CN102616767A - Foam carbon composite material and preparation method thereof - Google Patents
Foam carbon composite material and preparation method thereof Download PDFInfo
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- CN102616767A CN102616767A CN2012100846529A CN201210084652A CN102616767A CN 102616767 A CN102616767 A CN 102616767A CN 2012100846529 A CN2012100846529 A CN 2012100846529A CN 201210084652 A CN201210084652 A CN 201210084652A CN 102616767 A CN102616767 A CN 102616767A
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Abstract
The invention discloses a foam carbon composite material and a preparation method thereof, which belong to the field of carbon materials and relate to preparation technology for easily forming high-strength foam carbon composite materials. Thermosetting resin and nanometer reinforcing materials are used as raw materials, and the foam carbon composite material is prepared by means of processes of compounding, pre-polymerization, casting molding, curing and carbonization. The foam carbon composite material is high in strength, excellent in thermal protection performance, simple in process and low in preparation cost and equipment investment, and has remarkable economical and social benefits, the sizes of foams are uniform, additional foaming agent is omitted, and complicated molding of the foam carbon composite material can be realized at one step.
Description
Technical field
The invention belongs to raw material of wood-charcoal material field, relate to a kind of technology of preparing of easy-formation HS Carbon foam matrix material, be specifically related to a kind of Carbon foam matrix material and preparation method thereof.
Background technology
Carbon foam is a kind of light porous material of being made up of hole bubble and interconnective hole wall with tridimensional network; Except traditional performance with raw material of wood-charcoal material; Characteristics such as have also that porosity height, specific surface area are big, thermostability and shock absorption are good, high temperature resistant, corrosion-resistant, these characteristics make Carbon foam satisfy the requirement as structure-function integration material basically.Carbon foam is widely used at numerous areas such as Aeronautics and Astronautics, chemical industry, electronics at present, as can be used as high-performance insulation material, thermally conductive material, cushioning material, the body material of lightweight high precision space storehouse emission mirror and the filtering material of metal or gas etc.Especially, the rise of researchs such as biofuel cell electrode materials, the solid bacterium solid support material of biological bacteria, water treatment porous material has been injected new vitality for Carbon foam in the application in fields such as the energy, environmental protection, catalysis again in the recent period.Yet a significant disadvantage of foam carbon material is a poor mechanical property, when practical application, has great potential safety hazard.In addition, prepare in Carbon foam and also to have complex process, cost height, operational hazards in the process, be difficult to problems such as once complicated moulding, this has greatly restricted further developing and using of its.
Summary of the invention
The object of the present invention is to provide a kind of Carbon foam matrix material and preparation method thereof; Carbon foam composite material strength that the present invention makes is high, hole bubble size is even, heat-proof quality is excellent, and technology is simple, can once complicated moulding, production process safety, lower to equipment requirements.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
The mixing of the outfit, raw material that a kind of preparation method of Carbon foam matrix material comprises raw material and strongthener, pre-polymerization, casting, curing and charring process;
(1) outfit of raw material
Matrix material: one or several mixtures of bisphenol A cyanate ester, NSC 7352 bisphenol type cyanate, polyfunctional group cyanate, tetramethyl-Bisphenol F type cyanate, bis-phenol M type cyanate, Bisphenol F type cyanate, bisphenol E-type cyanate, bisphenol A cyanate ester performed polymer;
Strongthener: hydroxylation CNT, acidifying CNT, graphene oxide, organo montmorillonite, mesoporous silicon oxide, nano silicon a kind of;
Proportionlity between matrix material, the strongthener is: matrix material: 90-99.9wt%; Strongthener 0.1-10wt%;
(2) raw material and strongthener mixes
The raw material that above-mentioned outfit is good carries out ultra-sonic dispersion in solvent, concrete processing parameter is following:
Solvent: methylene dichloride, ethanol, acetone, N, dinethylformamide a kind of;
Temperature: 25-100 ℃;
Time: 0.1-2h;
Ultrasonic power: 100-600 W;
(3) solvent removes
The above-mentioned mixed solution for preparing packed into carry out desolventizing in the vacuum distillation apparatus, concrete parameter is following:
Temperature: 60-200 ℃;
Time: 0.1-2 h;
Vacuum tightness: 1.0 * 10
-1-1.0 * 10
5Pa;
Stirring velocity: 50-1000 rpm;
(4) pre-polymerization of raw mix
The above-mentioned mixture of sloughing solvent is moved in the reactor drum, carry out pre-polymerization, concrete parameter is following:
Temperature: 100-200 ℃;
Time: 0.1-4 h;
Protective atmosphere: N
2Perhaps Ar;
Gas flow: 50-200 ml/min;
Stirring velocity: 50-1000 rpm;
(5) casting
Above-mentioned prepolymer is poured in the mould of preheating, de-bubbled, concrete parameter is following:
Temperature: 200 ℃ of 100 –;
The de-bubbled time: 0.1 –, 5 h;
Vacuum tightness: 1.0 * 10
-1– 1.0 * 10
5Pa;
(6) solidify
Prepolymer is cured behind casting, and concrete parameter is following:
Solidification value: 300 ℃ of 100 –;
Set time: 1 –, 10 h;
Vacuum tightness: 1.0 * 10
-1– 1.0 * 10
5Pa;
(7) charring process
Matrix material after the curing is put into atmosphere furnace through after the demoulding, keeps for some time after being warming up to preset temperature with certain temperature rise rate then, cools to room temperature with the furnace and takes out, and processing parameter is:
Temperature rise rate: 50 ℃/min of 2 –;
Preset temperature: 1500 ℃ of 600 –;
Soaking time: 0.5 –, 10 h;
Protective atmosphere: N
2Perhaps Ar;
Gas flow: 50 –, 200 ml/min.
Polyreaction in the said step 4) or employing freely are warming up to 60-80 ℃ with temperature elder generation, and the temperature rise rate with 5-10 ℃/min is warming up to described 100-200 ℃ afterwards.
Curing schedule in the said step 6) or adopt staged to solidify, promptly 100-160 ℃/1-2h → 160-180 ℃/1-2h → 180-220 ℃/2h → 220-300 ℃/1-2h, temperature rise rate is 10 ℃/min.
Remarkable advantage of the present invention is: the present invention reaches the structure and the performance of the Carbon foam matrix material of adjustment through control matrix material, both ratios of strongthener, curing process and charring process.Adopt the obtained Carbon foam matrix material of preparation method of the present invention to have good mechanical performance and heat-proof quality, compressive strength 10 – 40MPa, density 0.2 – 0.8g/cm
3, thermal conductivity 0.05 – 5W/mk.Compared with prior art, advantage that the present invention had and effect are: product mechanical property and heat-proof quality are excellent; Technology is simple, need not to add whipping agent, can once complicated moulding; Low, the less equipment investment of preparation cost, simple to operate.
Embodiment
Below be several specific embodiment of the present invention, further specify the present invention, but the present invention be not limited only to this.
Embodiment 1
Bisphenol A cyanate ester and hydroxylation CNT are taken by weighing by 98:2 (weight ratio), add an amount of methylene dichloride and pack into after through 300W supersound process 1h in the vacuum distillation apparatus, under 60 ℃ and rotating speed 300rpm stir, be distilled to no bubble and emerge; The polymerization container of packing into then; Rotating speed 300rpm stirs 1h, then begins to heat up, and freely heats up before 60 ℃; Speed with 10 ℃/min after 60 ℃ heats up, and begins to feed N from intensification
2, N
2Flow is 50mL/min.Continued stirs 0.5h with rotating speed 500rpm and obtains prepolymer when temperature rises to 130 ℃, pours vacuumize degassing bubble 0.5h (vacuum tightness 1.0 * 10 in the mould (100 ℃) then into
-1Pa), be cured by following technology then: 160 ℃/2h+180 ℃/2h+200 ℃/2h+260 ℃/6h, the matrix material after solidifying is put into N
2In the special atmosphere oven, 3 ℃/min temperature rise rate keeps 2h after being warming up to 1000 ℃ of temperature then, cools to room temperature with the furnace and takes out, and promptly obtains the Carbon foam matrix material.Prepared Carbon foam matrix material has following performance: compressive strength 18.3MPa, density 0.362g/cm
3, thermal conductivity 1.28W/mk.
Embodiment 2
Bisphenol A cyanate ester, bisphenol E-type cyanate, mesoporous silicon oxide are taken by weighing by 60:30:10 (weight ratio), add an amount of N, in the vacuum distillation apparatus of packing into behind the dinethylformamide process 100W supersound process 2h; Under 60 ℃ and rotating speed 200rpm stir, be distilled to no bubble and emerge, the polymerization container of packing into then, rotating speed 300rpm stirs 1h; Then begin to heat up; Freely heated up before 70 ℃, the speed with 5 ℃/min after 70 ℃ heats up, and begins to feed N from intensification
2, N
2Flow is 100mL/min.Continued stirs 0.5h with rotating speed 500rpm and obtains prepolymer when temperature rises to 130 ℃, pours vacuumize degassing bubble 0.5h (vacuum tightness 1.0 * 10 in the mould (160 ℃) then into
3Pa), be cured by following technology then: 160 ℃/2h+180 ℃/2h+200 ℃/2+300 ℃/5h, the matrix material after solidifying is put into Ar
2In the special atmosphere oven, 5 ℃/min temperature rise rate keeps 10h after being warming up to 1400 ℃ of temperature then, cools to room temperature with the furnace and takes out, and promptly obtains the Carbon foam matrix material.Prepared Carbon foam nano composite material has following performance: compressive strength 33.2MPa, density 0.792g/cm
3, thermal conductivity 0.08W/mk.
Embodiment 3
Polyfunctional group cyanate, acidifying CNT are taken by weighing by 96:4 (weight ratio), add adequate amount of ethanol and pack into after through 150W supersound process 2h in the vacuum distillation apparatus, under 100 ℃ and rotating speed 200rpm stir, be distilled to no bubble and emerge; The polymerization container of packing into then; Rotating speed 300rpm stirs 1h, then begins to heat up, and freely heats up before 80 ℃; Speed with 5 ℃/min after 80 ℃ heats up, and begins to feed N from intensification
2, N
2Flow is 150mL/min.Continued stirs 60min with rotating speed 500rpm and obtains prepolymer when temperature rises to 130 ℃, pours vacuumize degassing bubble 0.5h (vacuum tightness 1.0 * 10 in the mould (150 ℃) then into
2Pa), be cured by following technology then: 160 ℃/2h+180 ℃/2h+220 ℃/2h+260 ℃/6h, the matrix material after solidifying is put into N
2In the special atmosphere oven, 25 ℃/min temperature rise rate keeps 2h after being warming up to 1250 ℃ of temperature then, cools to room temperature with the furnace and takes out, and promptly obtains foam carbon material.Prepared Carbon foam matrix material has following performance: compressive strength 22.1MPa, density 0.511g/cm
3, thermal conductivity 0.72W/mk.
Embodiment 4
Tetramethyl-Bisphenol F type cyanate, bis-phenol M type cyanate, Bisphenol F type cyanate, graphene oxide are taken by weighing by 42:40:16:2 (weight ratio); Add an amount of N; Dinethylformamide is packed into after through 600W supersound process 0.5h in the vacuum distillation apparatus, under 80 ℃ and rotating speed 50rpm stir, is distilled to no bubble and emerges, then with this mixture polymerization container of packing into; Speed with 10 ℃/min heats up, and begins to feed N from intensification
2, N
2Flow is 100mL/min, and accompanies by the 300rpm stirring.Continued stirs 0.5h with rotating speed 200rpm and obtains prepolymer when temperature rises to 130 ℃, pours vacuumize degassing bubble 0.5h (vacuum tightness 1.0 * 10 in the mould (170 ℃) then into
-1Pa), be cured by following technology then: 160 ℃/2h+180 ℃/2h+200 ℃/2h+250 ℃/5h, the matrix material after solidifying is put into Ar
2In the special atmosphere oven, 10 ℃/min temperature rise rate keeps 5h after being warming up to 1500 ℃ of temperature then, cools to room temperature with the furnace and takes out, and promptly obtains the Carbon foam matrix material.Prepared Carbon foam matrix material has following performance: compressive strength 37.2MPa, density 0.63g/cm
3, thermal conductivity 1.93W/mk.
Embodiment 5
Bisphenol A cyanate ester performed polymer and nano silicon are taken by weighing by 95:5 (weight ratio), add an amount of acetone and pack into after through 200W supersound process 0.5h in the vacuum distillation apparatus, under 120 ℃ and rotating speed 50rpm stir, be distilled to no bubble and emerge; The polymerization container of packing into then; Rotating speed 200rpm stirs 1h, begins to heat up, and freely heats up before 60 ℃; Speed with 5 ℃/min after 60 ℃ heats up, and begins to feed N from intensification
2, N
2Flow is 50mL/min.Continued stirs 0.8h with rotating speed 300rpm and obtains prepolymer when temperature rises to 130 ℃, pours vacuumize degassing bubble 0.5h (vacuum tightness 1.0 * 10 in the mould (150 ℃) then into
5Pa), be cured by following technology then: 160 ℃/2h+180 ℃/2h+220 ℃/2h+260 ℃/4h, the matrix material after solidifying is put into Ar
2In the special atmosphere oven, 50 ℃/min temperature rise rate keeps 4h after being warming up to 1300 ℃ of temperature then, cools to room temperature with the furnace and takes out, and promptly obtains the Carbon foam matrix material.Prepared Carbon foam matrix material has following performance: compressive strength 28.6MPa, density 0.48g/cm
3, thermal conductivity 0.24W/mk.
Embodiment 6
Bisphenol A cyanate ester performed polymer, bisphenol E-type cyanate and organo montmorillonite are taken by weighing by 55:44:1 (weight ratio), add an amount of N, in the vacuum distillation apparatus of packing into behind the dinethylformamide process 600W supersound process 0.1h; Under 140 ℃ and rotating speed 500rpm stir, be distilled to no bubble and emerge, the polymerization container of packing into then, rotating speed 1000rpm stirs 1h; Begin to heat up; Freely heated up before 80 ℃, the speed with 10 ℃/min after 80 ℃ heats up, and begins to feed N from intensification
2, N
2Flow is 50mL/min.Continued stirs 1h with rotating speed 500rpm and obtains prepolymer when temperature rises to 130 ℃, pours vacuumize degassing bubble 0.5h (vacuum tightness 1.0 * 10 in the mould (150 ℃) then into
3Pa), be cured by following technology then: 160 ℃/2h+180 ℃/2h+220 ℃/2h+260 ℃/4h, the matrix material after solidifying is put into Ar
2In the special atmosphere oven, 25 ℃/min temperature rise rate keeps 1h after being warming up to 1500 ℃ of temperature then, cools to room temperature with the furnace and takes out, and promptly obtains the Carbon foam matrix material.Prepared Carbon foam matrix material has following performance: compressive strength 35.1MPa, density 0.64g/cm
3, thermal conductivity 0.17W/mk.
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. the preparation method of a Carbon foam matrix material is characterized in that: the mixing of the outfit, raw material that described preparation method comprises raw material and strongthener, pre-polymerization, casting, curing and charring process;
(1) outfit of raw material
Matrix material: one or several mixtures of bisphenol A cyanate ester, NSC 7352 bisphenol type cyanate, polyfunctional group cyanate, tetramethyl-Bisphenol F type cyanate, bis-phenol M type cyanate, Bisphenol F type cyanate, bisphenol E-type cyanate, bisphenol A cyanate ester performed polymer;
Strongthener: hydroxylation CNT, acidifying CNT, graphene oxide, organo montmorillonite, mesoporous silicon oxide, nano silicon a kind of;
Proportionlity between matrix material, the strongthener is: matrix material: 90-99.9wt%; Strongthener 0.1-10wt%;
(2) raw material and strongthener mixes
The raw material that above-mentioned outfit is good carries out ultra-sonic dispersion in solvent, concrete processing parameter is following:
Solvent: methylene dichloride, ethanol, acetone, N, dinethylformamide a kind of;
Temperature: 25-100 ℃;
Time: 0.1-2h;
Ultrasonic power: 100-600 W;
(3) solvent removes
The above-mentioned mixed solution for preparing packed into carry out desolventizing in the vacuum distillation apparatus, concrete parameter is following:
Temperature: 60-200 ℃;
Time: 0.1-2 h;
Vacuum tightness: 1.0 * 10
-1-1.0 * 10
5Pa;
Stirring velocity: 50-1000 rpm;
(4) pre-polymerization of raw mix
The above-mentioned mixture of sloughing solvent is moved in the reactor drum, carry out pre-polymerization, concrete parameter is following:
Temperature: 100-200 ℃;
Time: 0.1-4 h;
Protective atmosphere: N
2Perhaps Ar;
Gas flow: 50-200 ml/min;
Stirring velocity: 50-1000 rpm;
(5) casting
Above-mentioned prepolymer is poured in the mould of preheating, de-bubbled, concrete parameter is following:
Temperature: 200 ℃ of 100 –;
The de-bubbled time: 0.1 –, 5 h;
Vacuum tightness: 1.0 * 10
-1– 1.0 * 10
5Pa;
(6) solidify
Prepolymer is cured behind casting, and concrete parameter is following:
Solidification value: 300 ℃ of 100 –;
Set time: 1 –, 10 h;
Vacuum tightness: 1.0 * 10
-1– 1.0 * 10
5Pa;
(7) charring process
Matrix material after the curing is put into atmosphere furnace through after the demoulding, keeps for some time after being warming up to preset temperature with certain temperature rise rate then, cools to room temperature with the furnace and takes out, and processing parameter is:
Temperature rise rate: 50 ℃/min of 2 –;
Preset temperature: 1500 ℃ of 600 –;
Soaking time: 0.5 –, 10 h;
Protective atmosphere: N
2Perhaps Ar;
Gas flow: 50 –, 200 ml/min.
2. the preparation method of Carbon foam matrix material according to claim 1; It is characterized in that: polyreaction in the said step 4) or employing freely are warming up to 60-80 ℃ with temperature elder generation, and the temperature rise rate with 5-10 ℃/min is warming up to described 100-200 ℃ afterwards.
3. the preparation method of Carbon foam matrix material according to claim 1; It is characterized in that: curing schedule in the said step 6) or employing staged are solidified; Be 100-160 ℃/1-2h → 160-180 ℃/1-2h → 180-220 ℃/2h → 220-300 ℃/1-2h, temperature rise rate is 10 ℃/min.
4. Carbon foam matrix material that preparation method as claimed in claim 1 obtains.
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| CN2012100846529A CN102616767A (en) | 2012-03-28 | 2012-03-28 | Foam carbon composite material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898118A (en) * | 2012-10-25 | 2013-01-30 | 中国地质大学（北京） | Coal ash reinforced foam carbon material and preparation method thereof |
| CN103058168A (en) * | 2012-12-27 | 2013-04-24 | 中国科学院广州地球化学研究所 | Preparation method for nano-carbon material having graphene-like structure |
| CN104909815A (en) * | 2015-06-04 | 2015-09-16 | 合肥和安机械制造有限公司 | Composite modified light-burned magnesium oxide-carbonized foamed phenolic resin-base heat insulating material for fork truck engine exhaust pipes and preparation method thereof |
| CN104926305A (en) * | 2015-06-04 | 2015-09-23 | 合肥和安机械制造有限公司 | Compound modified montmorillonite-carbonized foam phenolic resin based thermal insulation material for forklift engine exhaust pipe, and preparation method of thermal insulation material |
| CN105271177A (en) * | 2015-11-18 | 2016-01-27 | 福州大学 | Preparation method of graphene multilayer foam carbon material |
| CN104036973B (en) * | 2014-06-24 | 2016-08-17 | 福州大学 | A kind of ultracapacitor rich nitrogen Carbon foam electrode material and preparation method thereof |
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| CN104036973B (en) * | 2014-06-24 | 2016-08-17 | 福州大学 | A kind of ultracapacitor rich nitrogen Carbon foam electrode material and preparation method thereof |
| CN104909815A (en) * | 2015-06-04 | 2015-09-16 | 合肥和安机械制造有限公司 | Composite modified light-burned magnesium oxide-carbonized foamed phenolic resin-base heat insulating material for fork truck engine exhaust pipes and preparation method thereof |
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| CN105271177A (en) * | 2015-11-18 | 2016-01-27 | 福州大学 | Preparation method of graphene multilayer foam carbon material |
| CN105271177B (en) * | 2015-11-18 | 2017-10-20 | 福州大学 | A kind of preparation method of the multi-level foam carbon material of graphite alkylene |
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Application publication date: 20120801 |