CN106589791A - High-temperature ceramizable phenolic foam composite material and preparation method thereof - Google Patents
High-temperature ceramizable phenolic foam composite material and preparation method thereof Download PDFInfo
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- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
Abstract
The invention provides a high-temperature ceramizable phenolic foam composite material. The material is mainly prepared from, by mass, 100 parts of expandable phenolic resin, 5-10 parts of a foaming agent, 6-10 parts of a surfactant, 10-12 parts of a curing agent, 90-130 parts of high-temperature ceramizable composite inorganic filler and 2.5-4 parts of a silane coupling agent. A preparation method includes: weighing a certain quantity of the phenolic resin, proportionally adding the high-temperature ceramizable composite inorganic filler and the silane coupling agent, and using a stirrer for mixing completely; adding the surfactant, the foaming agent and the curing agent, fast stirring uniformly, injecting into a mould, and putting in a constant-temperature chamber for 150min+/-10min at 75+/-5 DEG C; cooling to the room temperature after curing molding, and demolding. The composite material is low in heat conductivity coefficient (smaller than or equal to W/(m.K) and high in compression strength, wherein normal-temperature compression strength is larger than or equal to 0.15MPa, and compression strength is larger than or equal to 0.1MPa after high-temperature treatment. In addition, appearance, performances and micro porous structures of the material can be kept under high-temperature aerobic conditions.
Description
Technical field
The present invention relates to polymer matrix foam composite technology field, and in particular to a kind of high temperature can ceramic phenolic aldehyde bubble
Foam composite and preparation method thereof, can be applicable to the field such as insulation, heat-insulated, fire prevention.
Background technology
Phenolic foam composite material has the excellent properties such as good fire retardant, low cigarette, low toxicity, heat-resisting, insulation, sound insulation, and
With very wide use temperature range (- 196 DEG C～+150 DEG C), in the fields such as Aero-Space, national defence, ship, building, chemical industry
Be widely used, be such as used as heat insulation tile of shuttle, rocket ablator, submarine thermal and sound insulating materials, civil aircraft bulkhead,
Architecture exterior wall insulating materials, the insulation of central air conditioner system airduct etc..The use temperature of phenolic foam composite material is better than polyphenyl second
Alkene (80 DEG C) and polyurethane (110 DEG C), but with (typically more than 650 DEG C) traditional inorganic guarantor such as mineral wool, perlite and glass cotton
Adiabator compares that gap is larger, so the still tradition of, heat insulation effect difference high using heat conductivity in a large number under the high temperature conditions at present
Inorganic heat insulation material, its heat conductivity is typically in more than 0.1W/ (mK).Therefore organic insulation material heat conductivity is being kept
On the premise of low, heat-insulating property is good, how to improve its resistance to elevated temperatures becomes an important topic.
In order to further improve the thermostability of phenolic foam composite material, researcher by it is modified to phenolic resin as matrix resin with
And be modified by introducing various fillers.Huang Jianqing et al. has synthesized foamable boron bakelite resin and has made by adding boric acid
For boron modification phenol formaldehyde foam, resistance to elevated temperatures is improved, and heat decomposition temperature is 450 DEG C, and the highest of boron modification phenol formaldehyde foam is used
Temperature be 200 DEG C (Huang Jianqing, Pan Anjian. the resistance to elevated temperatures of boron modification phenol formaldehyde foam. fiberglass/composite, 2007,6:
26-28.).Wang Bin et al. is by B2O3Phenol formaldehyde foam is introduced, the heat decomposition temperature and carbon yield of prepared modified phenolic foam are carried
Height, works as B2O3When content is mass fraction 7%, the resistance to elevated temperatures of phenol formaldehyde foam is optimum, in nitrogen atmosphere its weightless 10% when
Heat decomposition temperature be 447 DEG C (Wang Bin, Li Hejun, Zhang Yulei, Li Yunyu, Liu Zhangqing. boron modification phenolic foam composite material
Preparing and performance study. Chinese material is in progress, and 2013,32 (11)：641-646.).He Bin et al. is by adding Nano-meter SiO_22Carry
High phenol formaldehyde foam thermostability (He Bin, Yang Zhenguo. Nano-meter SiO_22The preparation of modified phenolic foam and sign. petrochemical industry,
2007,36 (12), 1266-1270.)；Improved using montmorillonite, carbon fiber composite modified phenolic aldehyde foam insulation material in position east et al.
Heat-resisting and mechanical property (position east, Li Dongfeng, Zhang Lu, Zhao Zhankui, Ao Yuhui. montmorillonite, carbon fiber composite modified phenolic aldehyde foam are protected
The research of adiabator. Chinese material seminar, 2011,5.17-5.20, Beijing National conference centre).
Can ceramic polymer matrix composite by polymeric matrix and high temperature can the inorganic filler of ceramic constitute, can make pottery
Porcelain fluidized polymer based composites have at normal temperatures the performance similar with general polymer based composites, and send out at high temperature
The processes such as raw cracking, melting, high-temperature phase-change are converted into ceramic phase or glass phase protective layer, with certain intensity and can bear one
Fixed impulsive force, it is of great interest in fire-retardant, fire prevention, thermal protection field.L.G.Hanu, J.MANSOURI and Y.B.Cheng
(L.G.Hanu,G.P.Simon,J.Mansouri,R.P.Burford,Y.B.Cheng.Development of polymer–
ceramic composites for improved fire resistance.Journal of Material
Processing Technology,2004,153–154:401-407.) the ceramic packing systems such as Muscovitum etc. are added in silicones
Standby high temperature can ceramic composite, in 1050 DEG C or so of hot-air there is eutectic reaction in composite cracking process
Mullite ceramic phase structure is formed, so as to improve high-temperature residual amount and pyrogenous residue intensity, having started can ceramic fluidized polymer
The beginning that based composites are studied and applied.In recent years, domestic and international polymer matrix composite can porcelainization research be concentrated mainly on
Silicone and silicone rubber art.
This research group be devoted to carbon-based resin composite can ceramic research and apply, ZL 201210145780X
Disclose one kind can Carbon-based polymer composite material capable of being ceramized and preparation method thereof, paper (Chih-hsiung Huang, fourth of Chih-hsiung Huang et al.
Outstanding person, Shi Minxian, Liu Tianxiang .ZrSi2The preparation of/boron phenolic foam and its mechanism and enhancement mechanism of pyrolysis product. composite journal,
2015 Network Priorities are published, DOI:10.13801/j.cnki.fhclxb.20151218.002.) disclose ZrSi2/ boron phenolic
The preparation of foam and its performance.
From document report analysis, phenolic foam composite material has good heat resistance, can make below 200 DEG C
With, but at higher temperatures, oxidation, cracking, weightless, structure and performance are serious the problems such as destruction.Can porcelain polymer matrix
Composite can be changed under the high temperature conditions inorganic ceramic material or glass ceramic material, be resistant to more than 1000 DEG C
High temperature, and can keep the structure and performance of composite, has certain research and should in fireproof cable, thermally protective materials field
With.The present invention propose a kind of high temperature can ceramic phenolic foam composite material and preparation method thereof, high temperature can ceramic phenolic aldehyde
The successful preparation of foamed composite and application, have extremely for the hot spot of societys such as energy-conserving and environment-protective, back-fire relief be heat-insulated are solved
Major and immediate significance, while also having particularly important economy and society meaning.
The content of the invention
Present invention solves the technical problem that being：There is provided a kind of high temperature can ceramic phenolic foam composite material and its preparation side
Method, the composite has relatively low heat conductivity, higher compressive strength in room temperature, and issues in high temperature aerobic conditions
The processes such as raw oxidation, cracking, ceramic transformation, ultimately form the ceramic phase or glass phase structure of porous, and can keep initial
Profile, performance and microcosmic loose structure.Traditional organic foam composite is solved in high-temp combustion or oxidizing condition high temperature resistant
The not enough difficult problem of performance.
The present invention solves its technical problem and adopts following technical scheme：
The present invention provide high temperature can ceramic phenolic foam composite material, be mainly made up of following raw material：Expandability
100 parts of phenolic resin, foaming agent 5-10 parts, surfactant 6-10 parts, firming agent 10-12 parts, high temperature can ceramic it is compound
Inorganic filler 90-130 parts, silane coupler 2.5-4 parts, are mass parts.
Described high temperature can ceramic compound inorganic stuffing by inorganic ceramic raw material, low melting point flux, high temperature pore
Agent, high-temperature expansion agent are constituted, and part by weight shared by each component is：Inorganic ceramic raw material 65%, low melting point flux 15%, high temperature
Porogen 15%, high-temperature expansion agent 5%.
Described inorganic ceramic raw material, is the one kind in Muscovitum, Pulvis Talci, Kaolin, montmorillonite, wollastonite, or two kinds
The mixture of any of the above ratio, its size is 1-35 μm.
Described low melting point flux is the frit of low softening temperature, and its softening range is 380-620 DEG C, mainly
Composition is SiO2、ZnO、B2O3、Na2O、CaO、K2O, its component participates in the ceramic transformation of inorganic ceramic raw material during high temperature.
Described high temperature porogen is one or more in aluminium hydroxide, limestone, dolomite, what pyrolytic was produced
Gas plays pore effect, decomposes the ceramic transformation that the inorganic oxide for producing participates in inorganic ceramic raw material.
Described high-temperature expansion agent be vermiculite power, crushed crude pearlite one or two.
The high temperature that the present invention is provided can ceramic phenolic foam composite material, its preparation method comprises the following steps：
(1) expandable phenolic resin is weighed；
(2) in the phenolic resin obtained by step (1), add by a certain percentage high temperature can the composite inorganic of ceramic fill out
Material, and be sufficiently mixed uniformly with agitator, obtain mixed liquor；
(3) surfactant, foaming agent and firming agent are added in the mixed liquor obtained by step (2), quick stirring is equal
It is even, obtain mixture；
(4) by the mixture injection mould obtained by step (3), it is placed in 150min in 75 DEG C ± 5 DEG C of calorstat
± 10min, obtains sample after curing molding；
(5) sample is cooled to into room temperature, the demoulding, obtaining described high temperature can ceramic phenolic foam composite material.
In said method, described phenolic resin is resol, and solid content is 75-80%.
In said method, described foaming agent is physical blowing agent, specially pentane；Described surfactant is to tell
Temperature -80；Described firming agent is p-methyl benzenesulfonic acid, and described silane coupler is KH-550.
In said method, resulting high temperature can ceramic phenolic foam composite material, its main performance index is：Room temperature
Comprcssive strength >=0.15MPa, comprcssive strength >=0.1MPa after high-temperature process, heat conductivity≤0.07W/ (mK).
The present invention due to add high temperature can ceramic compound inorganic stuffing, prepared foam densities are than existing
The density of phenol formaldehyde foam is big, but has the advantages that compared with existing phenolic foam composite material following main：
(1) high temperature can the addition of compound inorganic stuffing of ceramic phenolic foam material can be turned under the high temperature conditions
It is changed into ceramic phase or glass phase porous material, heat resistance is improved so that phenolic foam composite material is resistant to higher temperature
Degree and longer time.
(2) high temperature can ceramic phenolic foam composite material resistance to elevated temperatures significantly improve, but still lead with relatively low
Hot coefficient, heat conductivity≤0.07W/ (mK).
(3) under high temperature aerobic conditions, the high temperature can the experience oxidation of ceramic phenolic foam composite material, cracking, ceramic
The processes such as transformation, ultimately form ceramic phase or glass phase structure, and macro geometry and microcosmic loose structure are still kept substantially.
(4) with high intensity：Normal temperature compressed intensity >=0.15MPa, compressive strength >=0.1MPa after high-temperature process.
Description of the drawings
Fig. 1 is that high temperature can ceramic phenolic foam composite material cross-sectional scanning electron microphotograph at normal temperatures.
Fig. 2 is that high temperature can cross-sectional scanning electron microscope photograph of the ceramic phenolic foam composite material after 900 DEG C of process
Piece.
Specific embodiment
The present invention adopts expandability phenolic aldehyde for resin matrix, foaming agent, firming agent, surfactant, silane coupler etc.
For auxiliary agent, high temperature can ceramic composite inorganic component be filler, foamed according to certain foam process, ultimately provide
A kind of high temperature can porcelain phenolic foam composite material and preparation method thereof.Under burning or high temperature aerobic conditions, the high temperature can ceramics
Change the processes such as phenolic foam composite material experience oxidation, cracking, ceramic transformation, ultimately form ceramic phase or glass phase structure,
Still macro geometry and microcosmic loose structure are kept substantially.
With reference to embodiment and accompanying drawing, the invention will be further described, but is not limited solely to the following examples.
Embodiment 1
A kind of high temperature can ceramic phenolic foam composite material, consisting of：100 parts of expandable phenolic resin, foaming agent 5
Part, 6 parts of surfactant, 10 parts of firming agent, high temperature can ceramic 90 parts of compound inorganic stuffing (wherein containing Muscovitum 58.5
Part, 13.5 parts of frit, 13.5 parts of aluminium hydroxide, 4.5 parts of vermiculite power), 2.5 parts of silane coupler is mass parts.
Embodiment 2
A kind of high temperature can ceramic phenolic foam composite material, consisting of：100 parts of expandable phenolic resin, foaming agent
10 parts, 10 parts of surfactant, 12 parts of firming agent, high temperature can 130 parts of the compound inorganic stuffing of ceramic (wherein contain Kaolin
84.5 parts, 19.5 parts of frit, 19.5 parts of limestone, 6.5 parts of crushed crude pearlite), 4 parts of silane coupler is mass parts.
Embodiment 3
A kind of high temperature can ceramic phenolic foam composite material, consisting of：100 parts of expandable phenolic resin, foaming agent 8
Part, 8 parts of surfactant, 11 parts of firming agent, high temperature can 110 parts of the compound inorganic stuffing of ceramic (wherein contain wollastonite in powder
71.5 parts, frit 16.5,16.5 parts of dolomite, 5.5 parts of vermiculite power), 3 parts of silane coupler is mass parts.
Embodiment 4
A kind of high temperature can ceramic phenolic foam composite material, be in accordance with the following methods and step preparation method prepare
's：
(1) phenolic resin of 100g is weighed；
(2) in the phenolic resin obtained by step (1), add 120g high temperature can ceramic compound inorganic stuffing
(wherein containing mica powder 78g, frit 18g, aluminium hydroxide 18g, vermiculite power 6g), 3.5 parts of silane coupler, and use agitator
It is sufficiently mixed uniformly, is obtained mixed liquor；
(3) 10g tween 80s, 8g pentanes and 10g p-methyl benzenesulfonic acids are added in the mixed liquor obtained by step (2),
Quickly stir；
(4) by the mixture injection mould obtained by step (3), it is placed in 160min in 80 DEG C of calorstat；
(5) it is cooled to room temperature after curing molding, the demoulding, that is, the high temperature for obtaining the present invention can ceramic phenol formaldehyde foam composite wood
Material.
The high temperature obtained by composition described above and preparation method can ceramic phenolic foam composite material main performance index
For：Room temperature comprcssive strength 0.33MPa, comprcssive strength 0.19MPa after high-temperature process, heat conductivity 0.062W/ (mK).
Embodiment 5
A kind of high temperature can ceramic phenolic foam composite material, be in accordance with the following methods and step preparation method prepare
's：
(1) phenolic resin of 100g is weighed；
(2) in the phenolic resin obtained by step (1), add 110g high temperature can ceramic compound inorganic stuffing
(wherein containing mica powder 71.8g, frit 16.5g, aluminium hydroxide 10g, dolomite 6.5g, perlite 2.5g, vermiculite power 3g),
3 parts of silane coupler, and be sufficiently mixed uniformly with agitator, obtain mixed liquor；
(3) 10g tween 80s, 8g pentanes and 10g p-methyl benzenesulfonic acids are added in the mixed liquor obtained by step (2),
Quickly stir；
(4) by the mixture injection mould obtained by step (3), it is placed in 140min in 70 DEG C of calorstat；
(5) it is cooled to room temperature after curing molding, the demoulding, that is, the high temperature for obtaining the present invention can ceramic phenol formaldehyde foam composite wood
Material.
The high temperature obtained by composition described above and preparation method can ceramic phenolic foam composite material main performance index
For：Room temperature comprcssive strength 0.24MPa, comprcssive strength 0.17MPa after high-temperature process, heat conductivity 0.058W/ (mK).
Claims (10)
1. a kind of high temperature can ceramic phenolic foam composite material, it is characterized in that mainly being made up of following raw material：Expandability phenolic aldehyde
100 parts of resin, foaming agent 5-10 parts, surfactant 6-10 parts, firming agent 10-12 parts, high temperature can ceramic composite inorganic
Filler 90-130 parts, silane coupler 2.5-4 parts, are mass parts.
2. high temperature according to claim 1 can ceramic phenolic foam composite material, it is characterized in that described high temperature can make pottery
The compound inorganic stuffing of porcelain is made up of inorganic ceramic raw material, low melting point flux, high temperature porogen, high-temperature expansion agent, each group
Point shared part by weight is：Inorganic ceramic raw material 65%, low melting point flux 15%, high temperature porogen 15%, high-temperature expansion agent
5%.
3. high temperature according to claim 2 can ceramic phenolic foam composite material, it is characterised in that described inorganic pottery
Porcelain raw material, is the one kind in Muscovitum, Pulvis Talci, Kaolin, montmorillonite, wollastonite, or the mixture of two or more arbitrary proportions,
Its size is 1-35 μm.
4. high temperature according to claim 2 can ceramic phenolic foam composite material, it is characterised in that described low melting point
Flux is the frit of low softening temperature, and its softening range is 380-620 DEG C, and main component is SiO2、ZnO、B2O3、
Na2O、CaO、K2O, its component participates in the ceramic transformation of inorganic ceramic raw material during high temperature.
5. high temperature according to claim 2 can ceramic phenolic foam composite material, it is characterised in that described hyperthermia induced
Hole agent is one or more in aluminium hydroxide, limestone, dolomite, and the gas that pyrolytic is produced plays pore effect, decomposes
The inorganic oxide of generation participates in the ceramic transformation of inorganic ceramic raw material.
6. high temperature according to claim 2 can ceramic phenolic foam composite material, it is characterized in that described high-temperature expansion
Agent be vermiculite power, crushed crude pearlite one or two.
7. a kind of high temperature can ceramic phenolic foam composite material preparation method, it is characterized in that comprising the following steps：
(1) expandable phenolic resin is weighed；
(2) in the phenolic resin obtained by step (1), by a certain percentage add high temperature can ceramic compound inorganic stuffing, and
It is sufficiently mixed uniformly with agitator, is obtained mixed liquor；
(3) surfactant, foaming agent and firming agent are added in the mixed liquor obtained by step (2), is quickly stirred, obtained
To mixture；
(4) by obtained by step (3) mixture injection mould in, be placed in 150min in 75 DEG C ± 5 DEG C of calorstat ±
10min, obtains sample after curing molding；
(5) sample is cooled to into room temperature, the demoulding obtains in claim 1 to 7 that arbitrary described high temperature can ceramic phenol formaldehyde foam
Composite.
8. preparation method according to claim 7, it is characterised in that described phenolic resin is resol, admittedly contain
Measure as 75-80%.
9. preparation method according to claim 7, it is characterised in that described foaming agent is physical blowing agent, specially just
Pentane；Described surfactant is tween 80；Described firming agent is p-methyl benzenesulfonic acid, and described silane coupler is
KH-550。
10. preparation method according to claim 7, it is characterized in that gained high temperature can ceramic phenolic foam composite material,
Its main performance index is：Room temperature comprcssive strength >=0.15MPa, comprcssive strength >=0.1MPa after high-temperature process, heat conductivity≤
0.07W/(m·K)。
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| CN109319805A (en) * | 2017-08-01 | 2019-02-12 | 江苏宝源高新电工有限公司 | A kind of preparation method of ceramics fluxing agent and ceramic fluxing agent and its application |
| CN114736400A (en) * | 2022-05-20 | 2022-07-12 | 武汉理工大学 | Ceramizable phenolic aerogel and preparation method thereof |
| CN115972711A (en) * | 2022-12-13 | 2023-04-18 | 南京理工大学 | Fire-resistant explosion-proof composite board and preparation method thereof |
| CN117507515A (en) * | 2024-01-08 | 2024-02-06 | 宁波卓翔科技有限公司 | High-temperature ceramic fireproof heat-insulating pad with inorganic fiber cloth as framework |
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| CN114736400A (en) * | 2022-05-20 | 2022-07-12 | 武汉理工大学 | Ceramizable phenolic aerogel and preparation method thereof |
| CN114736400B (en) * | 2022-05-20 | 2024-02-02 | 武汉理工大学 | Ceramizable phenolic aerogel and preparation method thereof |
| CN115972711A (en) * | 2022-12-13 | 2023-04-18 | 南京理工大学 | Fire-resistant explosion-proof composite board and preparation method thereof |
| CN117507515A (en) * | 2024-01-08 | 2024-02-06 | 宁波卓翔科技有限公司 | High-temperature ceramic fireproof heat-insulating pad with inorganic fiber cloth as framework |
| CN117507515B (en) * | 2024-01-08 | 2024-04-05 | 宁波卓翔科技有限公司 | High-temperature ceramic fireproof heat-insulating pad with inorganic fiber cloth as framework |
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