CN106589791B - A kind of high temperature can ceramic phenolic foam composite material and preparation method thereof - Google Patents
A kind of high temperature can ceramic 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
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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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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
Abstract
High temperature provided by the invention can ceramic phenolic foam composite material, it is mainly prepared from the following raw materials: 100 parts of expandable phenolic resin, 5-10 parts of foaming agent, 6-10 parts of surfactant, 10-12 parts of curing agent, high temperature can be 90-130 parts of compound inorganic stuffing of ceramic, and 2.5-4 parts of silane coupling agent, be mass parts.Preparation method are as follows: weigh a certain amount of phenolic resin, by a certain percentage be added high temperature can ceramic compound inorganic stuffing and silane coupling agent, it is sufficiently mixed uniformly with blender, add surfactant, foaming agent and curing agent, quickly stir evenly, injection mold is placed in 150min ± 10min in 75 DEG C ± 5 DEG C of insulating box, is cooled to room temperature demoulding after curing molding.The composite material has lower thermal coefficient (≤0.07W/ (mK)), higher compressive strength (normal temperature compressed intensity >=0.15MPa, compressive strength >=0.1MPa after high-temperature process), shape, performance and microcosmic porous structure are able to maintain under high temperature aerobic conditions.
Description
Technical field
The present invention relates to polymer matrix foam composite technology fields, and in particular to a kind of high temperature can ceramic phenolic aldehyde bubble
Foam composite material and preparation method can be applied to the fields such as heat preservation, heat-insulated, fire prevention.
Background technique
Phenolic foam composite material has the excellent properties such as good fire retardant, low cigarette, low toxicity, heat-resisting, heat preservation, sound insulation, and
With very wide use temperature range (- 196 DEG C~+150 DEG C), in the fields such as aerospace, national defence, ship, building, chemical industry
Be widely used, such as be used as heat insulation tile of shuttle, rocket ablator, submarine thermal and sound insulating materials, civil aircraft bulkhead,
Architecture exterior wall insulating materials, the heat preservation of central air conditioner system air hose 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 the inorganic guarantor of mineral wool, perlite and mineral wool etc. (generally at 650 DEG C or more) tradition
Adiabator is larger compared to gap, so at present under the high temperature conditions still largely using thermal coefficient height, the tradition of heat insulation effect difference
Inorganic heat insulation material, thermal coefficient is generally more than 0.1W/ (mK).Therefore organic insulation material thermal coefficient is being kept
Under the premise of low, thermal insulation property is good, its high temperature resistance how is improved as an important topic.
In order to further increase the heat resistance of phenolic foam composite material, researcher by phenolic resin as matrix resin it is modified with
And it is modified by introducing various fillers.Huang Jianqing et al. has synthesized foamable boron bakelite resin by addition boric acid and has made
For boron modification phenol formaldehyde foam, high temperature resistance is improved, and thermal decomposition temperature is 450 DEG C, and the highest of boron modification phenol formaldehyde foam uses
Temperature be 200 DEG C (high temperature resistance glass reinforced plastic/composite material of Huang Jianqing, Pan Anjian boron modification phenol formaldehyde foam, 2007,6:
26-28.).Wang Bin et al. is by B2O3Phenol formaldehyde foam is introduced, the thermal decomposition temperature and carbon yield of prepared modified phenolic foam mention
Height works as B2O3When content is mass fraction 7%, the high temperature resistance of phenol formaldehyde foam is optimal, in nitrogen atmosphere when its weightlessness 10%
Thermal decomposition temperature be 447 DEG C (Wang Bin, Li Hejun, Zhang Yulei, Li Yunyu, Liu Zhangqing's boron modification phenolic foam composite material
Preparation is in progress with performance study Chinese material, 2013,32 (11): 641-646.).He Bin et al. passes through addition Nano-meter SiO_22It mentions
Heat resistance (He Bin, Yang Zhenguo the Nano-meter SiO_2 of high phenol formaldehyde foam2The preparation and characterization petrochemical industry of modified phenolic foam,
2007,36 (12), 1266-1270.)；It is improved using montmorillonite, carbon fiber composite modified phenolic aldehyde foam thermal insulation material in position east et al.
Heat-resisting and mechanical property (protect by position east, Li Dongfeng, Zhang Lu, Zhao Zhankui, Ao Yuhui montmorillonite, carbon fiber composite modified phenolic aldehyde foam
The research Chinese material seminar of adiabator, 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 form, can make pottery
Porcelain fluidized polymer based composites have the performance similar with general polymer based composites at normal temperature, 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, have certain intensity and can bear one
Fixed impact force, it is very concerned 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.) etc. the ceramic packings system such as mica is added in silicone resin
Standby high temperature can ceramic composite material, eutectic reaction occurs for composite material cracking process in 1050 DEG C or so of hot-air
Mullite ceramic phase structure is formed, to improve high-temperature residual amount and pyrogenous residue intensity, having started can ceramic fluidized polymer
The beginning of based composites research and application.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 dedicated to carbon-based resin composite material can ceramic research and application, ZL 201210145780X
Disclose one kind can Carbon-based polymer composite material capable of being ceramized and preparation method thereof, paper (Chih-hsiung Huang, the fourth of Chih-hsiung Huang et al.
Outstanding person, Shi Minxian, Liu Tianxiang .ZrSi2The preparation of/boron phenolic foam and its enhancing mechanism composite material journal of pyrolysis product,
2015 Network Priorities are published, DOI:10.13801/j.cnki.fhclxb.20151218.002.) disclose ZrSi2/ boron phenolic
The preparation and its performance of foam.
It is analyzed from document report, phenolic foam composite material has good heat resistance, can make at 200 DEG C or less
With but at higher temperatures, the problems such as oxidation, cracking, weightless, structure and performance are destroyed is serious.Can porcelain polymer matrix
Composite material can be changed into inorganic ceramic material or glass ceramic material under the high temperature conditions, be resistant to 1000 DEG C or more
High temperature, and be able to maintain the structure and performance of composite material, have certain research in fireproof cable, thermally protective materials field and answer
With.The invention proposes a kind of high temperature can ceramic phenolic foam composite material and preparation method thereof, high temperature can ceramic phenolic aldehyde
The successful preparation and application of foamed composite, the hot spot of societys such as heat-insulated for solution energy conservation and environmental protection, back-fire relief have extremely
Major and immediate significance, while also there is particularly important economy and society meaning.
Summary of the invention
It can ceramic phenolic foam composite material and its preparation side technical problem solved by the present invention is providing a kind of high temperature
Method, which has lower thermal coefficient, higher compressive strength at room temperature, and issues in high temperature aerobic conditions
The processes such as raw oxidation, cracking, ceramic transformation, ultimately form porous ceramic phase or glass phase structure, and are able to maintain initial
Shape, performance and microcosmic porous structure.Traditional organic foam composite material is solved in high-temp combustion or oxidizing condition high temperature resistant
The insufficient problem of performance.
The present invention solves its technical problem, and the following technical solution is employed:
High temperature provided by the invention can ceramic phenolic foam composite material, be mainly prepared from the following raw materials: expandability
100 parts of phenolic resin, 5-10 parts of foaming agent, 6-10 parts of surfactant, 10-12 parts of curing agent, high temperature can ceramic it is compound
90-130 parts of inorganic filler, 2.5-4 parts of silane coupling agent, be mass parts.
The high temperature can ceramic compound inorganic stuffing by inorganic ceramic raw material, low melting point fluxing agent, high temperature pore
Agent, high-temperature expansion agent form, weight ratio shared by each component are as follows: inorganic ceramic raw material 65%, low melting point fluxing agent 15%, high temperature
Pore-foaming agent 15%, high-temperature expansion agent 5%.
The inorganic ceramic raw material is one of mica, talcum powder, kaolin, montmorillonite, wollastonite or two kinds
The mixture of any of the above ratio, particle size are 1-35 μm.
The low melting point fluxing agent is the frit of low softening temperature, and softening range is 380-620 DEG C, mainly
Ingredient is SiO2、ZnO、B2O3、Na2O、CaO、K2O, its component participates in the ceramic transformation of inorganic ceramic raw material when high temperature.
The high temperature pore-foaming agent is one of aluminium hydroxide, lime stone, dolomite or a variety of, what pyrolytic generated
Gas plays pore, and the inorganic oxide for decomposing generation participates in the ceramic transformation of inorganic ceramic raw material.
The high-temperature expansion agent is the one or two of vermiculite power, crushed crude pearlite.
High temperature provided by the invention can ceramic phenolic foam composite material, preparation method includes the following steps:
(1) expandable phenolic resin is weighed；
(2) in step (1) resulting phenolic resin, be added by a certain percentage high temperature can the composite inorganic of ceramic fill out
Material, and be sufficiently mixed uniformly with blender, obtain mixed liquor；
(3) surfactant, foaming agent and curing agent are added in step (2) obtained mixed liquor, quickly stirring is equal
It is even, obtain mixture；
(4) by the obtained mixture injection mold of step (3), it is placed in 150min in 75 DEG C ± 5 DEG C of insulating box
± 10min obtains sample after curing molding；
(5) sample is cooled to room temperature, is demoulded, obtaining the high temperature can ceramic phenolic foam composite material.
In the above method, the phenolic resin is resol, solid content 75-80%.
In the above method, the foaming agent is physical blowing agent, specially pentane；The surfactant is to spit
Temperature -80；The curing agent is p-methyl benzenesulfonic acid, and the silane coupling agent is KH-550.
In the above method, obtained high temperature can ceramic phenolic foam composite material, main performance index are as follows: room temperature
Compression strength >=0.15MPa, compression strength >=0.1MPa after high-temperature process, thermal coefficient≤0.07W/ (mK).
The present invention due to joined 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 ceramic compound inorganic stuffing addition so that phenolic foam material can turn under the high temperature conditions
Become ceramic phase or glass phase porous material, heat resistance improves, so that phenolic foam composite material is resistant to higher temperature
Degree and longer time.
(2) high temperature can ceramic phenolic foam composite material high temperature resistance significantly improve, but still have and lower lead
Hot coefficient, thermal coefficient≤0.07W/ (mK).
(3) under high temperature aerobic conditions, which can the oxidation of ceramic phenolic foam composite material experience, cracking, ceramic
The processes such as transformation, ultimately form ceramic phase or glass phase structure, still keep macro geometry and microcosmic porous structure substantially.
(4) there is high intensity: normal temperature compressed intensity >=0.15MPa, compressive strength >=0.1MPa after high-temperature process.
Detailed description of the invention
Fig. 1 is that high temperature can the section scanning electron microscope photo of ceramic phenolic foam composite material at normal temperature.
Fig. 2 be high temperature can ceramic phenolic foam composite material at 900 DEG C treated section scanning electron microscope is shone
Piece.
Specific embodiment
The present invention uses expandability phenolic aldehyde for resin matrix, foaming agent, curing agent, surfactant, silane coupling agent etc.
For auxiliary agent, high temperature can the composite inorganic group of ceramic be divided into filler, foam, ultimately provide according to certain foam process
A kind of high temperature can porcelain phenolic foam composite material and preparation method thereof.Under burning or high temperature aerobic conditions, which can ceramics
Change the processes such as the oxidation of phenolic foam composite material experience, cracking, ceramic transformation, ultimately form ceramic phase or glass phase structure,
Still macro geometry and microcosmic porous structure are kept substantially.
Below with reference to examples and drawings, 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 curing agent, high temperature can ceramic 90 parts of compound inorganic stuffing (wherein contain mica 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 coupling agent, be 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 curing agent, high temperature can 130 parts of compound inorganic stuffing of ceramic (wherein contain kaolin
84.5 parts, 19.5 parts of frit, 19.5 parts of lime stone, 6.5 parts of crushed crude pearlite), 4 parts of silane coupling agent, be 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 curing agent, high temperature can 110 parts of 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 coupling agent, be mass parts.
Embodiment 4
A kind of high temperature can ceramic phenolic foam composite material, be in accordance with the following methods and the preparation of the preparation method of step
:
(1) phenolic resin of 100g is weighed；
(2) in step (1) obtained phenolic resin, be added 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 coupling agent, and use blender
It is sufficiently mixed uniformly, obtains mixed liquor；
(3) 10g Tween-80,8g pentane and 10g p-methyl benzenesulfonic acid are added in step (2) obtained mixed liquor,
Quickly stir evenly；
(4) by the obtained mixture injection mold of step (3), it is placed in 160min in 80 DEG C of insulating box；
(5) be cooled to room temperature after curing molding, demoulding to get to high temperature of the 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
Are as follows: room temperature compression strength 0.33MPa, compression strength 0.19MPa, thermal coefficient 0.062W/ (mK) after high-temperature process.
Embodiment 5
A kind of high temperature can ceramic phenolic foam composite material, be in accordance with the following methods and the preparation of the preparation method of step
:
(1) phenolic resin of 100g is weighed；
(2) in step (1) obtained phenolic resin, be added 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 coupling agent, and be sufficiently mixed uniformly with blender, obtain mixed liquor；
(3) 10g Tween-80,8g pentane and 10g p-methyl benzenesulfonic acid are added in step (2) obtained mixed liquor,
Quickly stir evenly；
(4) by the obtained mixture injection mold of step (3), it is placed in 140min in 70 DEG C of insulating box；
(5) be cooled to room temperature after curing molding, demoulding to get to high temperature of the 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
Are as follows: room temperature compression strength 0.24MPa, compression strength 0.17MPa, thermal coefficient 0.058W/ (mK) after high-temperature process.
Claims (9)
1. a kind of high temperature can ceramic phenolic foam composite material, it is characterized in that being mainly prepared from the following raw materials: expandability phenolic aldehyde
100 parts of resin, 5-10 parts of foaming agent, 6-10 parts of surfactant, 10-12 parts of curing agent, high temperature can ceramic composite inorganic
90-130 parts of filler, 2.5-4 parts of silane coupling agent, be mass parts；The high temperature can ceramic compound inorganic stuffing by
Inorganic ceramic raw material, low melting point fluxing agent, high temperature pore-foaming agent, high-temperature expansion agent form, weight ratio shared by each component are as follows: inorganic
Ceramic raw material 65%, low melting point fluxing agent 15%, high temperature pore-foaming agent 15%, high-temperature expansion agent 5%.
2. high temperature according to claim 1 can ceramic phenolic foam composite material, it is characterised in that the inorganic pottery
Porcelain raw material is the mixture of one of mica, talcum powder, kaolin, montmorillonite, wollastonite or two or more arbitrary proportions,
Its particle size is 1-35 μm.
3. high temperature according to claim 1 can ceramic phenolic foam composite material, it is characterised in that the low melting point
Fluxing agent is the frit of low softening temperature, and softening range is 380-620 DEG C, main component SiO2、ZnO、B2O3、
Na2O、CaO、K2O, its component participates in the ceramic transformation of inorganic ceramic raw material when high temperature.
4. high temperature according to claim 1 can ceramic phenolic foam composite material, it is characterised in that the hyperthermia induced
Hole agent is one of aluminium hydroxide, lime stone, dolomite or a variety of, and the gas that pyrolytic generates plays pore, is decomposed
The inorganic oxide of generation participates in the ceramic transformation of inorganic ceramic raw material.
5. high temperature according to claim 1 can ceramic phenolic foam composite material, it is characterized in that the high-temperature expansion
Agent is the one or two of vermiculite power, crushed crude pearlite.
6. high temperature described in a kind of claim 1-5 any one can ceramic phenolic foam composite material preparation method, it is special
Sign be the following steps are included:
(1) expandable phenolic resin is weighed；
(2) in step (1) resulting phenolic resin, by a certain percentage be added high temperature can ceramic compound inorganic stuffing, and
It is sufficiently mixed uniformly with blender, obtains mixed liquor；
(3) surfactant, foaming agent and curing agent are added in step (2) obtained mixed liquor, quickly stirs evenly, obtains
To mixture；
(4) in step (3) obtained mixture injection mold, will be placed in 150min in 75 DEG C ± 5 DEG C of insulating box ±
10min obtains sample after curing molding；
(5) sample is cooled to room temperature, is demoulded, obtaining high temperature can ceramic phenolic foam composite material.
7. preparation method according to claim 6, it is characterised in that the phenolic resin is resol, admittedly contain
Amount is 75-80%.
8. preparation method according to claim 6, it is characterised in that the foaming agent is physical blowing agent, is specifically positive
Pentane；The surfactant is Tween-80；The curing agent is p-methyl benzenesulfonic acid, and the silane coupling agent is
KH-550。
9. preparation method according to claim 6, it is characterized in that gained high temperature can ceramic phenolic foam composite material,
Main performance index are as follows: room temperature compression strength >=0.15MPa, compression strength >=0.1MPa after high-temperature process, thermal coefficient≤
0.07W/(m·K)。
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| CN109319805B (en) * | 2017-08-01 | 2021-11-05 | 江苏宝源高新电工有限公司 | Preparation method of ceramic fluxing agent, ceramic fluxing agent and application of ceramic fluxing agent |
| CN107698211A (en) * | 2017-08-29 | 2018-02-16 | 北京禾木之家科技发展有限公司 | The preparation method of light composite board |
| 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 |
| 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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| CN1613640A (en) * | 2003-11-05 | 2005-05-11 | 厦门新风机实业有限公司 | Nanometer light catalyst phenolic resin foaming suspended ceiling board and manufacture |
| CN1844233A (en) * | 2006-03-21 | 2006-10-11 | 上海胜星树脂涂料有限公司 | Method for preparing high temperature resistant phenol-formaldehyde foam composite thermal-insulating materials |
| CN101560111A (en) * | 2009-04-08 | 2009-10-21 | 吴汉阳 | Foamed ceramics energy saving and heat preservation decorative wall brick and manufacture method thereof |
| CN103058632A (en) * | 2013-01-14 | 2013-04-24 | 武汉理工大学 | Ceramic high carbon polymer matrix composite and preparation method thereof |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613640A (en) * | 2003-11-05 | 2005-05-11 | 厦门新风机实业有限公司 | Nanometer light catalyst phenolic resin foaming suspended ceiling board and manufacture |
| CN1844233A (en) * | 2006-03-21 | 2006-10-11 | 上海胜星树脂涂料有限公司 | Method for preparing high temperature resistant phenol-formaldehyde foam composite thermal-insulating materials |
| CN101560111A (en) * | 2009-04-08 | 2009-10-21 | 吴汉阳 | Foamed ceramics energy saving and heat preservation decorative wall brick and manufacture method thereof |
| CN103058632A (en) * | 2013-01-14 | 2013-04-24 | 武汉理工大学 | Ceramic high carbon polymer matrix composite and preparation method thereof |
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