CN109704768A - A kind of method that non-water-base gel casting prepares foamy carbon - Google Patents
A kind of method that non-water-base gel casting prepares foamy carbon Download PDFInfo
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Abstract
A kind of method that non-water-base gel casting prepares foamy carbon belongs to foamy carbon molding and fabricating technology field.This method comprises: according to the ratio, organic monomer and crosslinking agent being mixed, is dissolved in alcohols organic solution, obtains monomer premixed liquid；Carbon-based presoma, pore creating material are added in monomer premixed liquid, ball milling mixing is uniform, initiator is added, catalyst is added dropwise in stirring and dissolving, it is continuously stirring to solidification, after 40~50 DEG C dry, in 190~210 DEG C of 4~6h of pre-oxidation, under an inert atmosphere, in 900~1200 DEG C of 2~4h of carbonization, foamy carbon is obtained.This method prepares foamed carbon material using nonaqueous solvents, and solid concentration reaches 65vol%, and size performance is stable and has preferable mobility；Solvent volatilizees when body drying, and fast, the process time is short, and blank shape size can design, and size reserving degree is high；The foam carbon parts of complicated shape can be prepared.
Description
Technical field
The present invention provides a kind of method that non-water-base gel casting prepares foamy carbon, can be applied to chemical industry, aviation boat
It, the fields such as electronics, belong to foamy carbon molding and fabricating technology field.
Background technique
Foamy carbon is also known as Carbon foam (CarbonFoam), is that a kind of steeped by hole has with what hole steep that wall interconnected formed
The light porous material of tridimensional network.According to the microstructure of its hole wall, graphitization and non-graphitized foam can be divided into
Carbon.Non-graphitized foamy carbon is also referred to as reticulated vitreous foamy carbon (ReticulatedVitreousCarbonFoam), is a kind of
The light porous material with tridimensional network of carbon skeleton and interconnected vestibule composition, with certain between carbon atom
Bonding mode be connected with each other, density is about 0.05~0.1g/cm3.Non-graphitized foamy carbon is low with density, hot property is excellent
The advantages that different, good stability of the dimension, thermal-shock resistance is both the heat-barrier material of great potential a kind of and a kind of high performance
Structural material.These excellent performances keep Carbon foam latent in the great application of many technical fields such as chemical industry, aerospace, electronics
Power.
Sucrose is a kind of water soluble carbohydrates, its availability and carbon content (42.1%) is high；Meanwhile there is scholar
Research shows that foamy carbon is prepared to melt sucrose as carbon matrix precursor, since the high-crosslinking-degree between polymer chain is conducive to improve
Its mechanical property (bibliography: NarasimmanR, PrabhakaranK.Preparation of carbon foams with
enhanced oxidation resistance by foaming molten sucrose using aboricacid
blowing agent[J].Carbon,2013,55(55):305-312).Therefore, sucrose, which is expected to become, prepares high-intensitive foam
The most suitable carbon matrix precursor of carbon material.
Gelcasting Technique is a kind of near-net-shape technology of novel preparation high-quality complicated shape ceramics.
Compared with other forming techniques, Gelcasting Technique has many advantages, such as: 1) scope of application is wider, wants to powder without special
It asks；2) near-net-shape can be achieved, prepare the ceramics of complicated shape；3) it is made to be higher than conventional molding process for blank strength
Green body can be machined；4) green body content of organics is low；5) green body and sintered body performance uniformity are good.Gel injection-moulding skill
The forming principle of art is to form macromolecular network structure by the chemical reaction of gel rubber system in slurry to consolidate ceramic powder in situ
Change is shaped to green body, and in forming process, solvent does not occur mobile so not will cause the mobile rearrangement of powder granule, and then guarantees
The homogeneity of ingredients of molding blank, particularly suitable for multi-component foamy carbon body preparation.
According to the solvent used whether for aqueous solution, gel injection-moulding is divided into aqueous gel casting and non-aqueous gelcasting
Mould.Water-base gel casting green body process, in order to reduce body defect, the drying condition needed is harsh, exists simultaneously sugarcane
Sugar dissolves in aqueous solution, and then a series of problems, such as influence solid phase amount.
Summary of the invention
In order to overcome the problems of the above-mentioned prior art, the purpose of the present invention is to provide a kind of non-aqueous gel castings
The method that molding prepares foamy carbon can be used in the preparation with the foamed carbon material of complex internal structure.
The technical solution of the present invention is as follows:
A kind of method that non-water-base gel casting prepares foamy carbon, comprising the following steps:
Step 1: allotment monomer premixed liquid
According to the ratio, organic monomer and crosslinking agent are mixed, is dissolved in alcohols organic solution, obtains monomer premixed liquid；Its
In, in mass ratio, organic monomer: crosslinking agent=(3~20): 1, in monomer premixed liquid, the mass concentration of organic monomer is 19~
21%；
Step 2: preparing non-water base foamy carbon precursor pulp
Carbon-based presoma, pore creating material are added in monomer premixed liquid, ball milling mixing is uniform, obtains non-water base foamy carbon forerunner
Somaplasm material；Wherein, the percent by volume of solid phase is 50~65Vol.% in non-water base foamy carbon precursor pulp；By volume,
Pore creating material: carbon-based presoma=(30~80): 30；
Step 3: gel casting forming
Into non-water base foamy carbon precursor pulp, initiator is added, stirring to initiator is dissolved, and then will be added and is caused
In the non-water base foamy carbon precursor pulp injection mold of agent, catalyst is added dropwise, continuously stirs, until non-water base foamy carbon forerunner
Body slurry curing obtains wet base；Wherein, the addition quality of initiator is the 0.4 of non-water base foamy carbon precursor pulp gross mass
~0.6wt.%；By volume, catalyst: non-water base foamy carbon precursor pulp=10~20mL:1L；
Step 4: body drying
By wet base in 40~50 DEG C of dryings, drying is no longer shunk to wet base, obtains biscuit；
Step 5: biscuit pre-oxidation
By biscuit in air atmosphere, 4~6h, the biscuit after being pre-oxidized are pre-oxidized at 190~210 DEG C；
Step 6: atmosphere sintering
Under an inert atmosphere by the biscuit after pre-oxidation, it in 900~1200 DEG C of 2~4h of carbonization, is cooled to room temperature, is steeped
Foam carbon.
In the step 1, the organic monomer be 1 acrylamide functionality acrylamides and/
Or the acrylic ester compound of 1 acrylate-functional groups, specifically: acrylamide, Methacrylamide -2- hydroxyl second
One of ester, hydroxyethyl methacrylate or several mixing.
In the step 1, the crosslinking agent be at least two acrylamide functionality acrylamides,
And/or the acrylic ester compound of at least two acrylate-functional groups, specifically: N, N`- methylene-bisacrylamide, two
One of ethylene glycol diacrylamine, polyethylene glycol dimethacrylate or several mixing.
In the step 1, the alcohols organic solution is ethyl alcohol, methanol, propyl alcohol, ethylene glycol, propylene glycol, n-butanol
At least one or several mixing.
In the step 2, the carbon-based presoma is one or more of sucrose, pitch, coal, organic polymer
Mixing.
In the step 2, the pore creating material is microcapsules or glass microballoon.
In the step 2, the solid phase is the carbon-based presoma and pore creating material that cannot be dissolved in monomer premixed liquid.
In the step 2, the ball milling, rotational speed of ball-mill be 1500~2000 turns/min, Ball-milling Time be 30min~
2h。
In the step 3, the initiator is ammonium persulfate, one in benzoyl peroxide, n,N-Dimethylaniline
Kind or several mixing.
The catalyst is N, N, N`, N`-tetramethylethylenediamine, N, N-dimethylaniline, isopropyl benzene hydroperoxide
The mixing of middle one or several kinds.
In the step 3, the time of initiator dissolution is preferably 5~10min.
In the step 3, described is continuously stirred, and uses speed of agitator for 5~10 turns/min, and effect is to prevent
Under high-speed stirred, there is bubble in cured wet base.
In the step 3, the solidification, curing time is 2~10min.
In the step 4, the drying, drying time is 40~60h.
The method that a kind of non-water-base gel casting of the invention prepares foamy carbon is compared with the prior art, beneficial
Effect is:
(1) present invention prepares foamed carbon material using nonaqueous solvents, and solid concentration reaches 65vol%, and size performance is stablized
And it has preferable mobility；Solvent volatilizees when body drying, and fast, the process time is short, and blank shape size can design, ruler
Very little reserving degree is high；The foam carbon parts of complicated shape can be prepared.
(2) under foamy carbon optimal conditions of the invention its compressive strength up to 15MPa, specific compress strength 40MPacm3/
G, considerably beyond the compression strength values of the 10MPa of current report foamed carbon material.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
Embodiment 1
A kind of method that non-water-base gel casting prepares foamy carbon, comprising the following steps:
Step 1. deploys monomer premixed liquid
By organic monomer acrylamide and crosslinking agent N, N`- methylene-bisacrylamide, by acrylamide: N, N`- methylene
After the mixing of base bisacrylamide=4:1 mass ratio, it is dissolved in methanol, obtains monomer premixed liquid；Wherein, it is premixed in monomer
In liquid, acrylamide mass concentration is 19%；
Step 2. prepares non-water base foamy carbon precursor pulp
By microcapsules: partial size is 200 mesh cane sugar powder=30:30 (volume ratio) below, is added in monomer premixed liquid, is passed through
After ball milling 30min, it is configured to the non-water base foamy carbon precursor pulp that microcapsules+cane sugar powder total volume content is 50vol.%；
Step 3. gel casting forming
Into non-water base foamy carbon precursor pulp, initiator ammonium persulfate is added, ammonium persulfate is non-water base foamy carbon
The 0.4wt% of precursor pulp quality, stirring 5min (stirring is just completely dissolved to initiator), are injected into mold immediately,
The ratio of the catalyst of 15mL is added with the non-water base foamy carbon precursor pulp of 1L, instills catalyst n, N, N`, N` ,-tetramethyl
Ethylenediamine, and low speed is carried out with 10 turns/min and continuously stirs 10min, until solution solidifies, to form wet base；
Step 4. body drying
Wet base is dried into 30h (drying to wet base is no longer shunk) together with mold at 45 DEG C jointly, obtains biscuit；
The pre-oxidation of step 5. biscuit
By biscuit obtained in above-mentioned steps in air atmosphere, it is placed in 190 DEG C of pre-oxidation 6h, the element after being pre-oxidized
Base；
Step 6. atmosphere sintering
By the biscuit after pre-oxidizing obtained in above-mentioned steps, 1200 DEG C of carbonization 2h in inert atmosphere (argon gas) are cooling
Foamy carbon is obtained to room temperature.
Analysis test, intensity 15MPa are carried out to foamy carbon manufactured in the present embodiment, specific compress strength is
28.3MPacm3/g。
Embodiment 2
A kind of method that non-water-base gel casting prepares foamy carbon, comprising the following steps:
Step 1. deploys monomer premixed liquid
In mass ratio, organic monomer Methacrylamide -2- hydroxy methacrylate: crosslinking agent diethylene glycol diacrylamine=
After the ratio mixing of 15:1, it is dissolved in ethyl alcohol, obtains monomer premixed liquid；Wherein, in monomer premixed liquid, methacryl
The mass concentration of amine -2- hydroxy methacrylate is 20%；
Step 2. prepares non-water base foamy carbon precursor pulp
By microcapsules: sucrose=50:30 (volume ratio) is added in monomer premixed liquid, after ball milling 60min, is configured to
Solid phase microcapsules+cane sugar powder total content is the non-water base foamy carbon precursor pulp of 57vol%；
Step 3. gel casting forming
Into non-water base foamy carbon precursor pulp, initiator benzoyl peroxide, the quality of benzoyl peroxide is added
For the 0.5wt% of non-water base foamy carbon precursor pulp quality, 7min (stirring is just completely dissolved to initiator) is stirred, immediately
It is injected into mold, the ratio of the catalyst of 20mL is added with the non-water base foamy carbon precursor pulp of 1L, instills catalyst n, N-
Dimethylaniline, and the low speed of 8 turns/min continuously stirs 5min, until solution solidifies, to form wet base；
Step 4. body drying
Wet base is dried into 25h (drying to wet base is no longer shunk) together with mold at 50 DEG C jointly, obtains biscuit；
The pre-oxidation of step 5. biscuit
By biscuit obtained in above-mentioned steps in air atmosphere, it is placed in 200 DEG C of pre-oxidation 5h, the element after being pre-oxidized
Base；
Step 6. atmosphere sintering
By the biscuit after pre-oxidizing obtained in above-mentioned steps, 1100 DEG C of carbonization 3h in inert atmosphere (argon gas) are cooling
Foamy carbon is obtained to room temperature.
Analysis test, intensity 12MPa are carried out to foamy carbon manufactured in the present embodiment, specific compress strength is
34.2MPacm3/g。
Embodiment 3
A kind of method that non-water-base gel casting prepares foamy carbon, comprising the following steps:
Step 1. deploys monomer premixed liquid
By organic monomer hydroxyethyl methacrylate: crosslinking agent polyethylene glycol dimethacrylate=10:1 mass ratio
After example mixing, it is dissolved in propylene glycol, obtains monomer premixed liquid；Wherein, in monomer premixed liquid, hydroxyethyl methacrylate matter
Measuring concentration is 21%；
Step 2. prepares non-water base foamy carbon precursor pulp
By microcapsules: sucrose=80:30 (volume ratio) is added in monomer premixed liquid, after ball milling 120min, is configured to
Solid phase microcapsules+cane sugar powder total volume content is the non-water base foamy carbon precursor pulp of 65vol%；
Step 3. gel casting forming
To non-water base foamy carbon precursor pulp, it is slowly added to initiator n,N-Dimethylaniline, n,N-Dimethylaniline
Quality is the 0.6wt% of non-water base foamy carbon precursor pulp gross mass, and (stirring to initiator is just completely molten by stirring 10min
Solution), it is injected into mold immediately, the ratio of the catalyst of 20mL is added with the non-water base foamy carbon precursor pulp of 1L, instillation is urged
Agent isopropyl benzene hydroperoxide, and the low speed of 5 turns/min continuously stirs 2min, until solution solidifies, to form wet base；
Step 4. body drying
Wet base is dried into 20h (drying to wet base is no longer shunk) together with mold at 55 DEG C jointly, obtains biscuit；
The pre-oxidation of step 5. biscuit
By biscuit obtained in above-mentioned steps in air atmosphere, it is placed in 210 DEG C of pre-oxidation 4h, the element after being pre-oxidized
Base；
Step 6. atmosphere sintering
By the biscuit after pre-oxidizing obtained in above-mentioned steps, 900 DEG C of carbonization 4h, are cooled in inert atmosphere (argon gas)
Room temperature obtains foamy carbon.
Analysis test, intensity 8MPa are carried out to foamy carbon manufactured in the present embodiment, specific compress strength is
23.5MPacm3/g。
Embodiment 4
A kind of method that non-water-base gel casting prepares foamy carbon, comprising the following steps:
Step 1. deploys monomer premixed liquid
In mass ratio, organic monomer: after the mixing of crosslinking agent=20:1 ratio, it is dissolved in the mixed liquor of ethyl alcohol and propyl alcohol
In, obtain monomer premixed liquid；Wherein, in monomer premixed liquid, the mass concentration of organic monomer is 21%；
Wherein, the organic monomer is the mixing of Methacrylamide -2- hydroxy methacrylate and hydroxyethyl methacrylate
Object, in mass ratio, Methacrylamide -2- hydroxy methacrylate: hydroxyethyl methacrylate=1:1；
The crosslinking agent is the mixture of diethylene glycol diacrylamine and polyethylene glycol dimethacrylate, by matter
Measure ratio, diethylene glycol diacrylamine: polyethylene glycol dimethacrylate=1:1；
In mass ratio, ethyl alcohol: propyl alcohol=20:1.
Step 2. prepares non-water base foamy carbon precursor pulp
By glass microballoon: pitch=80:30 (volume ratio) is added in monomer premixed liquid, after ball milling 60min, configuration
The non-water base foamy carbon precursor pulp for being 50vol% at solid phase glass microballoon+pitch total content；
Step 3. gel casting forming
Into non-water base foamy carbon precursor pulp, initiator is added, the quality of initiator is non-water base foamy carbon forerunner
The 0.5wt% of body stock quality, stirring 10min (stirring is just completely dissolved to initiator), are injected into mold, immediately with 1L
The ratio of the catalyst of 10mL is added in non-water base foamy carbon precursor pulp, instills catalyst, and the low speed of 8 turns/min continuously stirs
5min is mixed, until solution solidifies, to form wet base；
The initiator is the mixture of benzoyl peroxide and n,N-Dimethylaniline, is in mass ratio benzoyl peroxide
Formyl: N, accelerine=1:1.
The catalyst be N, the mixture of N-dimethylaniline and isopropyl benzene hydroperoxide, in mass ratio, N, N-
Dimethylaniline: isopropyl benzene hydroperoxide=1:1；
Step 4. body drying
Wet base is dried into 25h (drying to wet base is no longer shunk) together with mold at 50 DEG C jointly, obtains biscuit；
The pre-oxidation of step 5. biscuit
By biscuit obtained in above-mentioned steps in air atmosphere, it is placed in 210 DEG C of pre-oxidation 4h, the element after being pre-oxidized
Base；
Step 6. atmosphere sintering
By the biscuit after pre-oxidizing obtained in above-mentioned steps, 1200 DEG C of carbonization 2h in inert atmosphere (argon gas) are cooling
Foamy carbon is obtained to room temperature.
Analysis test, intensity 10MPa are carried out to foamy carbon manufactured in the present embodiment, specific compress strength is
22.4MPacm3/g。
Claims (10)
1. a kind of method that non-water-base gel casting prepares foamy carbon, which comprises the following steps:
Step 1: allotment monomer premixed liquid
According to the ratio, organic monomer and crosslinking agent are mixed, is dissolved in alcohols organic solution, obtains monomer premixed liquid；Wherein, it presses
Mass ratio, organic monomer: crosslinking agent=(3~20): 1, in monomer premixed liquid, the mass concentration of organic monomer is 19~21%；
Step 2: preparing non-water base foamy carbon precursor pulp
Carbon-based presoma, pore creating material are added in monomer premixed liquid, ball milling mixing is uniform, obtains non-water base foamy carbon forerunner somaplasm
Material；Wherein, the percent by volume of solid phase is 50~65Vol.% in non-water base foamy carbon precursor pulp；By volume, pore-creating
Agent: carbon-based presoma=(30~80): 30；
Step 3: gel casting forming
Into non-water base foamy carbon precursor pulp, initiator is added, stirring to initiator is dissolved, and initiator then will be added
In non-water base foamy carbon precursor pulp injection mold, catalyst is added dropwise, continuously stirs, until non-water base foamy carbon forerunner somaplasm
Material solidification, obtains wet base；Wherein, the addition quality of initiator be non-water base foamy carbon precursor pulp gross mass 0.4~
0.6wt.%；By volume, catalyst: non-water base foamy carbon precursor pulp=10~20mL:1L；
Step 4: body drying
By wet base in 40~50 DEG C of dryings, drying is no longer shunk to wet base, obtains biscuit；
Step 5: biscuit pre-oxidation
By biscuit in air atmosphere, 4~6h, the biscuit after being pre-oxidized are pre-oxidized at 190~210 DEG C；
Step 6: atmosphere sintering
Under an inert atmosphere by the biscuit after pre-oxidation, it in 900~1200 DEG C of 2~4h of carbonization, is cooled to room temperature, obtains foam
Carbon.
2. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that the step
In rapid 1, the organic monomer be 1 acrylamide functionality acrylamides, and/or 1 acrylate official
The acrylic ester compound that can be rolled into a ball.
3. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that the step
In rapid 1, the crosslinking agent is the acrylamides, and/or at least two propylene of at least two acrylamide functionality
The acrylic ester compound of acid ester functionality.
4. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that the step
In rapid 1, the alcohols organic solution is ethyl alcohol, methanol, propyl alcohol, ethylene glycol, propylene glycol, n-butanol at least one or several
Mixing.
5. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that the step
In rapid 2, the carbon-based presoma is the mixing of one or more of sucrose, pitch, coal, organic polymer；Described makes
Hole agent is microcapsules or glass microballoon.
6. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that the step
In rapid 2, the ball milling, rotational speed of ball-mill is 1500~2000 turns/min, and Ball-milling Time is 30min~2h.
7. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that the step
In rapid 3, the initiator is ammonium persulfate, benzoyl peroxide, mixing one or several kinds of in n,N-Dimethylaniline；
The catalyst is N, N, N`, N`-tetramethylethylenediamine, N, one in N-dimethylaniline, isopropyl benzene hydroperoxide
Kind or several mixing.
8. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that the step
In rapid 3, the time of initiator dissolution is 5~10min；Described continuously stirs, and uses speed of agitator for 5~10 turns/min.
9. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that the step
In rapid 3, the solidification, curing time is 2~10min.
10. the method that non-water-base gel casting as described in claim 1 prepares foamy carbon, which is characterized in that described
In step 4, the drying, drying time is 40~60h.
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Application publication date: 20190503 |