CN109908878A - A kind of classifying porous cellulose base charcoal-aero gel and preparation method thereof - Google Patents
A kind of classifying porous cellulose base charcoal-aero gel and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of classifying porous cellulose base charcoal-aero gel, belong to charcoal-aero gel technical field.The present invention is using the extensive microcrystalline cellulose in source as raw material, and cheap and easy to get, production cost is low, meets sustainable development requirement；Preparation method provided by the invention is simple, environmental-friendly, meets green preparation and requires, is suitable for large-scale production；The present invention can realize the control to classifying porous charcoal-aero gel specific surface area, pore-size distribution, the classifying porous cellulose base charcoal-aero gel of gained has high-specific surface area and high porosity, and internal is in that multistage divides hole state by controlling activation condition.Embodiment shows classifying porous cellulose base charcoal-aero gel specific surface area provided by the invention up to 1123m2/ g, total hole volume is up to 0.5cm3/g。
Description
Technical field
The present invention relates to charcoal-aero gel technical field, in particular to a kind of classifying porous cellulose base charcoal-aero gel and its system
Preparation Method.
Background technique
Charcoal-aero gel is a kind of lightweight, porous, amorphous state, block nanometer Carbon Materials, had both aeroge high porosity,
The conduction of the characteristics of high-specific surface area and Carbon Materials, high temperature resistant, acid and alkali-resistance and it is degradable the advantages that, catalyst carrier,
The fields such as adsorbent material and electrochemistry have potential application.
The preparation of classifying porous charcoal-aero gel and the control of charcoal-aero gel pore structure are always scientific research emphasis.Mesh
Forward pass controlling is mainly phenolic aldehyde performed polymer substance for the raw material of charcoal-aero gel, and synthesis process is complicated, it is difficult to meet industrialization
Production；Simultaneously in the preparation classifying porous charcoal-aero gel of nanometer, generally use alkali activation and the techniques such as phosphoric acid activation, it is at high cost and
There is corrosivity to carbonization device, be unfavorable for industrialization development, and alkali activation can not control charcoal gas with phosphoric acid activation well
The pore structure of gel.
Summary of the invention
In view of this, it is an object of that present invention to provide a kind of classifying porous cellulose base charcoal-aero gels and preparation method thereof.
The preparation method of classifying porous cellulose base charcoal-aero gel provided by the invention is simple, environmental-friendly, meets green preparation and requires,
Suitable for large-scale production, obtained classifying porous cellulose base charcoal-aero gel has high-specific surface area and high porosity, and interior
Portion divides hole state in multistage.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
A kind of preparation method of classifying porous cellulose base charcoal-aero gel, comprising the following steps:
(1) it is successively freezed after mixing sodium hydroxide, urea with water, defrosting processing, obtains pretreatment fluid；
(2) microcrystalline cellulose and epoxychloropropane are sequentially added in Xiang Suoshu pretreatment fluid, are stood after stirring, are obtained primary
Gel；
(3) to precooling and freeze-drying is successively carried out after the primary gel washing, cellulose base aeroge is obtained；
(4) the cellulose base aeroge is heat-treated, obtains classifying porous cellulose base charcoal-aero gel；
The heat treatment includes three phases, is followed successively by pre- carbonization stage, carbonization stage and activation stage；
The protective atmosphere of the pre- carbonization stage be inert gas, temperature be 200~400 DEG C, soaking time be 0.5~
3h；
The protective atmosphere of the carbonization stage is inert gas, and temperature is 800~1100 DEG C, and soaking time is 0.5~3h；
The protective atmosphere of the activation stage is activated gas, and temperature is 800~1100 DEG C, and soaking time is 0.5~3h.
Preferably, the mass ratio of sodium hydroxide, urea and water is (5~8): (9~14) in the step (1): (78~
84)。
Preferably, the temperature freezed in the step (1) is -5~-12 DEG C, the time of freezing is 12~for 24 hours.
Preferably, the mass ratio of microcrystalline cellulose and pretreatment fluid is 0.5~3% in the step (2), the epoxy chlorine
The amount ratio of propane and pretreatment fluid is (8~12) mL:100g.
Preferably, the time stirred in the step (2) is 2~3h, the time of the standing is 18~for 24 hours.
Preferably, the precooling in the step (3) is Liquid nitrogen precooler jelly, and the time of the precooling is 0.5~3min；
The temperature of the freeze-drying is -50~-60 DEG C, and the time of freeze-drying is 40~48h.
Preferably, the heating rate of pre- carbonization stage is 2~5 DEG C/min in the step (4)；The liter of the carbonization stage
Warm rate is 3~8 DEG C/min.
Preferably, the activated gas of activation stage is CO in the step (4)2, vapor, flue gas, oxygen and air
One or more of.
Preferably, the flow of activation stage activated gas is 0.5~8L/min in the step (4).
The present invention provides the classifying porous cellulose base charcoal-aero gels of above-mentioned preparation method preparation.
The present invention provides a kind of preparation methods of classifying porous cellulose base charcoal-aero gel, first by sodium hydroxide, urea
It is mixed with water, microcrystalline cellulose is added after freezing, defrosting processing and epoxychloropropane obtains primary gel, then carries out precooling
And freeze-drying, cellulose base aeroge is obtained, finally cellulose base aeroge is heat-treated, obtains classifying porous fiber
Plain based charcoal aerogel.The present invention is using the extensive microcrystalline cellulose in source as raw material, and cheap and easy to get, production cost is low, and satisfaction can be held
Continuous demand for development；Preparation method of the present invention is simple, environmental-friendly, meets green preparation and requires, is suitable for large-scale production；This hair
It is bright to realize the control to porous charcoal-aero gel specific surface area, pore-size distribution, gained is classifying porous by controlling activation condition
Cellulose base charcoal-aero gel has high-specific surface area and high porosity, and internal is in that multistage divides hole state.Embodiment shows this hair
The classifying porous cellulose base charcoal-aero gel specific surface area of bright offer is up to 1123m2/ g, total hole volume is up to 0.5cm3/g。
Detailed description of the invention
Fig. 1 is the SEM figure of the 1 classifying porous cellulose base charcoal-aero gel of gained of embodiment；
Fig. 2 is the TEM figure of the 1 classifying porous cellulose base charcoal-aero gel of gained of embodiment；
Fig. 3 is nitrogen adsorption-desorption isotherm figure of the 1 classifying porous cellulose base charcoal-aero gel of gained of embodiment；
Fig. 4 is the specific surface area of the 1 classifying porous cellulose base charcoal-aero gel of gained of embodiment with varying aperture curve.
Specific embodiment
The present invention provides a kind of preparation methods of classifying porous cellulose base charcoal-aero gel, comprising the following steps:
(1) it is successively freezed after mixing sodium hydroxide, urea with water, defrosting processing, obtains pretreatment fluid；
(2) microcrystalline cellulose and epoxychloropropane are sequentially added in Xiang Suoshu pretreatment fluid, are stood after stirring, are obtained primary
Gel；
(3) to precooling and freeze-drying is successively carried out after the primary gel washing, cellulose base aeroge is obtained；
(4) the cellulose base aeroge is heat-treated, obtains classifying porous cellulose base charcoal-aero gel；
The heat treatment includes three phases, is followed successively by pre- carbonization stage, carbonization stage and activation stage；
The protective atmosphere of the pre- carbonization stage be inert gas, temperature be 200~400 DEG C, soaking time be 0.5~
3h；
The protective atmosphere of the carbonization stage is inert gas, and temperature is 800~1100 DEG C, and soaking time is 0.5~3h；
The protective atmosphere of the activation stage is activated gas, and temperature is 800~1100 DEG C, and soaking time is 0.5~3h.
The present invention successively freezes after mixing sodium hydroxide, urea with water, defrosting is handled, and obtains pretreatment fluid.?
In the present invention, the mass ratio of the sodium hydroxide, urea and water is preferably (5~8): (9~14): (78~84), more preferably
(6~7): (10~12): (80~82).The present invention does not have particular/special requirement to the hybrid mode of sodium hydroxide, urea and water, uses
Hybrid mode well known to those skilled in the art.In the present invention, the temperature of the freezing is preferably -5~-12 DEG C, more
Preferably -10 DEG C；The time of freezing is preferably 12~for 24 hours, more preferably 18~20h；The present invention preferably at room temperature will
Mixture after freezing thaws to just without the state of ice.The present invention is handled by freeze-thaw and can be destroyed between cellulose
Hydrogen bond, the dissolution of accelerating fibers element.
After obtaining pretreatment fluid, the present invention sequentially adds microcrystalline cellulose and epoxychloropropane into the pretreatment fluid,
It is stood after stirring, obtains primary gel.The present invention does not have specific requirement to the source of microcrystalline cellulose, uses this field routine city
The microcrystalline cellulose sold.In the present invention, the mass ratio of the microcrystalline cellulose and pretreatment fluid is preferably 0.5~3%,
More preferably 1~2%；The amount ratio of the epoxychloropropane and pretreatment fluid is preferably (8~12) mL:100g, more preferably
10mL:100g.In the present invention, the mode of the stirring is preferably magnetic agitation；Microcrystalline cellulose is preferably first added in the present invention
It is once stirred, adds epoxychloropropane and carry out secondary agitation, the time once stirred is preferably 2~4h, more excellent
It is selected as 3h；The time of the secondary agitation is preferably 2~3h, more preferably 2.5h.In the present invention, the time of the standing is excellent
It is selected as 18~for 24 hours.
After obtaining primary gel, the present invention is obtained to precooling and freeze-drying is successively carried out after the primary gel washing
To cellulose base aeroge.The present invention does not have particular/special requirement to the mode of the washing, and use is well known to those skilled in the art
Mode of washing is by the primary gel detergent to neutrality.In the present invention, the precooling is preferably that Liquid nitrogen precooler freezes, institute
The time for stating precooling is preferably 0.5~3min, more preferably 1~2min；The temperature of the freeze-drying preferably -50~-
60 DEG C, more preferably -55 DEG C；The time of freeze-drying is preferably 40~48h；It is dry that the present invention carries out freezing preferably in cooling driers
It is dry.
After obtaining cellulose base aeroge, the present invention is heat-treated cellulose base aeroge, obtains classifying porous fibre
Tie up plain based charcoal aerogel；In the present invention, it is described heat treatment include three phases, be followed successively by pre- carbonization stage, carbonization stage and
Activation stage.
In the present invention, the protective atmosphere of the pre- carbonization stage is inert gas, preferably nitrogen, helium, neon, argon
One or more of gas and xenon, temperature are 200~400 DEG C, and preferably 250~350 DEG C, soaking time is 0.5~3h, excellent
It is selected as 1~2h；The initial temperature of the pre- carbonization stage is preferably room temperature, and the heating rate of the pre- carbonization stage is preferably 2
Since~5 DEG C/min, more preferably 3~4 DEG C/min, the present invention calculate soaking time being warming up to pre- carbonization temperature.In this hair
In bright, pre- carbonization stage can remove the volatile materials in cellulose base aeroge.
In the present invention, the protective atmosphere of the carbonization stage is inert gas, preferably nitrogen, helium, neon, argon gas
One or more of with xenon, temperature is 800~1100 DEG C, and preferably 900~1000 DEG C, soaking time is 0.5~3h, excellent
It is selected as 1~2h；Initial temperature is preferably 200~400 DEG C, and more preferably 250~350 DEG C；The heating rate of the carbonization stage
Preferably 3~8 DEG C/min, more preferably 4~6 DEG C, since the present invention calculate soaking time being warming up to carbonization temperature.In this hair
In bright, carbonization stage can make cellulose base aeroge carbonize to form charcoal-aero gel charcoal skeleton.
In the present invention, the protective atmosphere of the activation stage is activated gas, and the activated gas is preferably CO2, water
One or more of steam, flue gas, oxygen and air, the ingredient of the flue gas are CO, CO2、H2O and O2Gaseous mixture；
The temperature of the activation is 800~1100 DEG C, and preferably 900~1000 DEG C, soaking time is 0.5~3h, preferably 1~2h.
In the present invention, the flow of the activated gas is preferably 0.5~8L/min, more preferably 3~5L/min.The present invention passes through work
Change gas to perform etching charcoal-aero gel charcoal skeleton, so that pore structure occurs in charcoal-aero gel charcoal, obtains classifying porous cellulose
Based charcoal aerogel.The present invention controls the etching degree of charcoal-aero gel charcoal skeleton by the temperature and time of control activation, passes through
The flow of activated gas is controlled to guarantee the stability of etching process.
After the completion of heat treatment, the present invention preferably cools down to the classifying porous cellulose base charcoal-aero gel.In this hair
In bright, the protective atmosphere of the cooling is preferably inert gas, more preferably one in nitrogen, helium, neon, argon gas and xenon
Kind is several.In the present invention, the mode of the cooling is preferably cooled to room temperature.
The present invention provides the classifying porous cellulose base charcoal-aero gels of above-mentioned preparation method preparation.Provided by the invention point
Grade porous cellulose based charcoal aerogel has high-specific surface area and high porosity, and internal is in that multistage divides hole state.
Classifying porous cellulose base charcoal-aero gel provided by the invention and preparation method thereof is carried out below with reference to embodiment
Detailed description, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
By 7g sodium hydroxide, 12g urea is dissolved in 81g distilled water, is put into refrigerator and is freezed under the conditions of -10 DEG C for 24 hours, takes
1.5g microcrystalline cellulose is added in thaw at RT out, and 9mL epoxychloropropane is added in magnetic agitation 2.5h, and magnetic agitation 2.5h takes
Magneton out is placed at room temperature for for 24 hours to gel is formed, and 10 times to neutral wash with distilled water, is slowly put into -196 DEG C of liquid nitrogen and carries out
Precooling, precooling time are 1min, and the sample of freezing is put into cooling driers after taking out and is freeze-dried, and are freeze-dried temperature
It is -55 DEG C, cooling time 48h, the sample after freeze-drying is put into tube furnace, N2It is warming up to 300 DEG C under gas shield, protects
60min is held, is warming up to 900 DEG C, closes N after keeping 60min2, it is passed through CO2, control CO2Flow is 5L/min, keeps 90min, is closed
Close CO2, it is passed through N2, naturally ring to room temperature and obtain classifying porous cellulose base charcoal-aero gel.
Electronic Speculum (SEM) analysis is scanned to the classifying porous cellulose base charcoal-aero gel of gained, gained SEM schemes such as Fig. 1 institute
Show；Transmission electron microscope (TEM) analysis is carried out to the classifying porous cellulose base charcoal-aero gel of gained, gained TEM figure is as shown in Figure 2.By
Fig. 1~2 are it is found that classifying porous cellulose base charcoal-aero gel provided by the invention has flourishing pore structure, and has classification
Porous characteristic.
Nitrogen adsorption-desorption test, gained nitrogen adsorption-desorption are carried out to the classifying porous cellulose base charcoal-aero gel of gained
Isollaothermic chart is as shown in figure 3, specific surface area is as shown in Figure 4 with varying aperture curve.Nitrogen adsorption-desorption isotherm is counted
It calculates, the results showed that the specific surface area of this classifying porous cellulose base charcoal-aero gel is up to 1123m2/ g, pore volume 0.5m3/ g, it is micro-
Hole ratio is 80%, average pore size 1.9nm.
Embodiment 2
By 60g sodium hydroxide, 100g urea is dissolved in 840g distilled water, is put into refrigerator and is freezed under the conditions of -10 DEG C
12h takes out thaw at RT, and 10g microcrystalline cellulose is added, and 90mL epoxychloropropane, magnetic agitation is added in magnetic agitation 4h
2.5h takes out magneton, is placed at room temperature for for 24 hours to gel is formed, wash with distilled water to neutral, be slowly put into -196 DEG C of liquid nitrogen into
Row precooling, precooling time are 3min, and the sample of freezing is put into cooling driers after taking out and is freeze-dried, freeze-drying temperature
Degree is -55 DEG C, and cooling time 48h, the sample after freeze-drying is put into tube furnace, is warming up to 350 DEG C under helium protection, protects
120min is held, is warming up to 1000 DEG C, closes helium after keeping 30min, is passed through vapor, control vapor flow is 0.5L/
Min keeps 120min, closes vapor, is passed through helium, naturally rings to room temperature and obtain classifying porous cellulose base charcoal-aero gel.
After tested, the specific surface area of this classifying porous cellulose base charcoal-aero gel is up to 1000m2/ g, pore volume are
0.45m3/ g, micropore ratio are 70%, average pore size 1.6nm.
Embodiment 3
By 8g sodium hydroxide, 14g urea is dissolved in 78g distilled water, is put into refrigerator and is freezed 18h under the conditions of -10 DEG C, takes
0.5g microcrystalline cellulose is added in thaw at RT out, and 8mL epoxychloropropane is added in magnetic agitation 4h, and magnetic agitation 2.5h takes out
Magneton is placed at room temperature for for 24 hours to gel is formed, wash with distilled water to neutrality, is slowly put into -196 DEG C of liquid nitrogen and carries out precooling,
The precooling time is 0.5min, and the sample of freezing is put into cooling driers after taking out and is freeze-dried, and freeze-drying temperature is -55
DEG C, cooling time 48h, the sample after freeze-drying is put into tube furnace, is warming up to 200 DEG C under argon gas protection, is kept
180min is warming up to 1100 DEG C, closes argon gas after keeping 180min, is passed through air, and control air mass flow is 8L/min, keeps
180min closes air, is passed through argon gas, naturally rings to room temperature and obtain classifying porous cellulose base charcoal-aero gel.
After tested, the specific surface area of this classifying porous cellulose base charcoal-aero gel is up to 980m2/ g, pore volume 0.5m3/
G, micropore ratio are 70%, average pore size 1.9nm.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of classifying porous cellulose base charcoal-aero gel, comprising the following steps:
(1) it is successively freezed after mixing sodium hydroxide, urea with water, defrosting processing, obtains pretreatment fluid；
(2) microcrystalline cellulose and epoxychloropropane are sequentially added in Xiang Suoshu pretreatment fluid, is stood after stirring, are obtained primary solidifying
Glue；
(3) to precooling and freeze-drying is successively carried out after the primary gel washing, cellulose base aeroge is obtained；
(4) the cellulose base aeroge is heat-treated, obtains classifying porous cellulose base charcoal-aero gel；
The heat treatment includes three phases, is followed successively by pre- carbonization stage, carbonization stage and activation stage；
The protective atmosphere of the pre- carbonization stage is inert gas, and temperature is 200~400 DEG C, and soaking time is 0.5~3h；
The protective atmosphere of the carbonization stage is inert gas, and temperature is 800~1100 DEG C, and soaking time is 0.5~3h；
The protective atmosphere of the activation stage is activated gas, and temperature is 800~1100 DEG C, and soaking time is 0.5~3h.
2. preparation method according to claim 1, which is characterized in that sodium hydroxide in the step (1), urea and water
Mass ratio is (5~8): (9~14): (78~84).
3. preparation method according to claim 1, which is characterized in that the temperature freezed in the step (1) is -5~-12
DEG C, time of freezing is 12~for 24 hours.
4. preparation method according to claim 1, which is characterized in that microcrystalline cellulose and pretreatment in the step (2)
The mass ratio of liquid is 0.5~3%, and the amount ratio of the epoxychloropropane and pretreatment fluid is (8~12) mL:100g.
5. preparation method according to claim 1 or 4, which is characterized in that the time stirred in the step (2) is 2~
3h, time of the standing is 18~for 24 hours.
6. preparation method according to claim 1, which is characterized in that the precooling in the step (3) is Liquid nitrogen precooler
Freeze, the time of the precooling is 0.5~3min；The temperature of the freeze-drying is -50~-60 DEG C, the time of freeze-drying
For 40~48h.
7. preparation method according to claim 1, which is characterized in that the heating speed of pre- carbonization stage in the step (4)
Rate is 2~5 DEG C/min；The heating rate of the carbonization stage is 3~8 DEG C/min.
8. preparation method according to claim 1, which is characterized in that the activated gas of activation stage in the step (4)
For CO2, vapor, flue gas, one or more of oxygen and air.
9. preparation method according to claim 1, which is characterized in that activation stage activated gas in the step (4)
Flow is 0.5~8L/min.
10. the classifying porous cellulose base charcoal-aero gel of the preparation of preparation method described in claim 1~9 any one.
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| CN113731359A (en) * | 2021-08-20 | 2021-12-03 | 西安理工大学 | Blocky carbon aerogel electro-adsorption material, preparation method and adsorbent |
| US20220080384A1 (en) * | 2020-09-16 | 2022-03-17 | Shaanxi University Of Science & Technology | Method for preparing modified cellulose aerogel for glycoprotein separation |
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| CN111439740A (en) * | 2020-04-07 | 2020-07-24 | 国际竹藤中心 | Nitrogen-doped bamboo cellulose carbon aerogel electrode material and preparation method thereof |
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