CN102977547A - Low temperature rapid-foaming phenol formaldehyde foam thermal insulation board preparation method - Google Patents
Low temperature rapid-foaming phenol formaldehyde foam thermal insulation board preparation method Download PDFInfo
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- CN102977547A CN102977547A CN201210377017XA CN201210377017A CN102977547A CN 102977547 A CN102977547 A CN 102977547A CN 201210377017X A CN201210377017X A CN 201210377017XA CN 201210377017 A CN201210377017 A CN 201210377017A CN 102977547 A CN102977547 A CN 102977547A
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Abstract
The present invention discloses a low temperature rapid-foaming phenol formaldehyde foam thermal insulation board preparation method, which is characterized in that the method comprises the following steps: (1) synthesizing a phenol formaldehyde resin capable of carrying out low temperature foaming: adding phenol and formaldehyde in a reaction vessel to mix, adding sodium hydroxide, carrying out a condensation polymerization reaction, carrying out neutralization with hydrochloric acid to achieve a neutral state, and carrying out vacuum reduced pressure dehydration until a viscosity is 1000-1200 mpa.s; and (2) selecting materials: selecting 100 parts by mass of the phenol formaldehyde resin capable of carrying out low temperature foaming, 4-7 parts by mass of a surfactant, 6-9 parts by mass of a foaming agent, 5-10 parts by mass of a modifier, 30-60 parts by mass of a solid filler, 2-5 parts by mass of a dispersant, and 20-40 parts by mass of a curing agent, carrying out mixing and complete stirring at a room temperature, rapidly conveying into a laminating machine, and carrying out curing cutting to obtain the low temperature rapid-foaming phenol formaldehyde foam thermal insulation board, wherein a non-woven fabric is pre-placed in the laminating machine. The method has characteristics of one time molding, simple process and continuous production. The prepared board has characteristics of low cost, high mechanical property and high fire retardation.
Description
Technical field
The invention belongs to the organic polymer composite technical field, specifically a kind of preparation method of low temperature fast foaming phenolic foam heat insulation plate.
Background technology
Phenolic foam material have low, the low smoke density of thermal conductivity, difficult combustion from put out, the excellent characteristic of fire resistance.All be to adopt the heat foaming at present both at home and abroad, energy consumption is large, yields poorly, and production cost is high, the warming plate of production exist intensity low, frangible, easily fall the defective such as slag.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, can realize serialization production, prepared warming plate cost is low, the preparation method of the low temperature fast foaming phenolic foam heat insulation plate that mechanical property and flame retardant properties are good.
In order to reach above purpose, the technical solution adopted in the present invention is: the preparation method of this a kind of low temperature fast foaming phenolic foam heat insulation plate is characterized in that: it may further comprise the steps makes:
(1) but, synthetic low-temp foaming resol: the mol ratio 1:(1.2-1.8 that in reaction vessel, press material) add the mixing of phenol and formaldehyde, press 2.7% of phenol quality and add sodium hydroxide catalyst, the question response mixture is warming up to 60-70 ℃, be incubated 2 hours, then 86 ℃ of polycondensations 1 hour, 80 ℃ of polycondensations 1 hour are neutralized to neutrality with hydrochloric acid soln, vacuum decompression dewater to viscosity be 1000-1200mpa.s, but make low-temp foaming resol;
(2), preparation low-temp foaming phenolic foam heat insulation plate: choose in mass ratio following material: but low-temp foaming resol: 100 parts; Tensio-active agent: 4-7 parts; Whipping agent: 6-9 parts; Properties-correcting agent: 5-10 parts; Solid packing: 30-60 parts; Dispersion agent: 2-5 parts; Solidifying agent: 20-40 parts; Under the room temperature, above-mentioned raw materials is mixed fully stirring, send into fast in the laminating machine of prior placement non-woven fabrics, at pressure 30-50Kg/cm
2, 3-5 m/mins of speed condition under, solidify cutting and namely get the low-temp foaming phenolic foam heat insulation plate.
Described tensio-active agent is any one or two kinds of mixture in tween T-80 and the methyl-silicone oil.
Described whipping agent is the solidliquid mixture of ammonium hydrogencarbonate and Skellysolve A, perhaps the solidliquid mixture of sodium bicarbonate and Skellysolve A.
Described properties-correcting agent is any one or two kinds of mixture in o-phthalic acid dibutyl ester and the ethylene glycol.
Described solid packing is any one or two kinds of mixture in aluminium hydroxide, magnesium hydroxide and the talcum powder.
Described dispersion agent is the mixture of any or two kinds in tripoly phosphate sodium STPP and the Sodium hexametaphosphate 99.
Described solidifying agent is any one or more mixture aqueous solution in sulfuric acid, methylsulphonic acid, phosphoric acid and the formic acid.
Beneficial effect of the present invention is: select solid-liquid mixed type whipping agent to improve the resin lather quickness, also avoided inflammable, the volatile fire safety hidden danger that causes of the organic lower boiling alkane of whole usefulness, fluorochlorohydrocarbon; Simultaneously, need not heating and can realize in 10-20 ℃ of scopes of low temperature that 5-10 minutes fast foamings solidify, saved the additional cost of investment boiler; And the inoganic solids filler that adds has improved flame retardant properties and the mechanical strength of foams.But the present invention's once shaped, technique is simple, can realize serialization production, and prepared warming plate cost is low, and mechanical property and flame retardant resistance are high, have eliminated the problem that common phenolic-aldehyde heat-insulation board is frangible, fall slag.
Embodiment
Embodiment 1:
A kind of preparation method of low temperature fast foaming resol warming plate is characterized in that: it may further comprise the steps makes:
(1) but, synthetic low-temp foaming resol: mol ratio 1:1.2 input phenol, the formaldehyde of in reaction vessel, press material, press 2.7% of phenol quality and add sodium hydroxide catalyst, the question response mixture is warming up to 60 ℃, insulation reaction 2 hours, then 1 hour, 80 ℃ polycondensations of 86 ℃ of polycondensations are 1 hour, be neutralized to neutrality with hydrochloric acid soln, vacuum decompression dewater to viscosity be 1200mpa.s, but make low-temp foaming resol;
(2), preparation low-temp foaming phenolic foam heat insulation plate: under the room temperature, but with 100 parts in low-temp foaming resol, 4 parts of tensio-active agent methyl-silicone oils, 3 parts of whipping agent sodium bicarbonates, 6 parts of Skellysolve As, 5 parts of properties-correcting agent o-phthalic acid dibutyl esters, 30 parts in solid packing aluminium hydroxide, 2 parts of pentasodium triphosphate of dispersing agent, 20 parts in solidifying agent sulfuric acid fully mixes stand-by.Simultaneously, by the good non-woven fabrics of specification requirement place mat, adjust 3 m/mins of laminating machine speed, pressure 30Kg/cm
2, the continuous foamed curing of input compound namely gets warming plate.
Embodiment 2:
A kind of preparation method of low temperature fast foaming resol warming plate is characterized in that: it may further comprise the steps makes:
(1) but, synthetic low-temp foaming resol: mol ratio 1:1.8 input phenol, the formaldehyde of in reaction vessel, press material, press 2.7% of phenol quality and add sodium hydroxide catalyst, the question response mixture is warming up to 70 ℃, insulation reaction 2 hours, then 1 hour, 80 ℃ polycondensations of 86 ℃ of polycondensations are 1 hour, be neutralized to neutrality with hydrochloric acid soln, vacuum decompression dewater to viscosity be 1100mpa.s, but make low-temp foaming resol;
(2), the preparation of low-temp foaming phenolic foam heat insulation plate: under the room temperature, but with 100 parts in low-temp foaming resol, 5 parts of tensio-active agent tween T-80,3 parts of whipping agent sodium bicarbonates, 6 parts of Skellysolve As, 10 parts of properties-correcting agent o-phthalic acid dibutyl esters, 30 parts of solid packing magnesium hydroxides, 2 parts of pentasodium triphosphate of dispersing agent, 20 parts of solidifying agent methylsulphonic acids fully mix stand-by.Simultaneously, by the good non-woven fabrics of specification requirement place mat, adjust 4 m/mins of laminating machine speed, pressure 30Kg/cm
2, the continuous foamed curing of input compound namely gets warming plate.
Embodiment 3:
A kind of preparation method of low temperature fast foaming resol warming plate is characterized in that: it may further comprise the steps makes:
(1) but, synthetic low-temp foaming resol: mol ratio 1:1.5 input phenol, the formaldehyde of in reaction vessel, press material, press 2.7% of phenol quality and add sodium hydroxide catalyst, the question response mixture is warming up to 65 ℃, insulation reaction 2 hours, then 1 hour, 80 ℃ polycondensations of 86 ℃ of polycondensations are 1 hour, be neutralized to neutrality with hydrochloric acid soln, vacuum decompression dewater to viscosity be 1000mpa.s, but make low-temp foaming resol;
(2), the preparation of low-temp foaming phenolic foam heat insulation plate: under the room temperature, but with 100 parts in low-temp foaming resol, 4 parts of tensio-active agent tween T-80,3 parts of whipping agent ammonium hydrogencarbonates, 3 parts of Skellysolve As, 10 parts of properties-correcting agent ethylene glycol, 30 parts of solid packing talcum powder, 5 parts of pentasodium triphosphate of dispersing agent, 0 part of solidifying agent phosphatase 24 fully mixes stand-by.Simultaneously, by the good non-woven fabrics of specification requirement place mat, adjust 5 m/mins of laminating machine speed, pressure 50Kg/cm
2, the continuous foamed curing of input compound namely gets warming plate.
Embodiment 4:
A kind of preparation method of low temperature fast foaming resol warming plate is characterized in that: it may further comprise the steps makes:
(1) but, synthetic low-temp foaming resol: mol ratio 1:1.8 input phenol, the formaldehyde of in reaction vessel, press material, press 2.7% of phenol quality and add sodium hydroxide catalyst, the question response mixture is warming up to 60 ℃, insulation reaction 2 hours, then 1 hour, 80 ℃ polycondensations of 86 ℃ of polycondensations are 1 hour, be neutralized to neutrality with hydrochloric acid soln, vacuum decompression dewater to viscosity be 1200mpa.s, but make low-temp foaming resol;
(2), the preparation of low-temp foaming phenolic foam heat insulation plate: under the room temperature, but with 100 parts in low-temp foaming resol, 7 parts of tensio-active agent tween T-80,3 parts of whipping agent sodium bicarbonates, 3 parts of Skellysolve As, 8 parts of properties-correcting agent o-phthalic acid dibutyl esters, 30 parts of solid packing magnesium hydroxides, 30 parts in aluminium hydroxide, 2 parts of sodium hexametaphosphate dispersants, 30 parts in solidifying agent formic acid fully mixes stand-by.Simultaneously, by the good non-woven fabrics of specification requirement place mat, adjust 4 m/mins of laminating machine speed, pressure 40Kg/cm
2, the continuous foamed curing of input compound namely gets warming plate.
Embodiment 5:
A kind of preparation method of low temperature fast foaming resol warming plate is characterized in that: it may further comprise the steps makes:
(1) but, synthetic low-temp foaming resol: mol ratio 1:1.2 input phenol, the formaldehyde of in reaction vessel, press material, press 2.7% of phenol quality and add sodium hydroxide catalyst, the question response mixture is warming up to 65 ℃, insulation reaction 2 hours, then 1 hour, 80 ℃ polycondensations of 86 ℃ of polycondensations are 1 hour, be neutralized to neutrality with hydrochloric acid soln, vacuum decompression dewater to viscosity be 1100mpa.s, but make low-temp foaming resol;
(2), the preparation of low-temp foaming phenolic foam heat insulation plate: under the room temperature, but with 100 parts in low-temp foaming resol, 5 parts of tensio-active agent methyl-silicone oils, 4 parts of whipping agent ammonium hydrogencarbonates, 4 parts of Skellysolve As, 8 parts of properties-correcting agent ethylene glycol, 20 parts of solid packing magnesium hydroxides, 20 parts of talcum powder, 4 parts of sodium hexametaphosphate dispersants, 10 parts of solidifying agent methylsulphonic acids, 30 parts of phosphoric acid fully mix stand-by.Simultaneously, by the good non-woven fabrics of specification requirement place mat, adjust 3 m/mins of laminating machine speed, pressure 40Kg/cm
2, the continuous foamed curing of input compound namely gets warming plate.
Embodiment 6:
A kind of preparation method of low temperature fast foaming resol warming plate is characterized in that: it may further comprise the steps makes:
(1) but, synthetic low-temp foaming resol: mol ratio 1:1.5 input phenol, the formaldehyde of in reaction vessel, press material, press 2.7% of phenol quality and add sodium hydroxide catalyst, the question response mixture is warming up to 70 ℃, insulation reaction 2 hours, then 1 hour, 80 ℃ polycondensations of 86 ℃ of polycondensations are 1 hour, be neutralized to neutrality with hydrochloric acid soln, vacuum decompression dewater to viscosity be 1000mpa.s, but make low-temp foaming resol;
(2), the preparation of low-temp foaming phenolic foam heat insulation plate: under the room temperature, but with 100 parts in low-temp foaming resol, 3 parts of tensio-active agent tween T-80,3 parts of methyl-silicone oils, 4 parts of whipping agent sodium bicarbonates, 4 parts of Skellysolve As, 5 parts of properties-correcting agent o-phthalic acid dibutyl esters, 3 parts of ethylene glycol, 20 parts in solid packing aluminium hydroxide, 30 parts of talcum powder, 2 parts of pentasodium triphosphate of dispersing agent, 3 parts of Sodium hexametaphosphate 99s, 20 parts in solidifying agent sulfuric acid, 20 parts of phosphoric acid fully mix stand-by.Simultaneously, by the good non-woven fabrics of specification requirement place mat, adjust 5 m/mins of laminating machine speed, pressure 50Kg/cm
2, the continuous foamed curing of input compound namely gets warming plate.
Claims (7)
1. the preparation method of a low temperature fast foaming phenolic foam heat insulation plate, it is characterized in that: it may further comprise the steps makes:
(1) but, synthetic low-temp foaming resol: the mol ratio 1:(1.2-1.8 that in reaction vessel, press material) add the mixing of phenol and formaldehyde, press 2.7% of phenol quality and add sodium hydroxide catalyst, the question response mixture is warming up to 60-70 ℃, be incubated 2 hours, then 86 ℃ of polycondensations 1 hour, 80 ℃ of polycondensations 1 hour are neutralized to neutrality with hydrochloric acid soln, vacuum decompression dewater to viscosity be 1000-1200mpa.s, but make low-temp foaming resol;
(2), preparation low-temp foaming phenolic foam heat insulation plate: choose in mass ratio following material: but low-temp foaming resol: 100 parts; Tensio-active agent: 4-7 parts; Whipping agent: 6-9 parts; Properties-correcting agent: 5-10 parts; Solid packing: 30-60 parts; Dispersion agent: 2-5 parts; Solidifying agent: 20-40 parts; Under the room temperature, above-mentioned raw materials is mixed fully stirring, send into fast in the laminating machine of prior placement non-woven fabrics, at pressure 30-50Kg/cm
2, 3-5 m/mins of speed condition under, solidify cutting and namely get the low-temp foaming phenolic foam heat insulation plate.
2. the preparation method of a kind of low temperature fast foaming phenolic foam heat insulation plate according to claim 1, it is characterized in that: described tensio-active agent is any one or two kinds of mixture in tween T-80 and the methyl-silicone oil.
3. the preparation method of a kind of low temperature fast foaming phenolic foam heat insulation plate according to claim 1, it is characterized in that: described whipping agent is the solidliquid mixture of ammonium hydrogencarbonate and Skellysolve A, perhaps the solidliquid mixture of sodium bicarbonate and Skellysolve A.
4. the preparation method of a kind of low temperature fast foaming phenolic foam heat insulation plate according to claim 1, it is characterized in that: described properties-correcting agent is any one or two kinds of mixture in o-phthalic acid dibutyl ester and the ethylene glycol.
5. the preparation method of a kind of low temperature fast foaming phenolic foam heat insulation plate according to claim 1, it is characterized in that: described solid packing is any one or two kinds of mixture in aluminium hydroxide, magnesium hydroxide and the talcum powder.
6. the preparation method of a kind of low temperature fast foaming phenolic foam heat insulation plate according to claim 1 is characterized in that: described dispersion agent is the mixture of any or two kinds in tripoly phosphate sodium STPP and the Sodium hexametaphosphate 99.
7. the preparation method of a kind of low temperature fast foaming phenolic foam heat insulation plate according to claim 1, it is characterized in that: described solidifying agent is any one or more mixture aqueous solution in sulfuric acid, methylsulphonic acid, phosphoric acid and the formic acid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210377017XA CN102977547A (en) | 2012-10-08 | 2012-10-08 | Low temperature rapid-foaming phenol formaldehyde foam thermal insulation board preparation method |
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| CN201210377017XA CN102977547A (en) | 2012-10-08 | 2012-10-08 | Low temperature rapid-foaming phenol formaldehyde foam thermal insulation board preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987461A (en) * | 2017-12-02 | 2018-05-04 | 范运昌 | A kind of foam heat-insulating board preparation method |
| CN110776712A (en) * | 2019-11-06 | 2020-02-11 | 徐州盛安化工科技有限公司 | Phenolic resin insulation board and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1990012058A1 (en) * | 1989-04-13 | 1990-10-18 | Nauchno-Proizvodstvennoe Obiedinenie 'polimersintez' | Method for obtaining liquid phenol-formaldehyde resin and a foam plastic based thereon |
| CN1428372A (en) * | 2001-12-26 | 2003-07-09 | 广州擎天新材料研究开发有限公司 | Phenolic foam plastic composite product and its production and forming process |
| CN101768326A (en) * | 2010-01-15 | 2010-07-07 | 上海虞城新型建材有限公司 | Preparation method of modified phenolic resin and application thereof |
| CN102443126A (en) * | 2011-09-02 | 2012-05-09 | 王博 | Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam |
-
2012
- 2012-10-08 CN CN201210377017XA patent/CN102977547A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1990012058A1 (en) * | 1989-04-13 | 1990-10-18 | Nauchno-Proizvodstvennoe Obiedinenie 'polimersintez' | Method for obtaining liquid phenol-formaldehyde resin and a foam plastic based thereon |
| CN1428372A (en) * | 2001-12-26 | 2003-07-09 | 广州擎天新材料研究开发有限公司 | Phenolic foam plastic composite product and its production and forming process |
| CN101768326A (en) * | 2010-01-15 | 2010-07-07 | 上海虞城新型建材有限公司 | Preparation method of modified phenolic resin and application thereof |
| CN102443126A (en) * | 2011-09-02 | 2012-05-09 | 王博 | Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987461A (en) * | 2017-12-02 | 2018-05-04 | 范运昌 | A kind of foam heat-insulating board preparation method |
| CN107987461B (en) * | 2017-12-02 | 2020-04-10 | 南通苏东新型外墙保温板有限公司 | Preparation method of foam insulation board |
| CN110776712A (en) * | 2019-11-06 | 2020-02-11 | 徐州盛安化工科技有限公司 | Phenolic resin insulation board and preparation method thereof |
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Application publication date: 20130320 |