the method for carbosphere fast, it is characterized in that: prepare carbosphere with gossypin and in reaction kettle, carry out, in heating, pressurization, hydrolysis, carbonation reaction, accomplish with gossypin; Reaction kettle is a round shape, makes with stainless material, and the top of reaction kettle (1) is sealing cover (2), and by sealing-ring (5) sealing, whisking appliance (3) and gasket (16), thermopair (4) and gasket (15) is set on sealing cover (2), and stretches in the reaction kettle (1); The interior bottom of reaction kettle (1) is that hydrating solution (8), top are water vapour (7); Reaction kettle (1) places on the reaction kettle heated seats (18); Reaction kettle heated seats (18) places on the reaction kettle supervisory control desk (9), and reaction kettle supervisory control desk (9) is provided with image display (10), power switch (11), electrically heated modulator (12), whisking appliance modulator (13), PL (14).
3. according to claim 1ly a kind ofly prepare the method for carbosphere fast with gossypin, it is characterized in that: reactor temperature and time coordinate relation are: Heating temperature begins to heat up by 20 ℃, i.e. A point, 5 ℃/min of heat-up rate; When temperature rises to 140 ℃ ± 3 ℃, i.e. B point, constant temperature, insulation 150min ± 2min, i.e. B-C section; The reaction that is hydrolyzed continues to rise to 300 ℃ ± 3 ℃ with 5 ℃/min speed then, i.e. D point is at this temperature constant temperature, insulation 420min ± 2min; Be the D-E section, carry out carburizing reagent, the gossypin modality is a carbosphere, stops heating then; Make it naturally cool to 20 ℃, i.e. F point, Heating temperature was directly proportional with the time.
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| CN110407334A (en) * | 2019-07-30 | 2019-11-05 | 南京大学 | A kind of preparation and application for adsorbing nitrate ion synchronous denitrification denitrification organisms filler |
| CN113750958A (en) * | 2021-08-10 | 2021-12-07 | 华南理工大学 | Granular starch-based carbon material and preparation method and application thereof |
| CN113750958B (en) * | 2021-08-10 | 2023-10-20 | 华南理工大学 | Granular starch-based carbon material and preparation method and application thereof |
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