CN102775724A - Honeycomb-reinforced phenolic foam material and preparation method thereof - Google Patents
Honeycomb-reinforced phenolic foam material and preparation method thereof Download PDFInfo
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- CN102775724A CN102775724A CN2012101932593A CN201210193259A CN102775724A CN 102775724 A CN102775724 A CN 102775724A CN 2012101932593 A CN2012101932593 A CN 2012101932593A CN 201210193259 A CN201210193259 A CN 201210193259A CN 102775724 A CN102775724 A CN 102775724A
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Abstract
The invention relates to a honeycomb-reinforced phenolic foam material and a preparation method thereof, which belong to the field of polymer matrix composites. The honeycomb-reinforced phenolic foam material is characterized by taking phenolic foam as a matrix and a honeycomb material as a reinforcing material, wherein the honeycomb diameter of the honeycomb material is 1mm-10mm, and the slicing thickness of the honeycomb material is 1mm-10mm. The preparation method comprises the steps of completely dipping the honeycomb reinforcing material in the mixed raw materials, pre-foaming the material on a plate vulcanizing machine at 40-45 DEG C, and then heating and pressing the material on a plate vulcanizing machine at 85-95 DEG C for molding. The density of the prepared material ranges from 0.1g/cm<3> to 0.25g/cm<3>, and the material has favorable specific strength and fire resistance.
Description
Technical field
Present method belongs to the polymer matrix composite field, is specifically related to a kind of paper wasp nest, aramid fiber honeycomb enhancing phenolic foam material and preparation method thereof.
Background technology
The most outstanding characteristics of phenol formaldehyde foam are difficult combustion, low cigarette, high temperature creep-resisting.But it can cast-in-site foaming, can be molded, also mechanical workout, can be made into sheet material, shell and various special-shaped product.Because polystyrene foam and polyurethane foam are all inflammable, non-refractory, the restriction that in some industrially developed country, is just receiving fire department is used, and to the strict place of fire protection requirement, the existing explicit stipulation of government department can only be used phenol formaldehyde foam and sandwich board thereof.Thereby phenolic aldehyde foam thermal insulation material is to be more suitable for the high performance material that uses under the harsh envrionment conditions that requires in having, and bright development prospect is arranged.
The performance deficiency of the application of current restriction phenol formaldehyde foam mainly comes from two aspects, at first is that the fragility of phenolic foam material is big, and mechanical property is not enough.Next is that the phenol formaldehyde foam efflorescence is serious, can't use usually in the occasion that environmental requirement is higher.
Summary of the invention
The object of the present invention is to provide a kind of strength of materials height and can suppress honeycomb enhancing phenolic foam material of phenol formaldehyde foam powder phenomenon-tion and preparation method thereof.
A kind of honeycomb strengthens phenolic foam material, and it is characterized in that: as matrix, paper wasp nest or aramid fiber honeycomb are as strongthener by phenol formaldehyde foam for material; Wherein the phenol formaldehyde foam matrix comprises following quality component: 100 parts of resoles, tensio-active agent 1-8 part, paracril powder 0-20 part, composite whipping agent 2-20 part, solidifying agent 3-10 part; Described composite whipping agent is an Ethylene Dichloride: normal hexane is the mixture of 1:10-1:1; Described solidifying agent is a Phenylsulfonic acid; Described tensio-active agent is a kind of in DC193, tween 80, the polysorbas20; Wherein the honeycomb diameter of paper wasp nest or aramid fiber cellular material is 1mm ~ 10mm, and it is 1mm-10mm that sheet is cut thickness.Preferred version is: it is 1mm-2mm that diameter 1mm-4mm, sheet cut thickness.
Above-mentioned honeycomb strengthens the preparation method of phenolic foam material, and it is characterized in that may further comprise the steps: (1), all raw materials all adopt the proportioning in the claim 1; (2), resole, tensio-active agent and paracril thorough mixing is subsequent use; (3), the mixture and the composite whipping agent thorough mixing that under 0 ~ 30 ℃ environment, step (2) are obtained, add solidifying agent therein and also mix once more; (4), cellular material is impregnated into the mixture that step (3) obtains, and suitably shake cellular material to obtain sufficient dipping; (5), the impregnated cellular material of step (4) is put into mould; And send on the vulcanizing press that is preheating to 40 ~ 45 ℃ and place 3-5min; Treat wherein lower boiling composite whipping agent methylene dichloride foaming back taking-up, put into heating and pressurizing moulding on 85 ~ 95 ℃ of vulcanizing presses.
The resol that the present invention adopts have do not fire, low cigarette, high temperature creep-resisting and cheap advantage, this resin has been given the performance of using under corresponding fire prevention of product of the present invention and the hot environment; The present invention carries out foaming treatment to resol, makes the finished product have lower density (0.1-0.2g/cm
3); The present invention adopts cellular material that resol is carried out enhancement process, makes final product have good intensity and rigidity, and has controlled the powder phenomenon-tion of phenol formaldehyde foam well.Compare with fibre-reinforced phenol formaldehyde foam, this cellular structural material is as strengthening body, and the rigidity of its product is more excellent.In the technology implementation procedure, honey-combed is simple to obtain good dipping effect easily, the phenomenon of hollowization of subregion that can not occur occurring in the fiber reinforcement technology.More than comprehensive, the characteristics of the finished product of the present invention are HS, high rigidity, fire prevention, high temperature resistant and cost is low.
In the present invention; Influence of surfactant is the size of control abscess; The adding of tensio-active agent can reduce the surface tension of resol, thereby makes that the abscess after the foaming is more tiny, even, and little abscess under equal conditions can obtain better mechanical property.
The whipping agent that the present invention adopted is the compound system of methylene dichloride and normal hexane; The foam process that is adopted is a second time of foaming technology; Methylene dichloride begins foaming when being heated to 40 ~ 45 ℃; This moment, resol still was in the lower stage of viscosity, have certain fluidity can, the various piece of filled honeycomb material well under the promotion of methylene dichloride bubble; The content of methylene dichloride is less in the whipping agent compound system simultaneously, thereby is unlikely to cause resol to overflow outside the enhancing system.When 85 ~ 95 ℃ of heating, the normal hexane foaming is full of entire die phenolic resin curing moulding simultaneously, finally obtains material according to the invention.
Description of drawings
Fig. 1 is the performance data of embodiment and reference examples sample.
Embodiment
Below in conjunction with specific embodiments the present invention is done and to further describe.
The source of the main raw material that following examples adopted: whipping agent methylene dichloride, normal hexane, surfactant D C193, tween 80, polysorbas20, Phenylsulfonic acid are available from the tender sub-rattan science equipment in Nanjing ltd; The paracril powder is available from the positive nation in Jiangyin; Resole is synthetic for voluntarily, and its solid content is about 80%.The consumption unit of following embodiment and the used each component of reference examples is mass parts.
Reference examples 1 does not adopt cellular material to strengthen
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 5 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process:
Adopt whisking appliance that resole, DC193 and paracril were stirred 10 minutes, add composite whipping agent stirring and add Phenylsulfonic acid stirring 2 minutes after 5 minutes again.The resin that mixes is poured in the mould, mould is put into heating and pressurizing foaming on 90 ℃ the vulcanizing press.
Reference examples 2 does not adopt cellular material to strengthen (1 and 2 mainly is that density is different)
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 20 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process:
Adopt whisking appliance that resole, DC193 and paracril were stirred 10 minutes, add composite whipping agent stirring and add Phenylsulfonic acid stirring 2 minutes after 5 minutes again.The resin that mixes is poured in the mould, mould is put into heating and pressurizing foaming on 90 ℃ the vulcanizing press.
Embodiment 1
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
Honeycomb honeycomb strongthener: honeycomb diameter 1mm, sheet cut the aramid fiber honeycomb of thickness 1mm;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 5 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process:
(1), resole, DC193 and paracril powder thorough mixing is subsequent use;
(2), the mixture and the composite whipping agent thorough mixing that under 30 ℃ environment, step (1) are obtained, add Phenylsulfonic acid therein and also mix once more;
(3), cellular material is impregnated into the mixture that step (2) obtains, and suitably shake cellular material to obtain sufficient dipping;
(4), the impregnated cellular material of step (3) is put into mould; And send on the vulcanizing press that is preheating to 45 ℃ and place 3-5min; Treat wherein lower boiling whipping agent methylene dichloride foaming back taking-up, put into heating and pressurizing 15min moulding on 90 ℃ of vulcanizing presses.
Embodiment 2
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
Honeycomb honeycomb strongthener: honeycomb diameter 1mm, sheet cut the aramid fiber honeycomb of thickness 1mm;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 20 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 3
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:5;
The honeycomb strongthener: honeycomb diameter 2mm, sheet cut the aramid fiber honeycomb of thickness 1mm;
100 parts of resoles, 1 part of DC193,20 parts in paracril powder, 15 parts of composite whipping agents, 3 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 4
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
The honeycomb strongthener: honeycomb diameter 10mm, sheet cut the aramid fiber honeycomb of thickness 10mm;
100 parts of resoles, 8 parts of tween 80s, 10 parts in paracril powder, 20 parts of composite whipping agents, 3 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 5
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:1;
The honeycomb strongthener: honeycomb diameter 4mm, sheet cut the aramid fiber honeycomb of thickness 2mm;
100 parts of resoles, 1 part of polysorbas20,0 part in paracril powder, 20 parts of composite whipping agents, 10 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 6
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
Honeycomb honeycomb strongthener: honeycomb diameter 5mm, sheet cut the aramid fiber honeycomb of thickness 1mm;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 5 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 7
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
Honeycomb honeycomb strongthener: honeycomb diameter 10mm, sheet cut the aramid fiber honeycomb of thickness 1mm;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 5 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 8
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:5;
The honeycomb strongthener: honeycomb diameter 5mm, sheet cut the aramid fiber honeycomb of thickness 10mm;
100 parts of resoles, 5 parts of DC193,10 parts in paracril powder, 2 parts of composite whipping agents, 10 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
Honeycomb honeycomb strongthener: honeycomb diameter 1mm, sheet cut the paper synthetic fibre honeycomb of thickness 1mm;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 5 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 10
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
Honeycomb honeycomb strongthener: honeycomb diameter 5mm, sheet cut the paper synthetic fibre honeycomb of thickness 1mm;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 5 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 11
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
The honeycomb strongthener: honeycomb diameter 10mm, sheet cut the paper synthetic fibre honeycomb of thickness 10mm;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 5 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Embodiment 12
Prescription:
Composite whipping agent: Ethylene Dichloride: normal hexane=1:10;
Honeycomb honeycomb strongthener: honeycomb diameter 10mm, sheet cut the paper synthetic fibre honeycomb of thickness 10mm;
100 parts of resoles, 3 parts of DC193,10 parts in paracril powder, 20 parts of composite whipping agents, 8 parts of Phenylsulfonic acids.
The preparation process is with embodiment 1.
Performance relatively
The finished product that embodiment, reference examples are obtained carries out the sample preparation processing, and the sample that makes is carried out density, tensile strength, limiting oxygen index(LOI), and wherein, the tensile property test is undertaken by the GB/T1040-90 standard; The shock strength test is undertaken by the GB/T1043.1-2008 standard; Density measurement is undertaken by ASTM D792 standard; The limiting oxygen index(LOI) test is carried out according to GB/T 240-2008.The gained result is as shown in table 1.The unit of each index is following: density: g/cm
3, tensile strength: MPa, shock strength: KJ/m
2, limiting oxygen index(LOI): %.
Can find out that from table 1 reference examples 1,2 does not use cellular material to strengthen, specific tenacity, toughness all improve a lot mutually with reference examples to use cellular material enhanced phenolic resin foam under the equal densities.The limiting oxygen index(LOI) of phenol formaldehyde foam descends but the range of decrease and not obvious to some extent to adopt cellular material to strengthen afterwards, and employing paper wasp nest enhanced phenol formaldehyde foam limiting oxygen index(LOI) has decline to a certain degree but still belongs to A level non-fire material.Embodiment can find out that the size of strongthener honeycomb diameter has determined the strength of materials, flexible height to a great extent, and the more little then intensity of honeycomb diameter is high more, toughness is good more.Can find out from each embodiment The performance test results; Under equal densities, the same matrix formulation; The intensity of paper wasp nest enhanced phenol formaldehyde foam and toughness all are lower than aramid fiber honeycomb enhanced phenol formaldehyde foam, still have raising by a relatively large margin but compare its intensity with enhanced reference examples not.After adding cellular material, the powder phenomenon-tion of phenol formaldehyde foam sample obviously alleviates.
The above only is the embodiment that the present invention enumerates, and technical scope of the present invention is not done any restriction.
Claims (3)
1. a honeycomb strengthens phenolic foam material, and it is characterized in that: as matrix, paper wasp nest or aramid fiber honeycomb are as strongthener by phenol formaldehyde foam for material;
Wherein the phenol formaldehyde foam matrix comprises following quality component: 100 parts of resoles, tensio-active agent 1-8 part, paracril powder 0-20 part, composite whipping agent 2-20 part, solidifying agent 3-10 part; Described composite whipping agent is an Ethylene Dichloride: normal hexane is the mixture of 1:10-1:1; Described solidifying agent is a Phenylsulfonic acid; Described tensio-active agent is a kind of in DC193, tween 80, the polysorbas20;
Wherein the honeycomb diameter of paper wasp nest or aramid fiber cellular material is 1mm ~ 10mm, and it is 1mm-10mm that sheet is cut thickness.
2. honeycomb according to claim 1 strengthens phenolic foam material, and it is characterized in that: the honeycomb diameter 1mm-4mm of above-mentioned paper wasp nest or aramid fiber cellular material, it is 1mm-2mm that sheet is cut thickness.
3. strengthen the preparation method of phenolic foam material based on claim 1 honeycomb, it is characterized in that may further comprise the steps:
(1), all raw materials all adopt the proportioning in the claim 1;
(2), resole, tensio-active agent and paracril thorough mixing is subsequent use;
(3), the mixture and the composite whipping agent thorough mixing that under 0 ~ 30 ℃ environment, step (2) are obtained, add solidifying agent therein and also mix once more;
(4), cellular material is impregnated into the mixture that step (3) obtains, and suitably shake cellular material to obtain sufficient dipping;
(5), the impregnated cellular material of step (4) is put into mould; And send on the vulcanizing press that is preheating to 40 ~ 45 ℃ and place 3-5min; Treat wherein lower boiling composite whipping agent methylene dichloride foaming back taking-up, put into heating and pressurizing moulding on 85 ~ 95 ℃ of vulcanizing presses.
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| CN2012101932593A CN102775724A (en) | 2012-06-13 | 2012-06-13 | Honeycomb-reinforced phenolic foam material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103552245A (en) * | 2013-11-13 | 2014-02-05 | 宁波市鄞州科启动漫工业技术有限公司 | Method for forming honeycomb rubber product |
| CN104788895A (en) * | 2015-04-17 | 2015-07-22 | 广西藤县通轩立信化学有限公司 | Preparation method for expandable phenolic resin composition |
| CN104788891A (en) * | 2015-04-17 | 2015-07-22 | 广西藤县通轩立信化学有限公司 | Preparation method for expandable phenolic resin composition |
| CN105542386A (en) * | 2016-02-15 | 2016-05-04 | 上海尖端工程材料有限公司 | Preparation method of continuous phenolic-foam-filled honeycomb material with fixed height and thickness |
| CN108164741A (en) * | 2017-12-12 | 2018-06-15 | 湖北航天化学技术研究所 | A kind of silicon substrate heat-insulating material of aramid fiber Honeycomb and preparation method thereof |
| CN108727771A (en) * | 2018-05-22 | 2018-11-02 | 长春珑鑫新材料有限公司 | A kind of composite material and preparation method of honeycomb filling in situ phenol formaldehyde foam |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108164741A (en) * | 2017-12-12 | 2018-06-15 | 湖北航天化学技术研究所 | A kind of silicon substrate heat-insulating material of aramid fiber Honeycomb and preparation method thereof |
| CN108164741B (en) * | 2017-12-12 | 2021-03-26 | 湖北航天化学技术研究所 | Silicon-based heat-insulating material reinforced by aramid honeycomb and preparation method thereof |
| CN108727771A (en) * | 2018-05-22 | 2018-11-02 | 长春珑鑫新材料有限公司 | A kind of composite material and preparation method of honeycomb filling in situ phenol formaldehyde foam |
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Application publication date: 20121114 |