CN1895770A - Carbon-gas gel powder and its preparation - Google Patents
Carbon-gas gel powder and its preparation Download PDFInfo
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- CN1895770A CN1895770A CN 200610021241 CN200610021241A CN1895770A CN 1895770 A CN1895770 A CN 1895770A CN 200610021241 CN200610021241 CN 200610021241 CN 200610021241 A CN200610021241 A CN 200610021241A CN 1895770 A CN1895770 A CN 1895770A
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Abstract
A process for preparing nano-class or submicron-class carbon aerogel powder includes such steps as uniformly dispersing resorcin-formaldehide solution in insoluble oil phase under ultrasonic action while heating for gel polymerizing reaction, separating, washing, and carbonizing.
Description
Technical field
The present invention relates to the aerogel powder preparation field, particularly resorcinol-formaldehyde organic aerogel powder and carbon-gas gel powder and preparation method thereof.
Background technology
The characteristics of aeroge nano-powder material are exactly that particle size is little, effective surface area is big, and these characteristics make it have special small-size effect, skin effect, quantum size effect and macro quanta tunnel effect.This material have low atomic number, good conductivity, thermal conductivity low, with characteristics such as biocompatible, demonstrated wide application prospect in a lot of fields.Electrode material, Cerenkov detector, superinsulation material, catalyst and the carrier etc. that can be used as ultracapacitor and efficient rechargeable battery.
U.S. Patent number is 4997804,4873218 patent " low-density resorcinol formaldehyde aerogels " (Low density by people's such as Pekala application, resorcinol-formaldehyde aerogels), it is characterized in that utilizing base catalyst to prepare block resorcinol-formaldehyde low density foam.The block carbon aeroge is subjected to certain limitation on using.And high-specific surface area and the absorption property of powder formed carbon aeroge except possessing block aeroge also possesses good dispersiveness.
China Patent No. is 1135136 patents " a kind of method for preparing charcoal-aero gel " by people such as Li Yi application, it is characterized in that utilizing pitch, mesophase pitch, green coke to be raw material, forms granular charcoal-aero gel through adding thermal explosion.Though point out in the invention that particle size in the carbon aerogels network structure is less than 20nm, but specifically do not indicate the size of formed spacer gel particle, the dispersiveness of gel particle has material impact to catalyst performance, and the heating blast process in preparation technology exists unsafe factor.
Summary of the invention
The purpose of this invention is to provide a kind of carbon-gas gel powder and preparation method thereof.
The particle diameter of the carbon-gas gel powder of the present invention preparation is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 500m
2/ g～1000m
2/ g.
The preparation method of carbon-gas gel powder of the present invention in turn includes the following steps:
(a) solution preparation according to the mol ratio of resorcinol and formaldehyde be 1/2, resorcinol and catalyst n a
2CO
3Mol ratio be 50～1000 proportioning, being mixed with the mass percent concentration scope with triple distillation water is 5%～80% reaction solution;
(b) ultrasonic processing is under 5 ℃～10 ℃ conditions, and the reaction solution that step a is prepared joins in the airtight container that insoluble oil phase silicone oil is housed, through ultrasonication 0.5h～2h; 10 ℃～30 ℃ of control reaction temperatures continue ultrasonication 1h～5h, get light yellow suspension;
(c) product purification carries out centrifugation with the suspension of step b gained, gets yellow sludge thing; With n-hexane washing and precipitating thing 3～5 times, and centrifugation; Use ethanol washing and precipitating thing 1～3 time again, get alcohol suspending liquid;
(d) dry at 230 ℃～250 ℃, the alcohol suspending liquid of step c gained is carried out the ethanol supercritical drying, obtain yellowish-brown organic aerogel powder;
(e) carbonization vacuumizes degasification with the yellowish-brown organic aerogel powder of steps d gained at 150 ℃; under inert gas shielding, heat up with the heating rate of 1.5 ℃/min～5 ℃/min, in 600 ℃～1050 ℃ scope; constant temperature 5 hours, the carbon-gas gel powder of black.
The ultrasonication time first time of step b is 30 minutes.The insoluble oil phase silicone oil of step b adopts diethyl phthalate and homologue thereof to substitute.
The ethanol supercritical drying condition of steps d is 250 ℃, 5MPa.
The inert gas of step e is a kind of in nitrogen, helium, carbon dioxide or the argon gas.
The resorcinol of step a adopts a kind of replacement in phenol, hydroquinones and the phloroglucin.
The preparation of aerogel powder mainly adopts sol-gel process to combine with ultrasonic decentralized photo, the former is that the reaction solution with RF is dispersed among the insoluble oil phase material, form minimum micro emulsion drop, addition, cross-linking reaction take place in the drop scope and generate final aerogel powder.The latter utilizes the powerful ultrasonic energy of ultrasonic wave and cavitation and shear action, can form uniform reaction emulsion, and keeps microgel particle evenly to disperse by temperature controlling in course of reaction, does not take place big crosslinked.These two kinds of methods combine sol-gel process with ultrasonic decentralized photo, select and temperature control by dispersant, have obtained uniform sub-micron organic aerogel particle, obtain the littler carbon-gas gel powder of particle diameter through after the carbonization.In addition, in organic aerogel powder forming process, except hyperacoustic decisive role, the temperature control of the volume ratio of the selection of some experiment conditions such as dispersant, dispersant and decentralized photo and reaction system etc. also plays a part very crucial.The form of common organic aerogel and carbon gas gel generally is bulk, film and microballoon.Block RF aeroge can pass through mould molding or carbon gas gel (CRF) machine-shaping.Aerogel can be formed by bulk section, or by model or be coated with film preparation.Aerogel microball can be by the preparation of emulsion micro-packaging technology.
The invention provides and adopt sol-gel process to combine preparation resorcinol-formaldehyde organic aerogel powder and carbon-gas gel powder with ultrasonic decentralized photo.Ultrasonic wave energy discharges huge energy, localized hyperthermia's hyperbaric environment that produces and microjet with intense impact power, realize each evenly mixing mutually easily, the elimination local concentration is inhomogeneous, improve reaction speed, stimulate the formation of cenotype, and can also play shear action reuniting, the formation product that helps molecule is dispersed in the microemulsion with the form of nanoparticle, and can stable existence.The carbon-gas gel powder of this structure is the powder with loose structure, preparation method of the present invention, and reaction condition is gentle, is easy to control, and product stability at normal temperatures is high, and the aperture is little, self good dispersion.Carbon-gas gel powder of the present invention can be applicable to aspects such as battery terminal, electrode of super capacitor, air cleaning, drink water purifying, medicament slow release and catalyst loading.
Description of drawings
Fig. 1 is the resorcinol-formaldehyde organic aerogel powder transmission electron microscope photo among the present invention
Fig. 2 is a carbon gas gel powder transmission electron microscope photo of the present invention
The specific embodiment
Further specify the present invention below by specific embodiment.
Embodiment 1
To be catalyst with sodium carbonate, concentration be that 5% the resorcinol and the aqueous solution of formaldehyde are reactant liquor 5ml, and 250ml silicone oil is dispersant, and ultrasonication 1h under 5 ℃ of cryogenic conditions is warming up to 10 ℃ of ultrasonic 3h, is warming up to 20 ℃ then and continues ultrasonic 3h.By centrifugation nanoparticle product and oil phase, get yellow mud shape product.Clean mud shape product and centrifugation repeatedly with n-hexane.Clean and centrifugation with ethanol at last, parameter of noncentricity is: 10000 commentaries on classics/min, 10min gets yellow alcohol suspending liquid, gets resorcinol-formaldehyde organic aerogel powder with the ethanol supercritical drying.Temperature vacuumizes degasification for 150 ℃, at N
2Protect following 1.5 ℃/min to be warming up to 1050 ℃ of constant temperature 5 hours, obtain the carbon-gas gel powder of black.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 940m
2/ g.
Embodiment 2
Repeat the method for embodiment 1, but experiment condition is ultrasonication 2h under 4.5 ℃ of cryogenic conditions, is warming up to 8 ℃ of ultrasonic 3h, is warming up to 15 ℃ then and continues ultrasonic 3h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 960m
2/ g.
Embodiment 3
Repeating the method for embodiment 1, is reactant liquor but concentration is 10% resorcinol with the aqueous solution of formaldehyde, and silicone oil is dispersant, and ultrasonication 1h under 5 ℃ of cryogenic conditions is warming up to 8 ℃ of ultrasonic 3h, is warming up to 15 ℃ of ultrasonic 3h of continuation then.Temperature vacuumizes degasification for 150 ℃, and 1.5 ℃/min was warming up to 600 ℃ of constant temperature 5 hours under Ar protection, and the end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm-10nm, specific area 840m
2/ g.
Embodiment 4
Repeat the method for embodiment 3, but experiment condition is ultrasonication 2h under 4.5 ℃ of cryogenic conditions, is warming up to 9 ℃ of ultrasonic 3h, is warming up to 10 ℃ then and continues ultrasonic 3h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 850m
2/ g.
Embodiment 5
Repeat the method for embodiment 1, but concentration is that 15% the resorcinol and the aqueous solution of formaldehyde are reactant liquor, silicone oil is dispersant, and ultrasonication 1h under 5 ℃ of cryogenic conditions is warming up to 15 ℃ of ultrasonic 5h.Carbonisation 1.5 ℃/min under He protection was warming up to 800 ℃ of constant temperature 5 hours, and the end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 6.17nm, specific area 510m
2/ g.
Embodiment 6
The method of multiple embodiment 5, but experiment condition is ultrasonication 2h under 4.5 ℃ of cryogenic conditions, is warming up to 7 ℃ of ultrasonic 3h, is warming up to 9 ℃ then and continues ultrasonic 3h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 620m
2/ g.
Embodiment 7
Repeat the method for embodiment 1, but concentration is that 20% the resorcinol and the aqueous solution of formaldehyde are reactant liquor, silicone oil is dispersant, and ultrasonication 1h under 5 ℃ of cryogenic conditions is warming up to 12 ℃ of ultrasonic 5h.Carbonisation is at CO
2Protect following 1.5 ℃/min to be warming up to 900 ℃ of constant temperature 5 hours, the end product particle diameter is distributed in 50nm～500nm, and average pore size is at 3.98nm, specific area 930m
2/ g.
Embodiment 8
Repeat the method for embodiment 7, but experiment condition is ultrasonication 2h under 4.5 ℃ of cryogenic conditions, is warming up to 10 ℃ of ultrasonic 6h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 920m
2/ g
Embodiment 9
Repeat the method for embodiment 1, but concentration is that 30% the resorcinol and the aqueous solution of formaldehyde are reactant liquor, silicone oil is dispersant, and ultrasonication 2h under 4.5 ℃ of cryogenic conditions is warming up to 10 ℃ of ultrasonic 5h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～50nm, specific area 720m
2/ g.
Embodiment 10
Repeat the method for embodiment 1, but concentration is that 40% the resorcinol and the aqueous solution of formaldehyde are reactant liquor, silicone oil is dispersant, and ultrasonication 2h under 4 ℃ of cryogenic conditions is warming up to 9 ℃ of ultrasonic 5h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 660m
2/ g.
Embodiment 11
Repeating the method for embodiment 1, is reactant liquor but concentration is the aqueous solution of 50% resorcinol and formaldehyde, and silicone oil is dispersant, and ultrasonication 2h under 4 ℃ of cryogenic conditions is warming up to 8 ℃ of ultrasonic 5h.Carbonisation is at CO
2Protect following 2 ℃/min to be warming up to 900 ℃ of constant temperature 5 hours, the end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 650m
2/ g.
Embodiment 12
Repeat the method for embodiment 1, but concentration is that 60% the resorcinol and the aqueous solution of formaldehyde are reactant liquor, diethyl phthalate is a dispersant, and ultrasonication 2h under 4 ℃ of cryogenic conditions is warming up to 8 ℃ of ultrasonic 5h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 540m
2/ g.
Embodiment 13
Repeat the method for embodiment 1, but concentration is that 20% the phloroglucin and the aqueous solution of formaldehyde are reactant liquor, ultrasonication 2h under 4 ℃ of cryogenic conditions is warming up to 8 ℃ of ultrasonic 5h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 650m
2/ g.
Embodiment 14
Repeat the method for embodiment 1, but concentration is that 40% the phenol and the aqueous solution of formaldehyde are reactant liquor, ultrasonication 2h under 4 ℃ of cryogenic conditions is warming up to 8 ℃ of ultrasonic 5h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 550m
2/ g.
Embodiment 15
Repeat the method for embodiment 1, but concentration is that 40% the hydroquinones and the aqueous solution of formaldehyde are reactant liquor, ultrasonication 2h under 4 ℃ of cryogenic conditions is warming up to 8 ℃ of ultrasonic 5h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 500m
2/ g.
Embodiment 16
Repeating the method for embodiment 1, is reactant liquor but concentration is 40% the aqueous solution to benzenetriol and formaldehyde, and ultrasonication 2h under 4 ℃ of cryogenic conditions is warming up to 8 ℃ of ultrasonic 5h.The end product particle diameter is distributed in 50nm～500nm, and pore-size distribution is at 0.5nm～10nm, specific area 560m
2/ g.
Fig. 1 be with the resorcinol of gained among the present invention-formaldehyde organic aerogel powder suspension in ethanol, carry out the ultrasonic transmission electron microscope photo that disperses the back to be done.Photo shows that organic aerogel powder particle diameter is less than 500nm.
Fig. 2 is that the carbon gas gel powder with gained of the present invention is suspended in the ethanol, carries out the ultrasonic transmission electron microscope photo that disperses the back to be done.Show in the photo that carbonization gel powder particle diameter is less than 100nm.
Claims (7)
1. a carbon-gas gel powder is characterized in that, described carbon-gas gel powder possesses following parameter:
Particle diameter distribution 50nm～500nm, pore-size distribution 0.5nm～10nm, specific area 500m
2/ g～1000m
2/ g.
2. preparation method who is used for the carbon-gas gel powder of claim 1 in turn includes the following steps:
(a) solution preparation according to the mol ratio of resorcinol and formaldehyde be 1/2, resorcinol and catalyst n a
2CO
3Mol ratio be 50～1000 proportioning, being mixed with the mass percent concentration scope with triple distillation water is 5%～80% reaction solution;
(b) ultrasonic processing is under 5 ℃～10 ℃ conditions, and the reaction solution that step a is prepared joins in the airtight container that insoluble oil phase silicone oil is housed, through ultrasonication 0.5h～2h; 10 ℃～30 ℃ of control reaction temperatures continue ultrasonication 1h～5h, get light yellow suspension;
(c) product purification carries out centrifugation with the suspension of step b gained, gets yellow sludge thing; With n-hexane washing and precipitating thing 3～5 times, and centrifugation; Use ethanol washing and precipitating thing 1～3 time again, get alcohol suspending liquid;
(d) dry at 230 ℃～250 ℃, the alcohol suspending liquid of step c gained is carried out the ethanol supercritical drying, obtain yellowish-brown organic aerogel powder;
(e) carbonization vacuumizes degasification with the yellowish-brown organic aerogel powder of steps d gained at 150 ℃; under inert gas shielding, heat up with the heating rate of 1.5 ℃/min～5 ℃/min, under 600 ℃～1050 ℃; constant temperature 5 hours, the carbon-gas gel powder of black.
3. the preparation method of carbon-gas gel powder according to claim 2 is characterized in that, the ultrasonication time first time of described step b is 30 minutes.
4. the preparation method of carbon-gas gel powder according to claim 2 is characterized in that, the ethanol supercritical drying condition of described steps d is 250 ℃, 5MPa.
5. the preparation method of carbon-gas gel powder according to claim 2 is characterized in that, the inert gas of described step e is a kind of in nitrogen, helium, carbon dioxide or the argon gas.
6. the preparation method of carbon-gas gel powder according to claim 2 is characterized in that, the insoluble oil phase silicone oil of described step b adopts diethyl phthalate and homologue thereof to substitute.
7. the preparation method of carbon-gas gel powder according to claim 2 is characterized in that, the resorcinol of described step a adopts a kind of replacement in phenol, hydroquinones and the phloroglucin.
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