CN104356592A - Phenolic foam insulation material improved by glass fiber powder and sericite - Google Patents
Phenolic foam insulation material improved by glass fiber powder and sericite Download PDFInfo
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- CN104356592A CN104356592A CN201410618365.0A CN201410618365A CN104356592A CN 104356592 A CN104356592 A CN 104356592A CN 201410618365 A CN201410618365 A CN 201410618365A CN 104356592 A CN104356592 A CN 104356592A
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Abstract
The invention relates to a phenolic foam insulation material improved by glass fiber powder and sericite. The insulation material is characterized by being mainly prepared from the following raw materials: 100 parts of phenolic resin, 2-10 parts of a phenolic resin fluidity improver, 0.5-5 parts of foam stabilizer, 1-10 parts of toughening/reinforcing agents, 6-15 parts of a foaming agent and 6-55 parts of a reactive acid curing agent. The insulation material disclosed by the invention, which adopts polyoxyethylene grafted or blocked water-based methyl silicone oil as the foam stabilizer, is delicate and uniform in foam cells, low in heat conductivity coefficient and good in insulation performance; and the insulation material, by taking the glass fiber powder and the sericite as the toughening/reinforcing agents, can be used for reducing the cost, improving the flame retardation of foam and reducing the smoke density.
Description
Technical field
The present invention relates to a kind of preparation method of phenolic aldehyde foam thermal insulation material, belong to the category of synthesized polymer material.Phenolic aldehyde foam thermal insulation material prepared by the present invention can be used for the industry heat-insulation and heat-preservations such as building exterior wall heat preserving, ventilator trunk, petrochemical pipe, electrical equipment, instrument.
Background technology
The porous plastics such as polystyrene, polyethylene, urethane, because of features such as thermal conductivity is low, lightweight, easy constructions, are used widely in fields such as external wall heat-insulation and heat-preservation, ventilator trunk, petrochemical pipe insulations.But now widely used several porous plastics also exists the shortcomings such as easy firing, the amount of being fuming is large, toxicity is high, heat resisting temperature is low as urethane, polystyrene etc., its application in external wall, marine piping, the insulation of high temperature petrochemical pipe etc. is very limited.And phenolic foamed plastics have fire resistance good, do not burn, the advantage such as the amount of being fuming is little, fire penetration resistance is good, a kind of fire prevention of excellent performance, heat insulation, sound insulation, lightweight, energy-saving material, thermal conductivity only has 0. 018 0. 042ff/mk, heat-insulating property is better than polystyrene, urethane, polyethylene etc., the lagging material that heat insulation effect is more traditional than mineral wool, jelutong bukit, perlite, glass wool etc. is high more than 1 times, have again simultaneously the foams such as polystyrene, urethane, polyethylene far away from flame retardant property.Exist in current phenolic foamed plastics production process: (1) system viscosity is large, material transfer difficulty; (2) lower boiling alkane and hydrochloric ether is used to make whipping agent, to environmental danger; (3) foam bubble hole uneven, affect heat conductivility; (4) foams toughness, intensity are low, fall slag rate high; (5) resin originating party amount is little, foam cost height more obvious than polystyrene foam, affects its spread and uses.
Summary of the invention
The present invention is directed to the preparation method that the problems referred to above disclose a kind of phenol formaldehyde foam, the present invention adopts ethylene bis stearamide (EBS) and Tegin 55G as resol fluidity improver in phenol formaldehyde foam preparation technology, reduces the viscosity of phenolic foam system; Adopt methylal Substitute For Partial lower boiling alkane and hydrochloric ether as environmentally friendly whipping agent; Polyoxyethylene grafting methyl water-based silicone oil or block type aqueous dimethylformamide silicone oil is adopted to be foam emulsion stablizer; Adopt glass fiber powder and sericite in powder and sericite in powder as toughness reinforcing, strengthen and fire retardant; Sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol and sulfonated castor oil is adopted to be reactive acid solidifying agent.The phenol formaldehyde foam prepared by present method has uniform foam cell, exquisiteness, intensity are high, good toughness, falls the features such as slag rate is low, reactive acid solidifying agent addition content is large, cost is low.Solve that phenol formaldehyde foam easily falls slag, matter is crisp, intensity is low, poor toughness, high in cost of production shortcoming, maintain again the traditional advantages such as low, the low cigarette of phenol formaldehyde foam thermal conductivity, superior flame retardant property.
Technical solution of the present invention is: the phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 2-10 part
Suds-stabilizing agent: 0.5-5 part
Toughness reinforcing, toughener: 1-10 part
Whipping agent: 6-15 part
Reactive acid solidifying agent: 6-55 part.
The described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, preferably, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 4-8 part
Suds-stabilizing agent: 2-4 part
Toughness reinforcing, toughener: 3-8 part
Whipping agent: 8-12 part
Reactive acid solidifying agent: 12-45 part.
The described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, preferably, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 6 parts
Suds-stabilizing agent: 3 parts
Toughness reinforcing, toughener: 6 parts
Whipping agent: 10 parts
Reactive acid solidifying agent: 20 parts.
The described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, preferably, described resol is common resole or Aromatic Polyester Polyols modified phenolic resins.
The described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, preferably, described resol fluidity improver is one in EBS, Tegin 55G or two kinds and above mixture.
The described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, preferably, described suds-stabilizing agent is polyoxyethylene grafting or block type aqueous dimethylformamide silicone oil.
The described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, preferably, described whipping agent is sherwood oil (30 ~ 60 ° of C), sherwood oil (60 ~ 90 ° of C), methylene dichloride and methylal two kinds and above mixture.
The described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, preferably, described reactive acid solidifying agent is sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol, the one of sulfonated castor oil or two kinds and above mixture.
The described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder, preferably, described toughness reinforcing, mixture that toughener is glass fiber powder and sericite in powder composition.Described toughness reinforcing, more preferably the mixture of 80:20-50:50 mass ratio pressed by glass fiber powder and sericite in powder to toughener.Wherein glass fiber powder specification is: particle diameter 400-800 order, water ratio <0.5%, density 2.20-2.35g/cm
3; Sericite in powder specification is: particle diameter: 400-1250 order, water ratio <0.5%, whiteness>=75%.
The preparation method of the described phenolic aldehyde foam thermal insulation material using glass fiber powder and sericite in powder to improve, first resol and suds-stabilizing agent, resol fluidity improver, toughness reinforcing, toughener high-speed stirring are mixed, and then it is even to add whipping agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 60-70 ° of C baking oven, be incubated foaming in 6-12 hour, slaking 24 hours, the demoulding, obtain product.
The present invention relates to a kind of preparation method of modified phenolic foam lagging material.The present invention adopts ethylene bis stearamide (EBS) and Tegin 55G as resol fluidity improver in phenol formaldehyde foam preparation technology, reduces the viscosity of phenolic foam system; Adopt methylal Substitute For Partial lower boiling alkane and hydrochloric ether as environmentally friendly whipping agent; Polyoxyethylene grafting or block type aqueous dimethylformamide silicone oil is adopted to be foam emulsion stablizer; Adopt glass fiber powder and sericite in powder as toughness reinforcing, strengthen and fire retardant; Sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol and sulfonated castor oil is adopted to be reactive acid solidifying agent.The phenol formaldehyde foam prepared by present method has uniform foam cell, exquisiteness, intensity are high, good toughness, falls the features such as slag rate is low, reactive acid solidifying agent addition content is large, cost is low.Solve that phenol formaldehyde foam easily falls slag, matter is crisp, intensity is low, poor toughness, high in cost of production shortcoming, maintain again the traditional advantages such as low, the low cigarette of phenol formaldehyde foam thermal conductivity, superior flame retardant property.
Advantage of the present invention is also embodied in:
1, adopt EBS, Tegin 55G, as internal lubricant, improves resol mobility, reduces its bulk viscosity;
2, adopt reactable acid to make solidifying agent, not only play catalysis, solidification, also become a resin body part, addition content is many simultaneously, but residual acid is few, and system acidity is little, little to materials for wall corrodibility; And cost is low, originating party amount is large;
3. methylal belongs to environmentally friendly whipping agent, as mixed foaming agent component;
4. adopt polyoxyethylene grafting or block type aqueous dimethylformamide silicone oil to be suds-stabilizing agent, the foam cell of preparation is fine and smooth evenly, thermal conductivity is little, good heat insulating;
5. adopt glass fiber powder and sericite in powder to be toughness reinforcing, toughener and foam flame retardant properties can be improved.
Embodiment
Below by embodiment, the present invention is described in further detail.
The raw materials used Aromatic Polyester Polyols modified phenolic resins of the present invention, sulfonation polyoxyethylene nonylphenol ether and sulfonation cardanol are self-control; Other raw materials all can be bought from market.
Preparation method is as follows for Aromatic Polyester Polyols modified phenolic resins:
First prepare Aromatic Polyester Polyols
:ethylene glycol, glycol ether, Triethylene glycol, dipropylene glycol, glycerine are added reactor, warming while stirring, then under agitation adds terephthalic acid, m-phthalic acid, phthalic anhydride, then titanic acid ester is added, first control at low temperatures, reaction certain hour, then raised temperature, and held for some time, cooling vacuumizes, and maintain certain hour, cooling discharge obtains product Aromatic Polyester Polyols
.
Prepare toughening modifying resol
:reactor is added after first being dissolved by phenol, add formaldehyde solution, basic catalyst stage by stage again, regulate pH=9, add triphenylphosphate or triphenyl phosphite or triphenyl borate and make resol prepolymer at a certain temperature, add the Aromatic Polyester Polyols of above-mentioned preparation again, regulate reaction solution pH=5 with formic acid, continue to react 1h at 85 DEG C-90 DEG C, add basic solution and regulate pH=7.5, make mixture be cooled to rapidly 75 DEG C with cooling bath; Decompression dehydration 1-1.5h at 75 DEG C, viscosity controller, at 20-30mPas, obtains toughening modifying resol
.
Preparation method is as follows for sulfonation polyoxyethylene nonylphenol ether:
In reaction flask, add 100 parts of polyoxyethylene nonylphenol ethers, 20 parts of Diethylene Glycols, start stirring, temperature control 20-30 DEG C under agitation slowly (in 60-90 minute) drip 60 parts of vitriol oils; Slowly heat up after adding acid 80-85 DEG C, reacts 3 hours, be cooled to 40 DEG C, then add 10 parts of Diethylene Glycols, discharging.
Preparation method is as follows for sulfonation cardanol:
In reaction flask, add 100 parts of cardanols, temperature control 20-30 DEG C, under agitation slowly (in 60 minutes) drip 50 parts of vitriol oils, slowly heat up 85 DEG C after adding acid, react 4 hours, continue reaction 3 hours after adding acid, be cooled to 40 DEG C, add 10 parts of Diethylene Glycols again, discharging.
Normal practice of the present invention: a kind of toughen and intensify type phenolic aldehyde foam thermal insulation material, is prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 2-10 part
Suds-stabilizing agent: 0.5-5 part
Toughness reinforcing, toughener: 1-10 part
Whipping agent: 6-15 part
Reactive acid solidifying agent: 6-55 part.
The preparation method of described toughen and intensify type phenolic aldehyde foam thermal insulation material, first resol and resol fluidity improver, toughness reinforcing, toughener high-speed stirring are mixed, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 60-70 ° of C baking oven, be incubated foaming in 6-12 hour, slaking 24 hours, the demoulding, obtain product.
Described resol is common resole or Aromatic Polyester Polyols modified phenolic resins.Described resol fluidity improver is one in ethylene bis stearamide, Tegin 55G or two kinds and above mixture.Described reactive acid solidifying agent is sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol, the one of sulfonated castor oil or two kinds and above mixture; Described toughness reinforcing, toughener is glass fiber powder and the sericite in powder mixture by 80:20-50:50 mass ratio.
Embodiment 1
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 65 ° of C baking ovens, be incubated foaming in 8 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 1.
Resol: 100 parts
Resol fluidity improver: 8 parts
Suds-stabilizing agent: 4 parts
Toughness reinforcing, toughener: 8 parts
Whipping agent: 12 parts
Reactive acid solidifying agent: 45 parts.
Embodiment 2
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 70 ° of C baking ovens, be incubated foaming in 8 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 2.
Aromatic Polyester Polyols modified phenolic resins: 100 parts
Resol fluidity improver: 5 parts
Suds-stabilizing agent: 2 parts
Toughness reinforcing, toughener: 1.5 parts
Mixed foaming agent: 10 parts
Reactive acid solidifying agent: 45 parts.
Embodiment 3
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 70 ° of C baking ovens, be incubated foaming in 6 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 3.
Aromatic Polyester Polyols modified phenolic resins: 100 parts
Resol fluidity improver: 4 parts
Suds-stabilizing agent: 2 parts
Toughness reinforcing, toughener: 1.5 parts
Whipping agent: 9 parts
Reactive acid solidifying agent: 35 parts.
Embodiment 4
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 70 ° of C baking ovens, be incubated foaming in 7 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 3.
Resol: 100 parts
Resol fluidity improver: 6 parts
Suds-stabilizing agent: 3 parts
Toughness reinforcing, toughener: 6 parts
Whipping agent: 10 parts
Reactive acid solidifying agent: 20 parts.
Embodiment 5
Successively resol and emulsifying agent, suds-stabilizing agent, Resin Flow improving agent, toughness reinforcing, toughener high-speed stirring are mixed by following formula, and then it is even to add composite foamable agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 70 ° of C baking ovens, be incubated foaming in 7 hours, slaking 24 hours, the demoulding, obtain phenolic foam products 3.
Resol: 100 parts
Resol fluidity improver: 5 parts
Suds-stabilizing agent: 3 parts
Whipping agent: 10 parts
Reactive acid solidifying agent: 25 parts.
Gained phenol formaldehyde foam salient features is as following table:
Can find out from upper table experimental result: it is low that phenol formaldehyde foam prepared by toughness reinforcing, the toughener that add glass fiber powder and sericite in powder composition falls slag rate, and compressive strength is high, and good toughness, thermal conductivity are little, good heat insulating.
Claims (10)
1., with the phenolic aldehyde foam thermal insulation material that glass fiber powder and sericite in powder improve, it is characterized in that, be prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 2-10 part
Suds-stabilizing agent: 0.5-5 part
Toughness reinforcing, toughener: 1-10 part
Whipping agent: 6-15 part
Reactive acid solidifying agent: 6-55 part.
2. the phenolic aldehyde foam thermal insulation material of glass fiber powder according to claim 1 and sericite in powder improvement, is characterized in that, be prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 4-8 part
Suds-stabilizing agent: 2-4 part
Toughness reinforcing, toughener: 3-8 part
Whipping agent: 8-12 part
Reactive acid solidifying agent: 12-45 part.
3. the phenolic aldehyde foam thermal insulation material of glass fiber powder according to claim 1 and sericite in powder improvement, is characterized in that, be prepared from primarily of following raw material:
Resol: 100 parts
Resol fluidity improver: 6 parts
Suds-stabilizing agent: 3 parts
Toughness reinforcing, toughener: 6 parts
Whipping agent: 10 parts
Reactive acid solidifying agent: 20 parts.
4., according to the arbitrary described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder of claim 1-3, it is characterized in that, described resol is common resole or Aromatic Polyester Polyols modified phenolic resins.
5. according to the arbitrary described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder of claim 1-3, it is characterized in that, described resol fluidity improver is one in ethylene bis stearic acid amide, Tegin 55G or two kinds and above mixture.
6., according to the arbitrary described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder of claim 1-3, it is characterized in that, described suds-stabilizing agent is polyoxyethylene grafting or block type aqueous dimethylformamide silicone oil.
7. according to the arbitrary described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder of claim 1-3, it is characterized in that, described whipping agent is sherwood oil (30 ~ 60 ° of C), sherwood oil (60 ~ 90 ° of C), methylene dichloride and methylal two kinds and above mixture.
8. according to the arbitrary described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder of claim 1-3, it is characterized in that, described reactive acid solidifying agent is sulfonation polyoxyethylene nonylphenol ether, sulfonation cardanol, the one of sulfonated castor oil or two kinds and above mixture.
9. according to the arbitrary described phenolic aldehyde foam thermal insulation material improved with glass fiber powder and sericite in powder of claim 1-3, it is characterized in that, described toughness reinforcing, toughener is glass fiber powder and sericite in powder, and by the mixture of 80:20-50:50 mass ratio, (wherein glass fiber powder specification is: particle diameter 400-800 order, water ratio <0.5%, density 2.20-2.35g/cm
3; Sericite in powder specification is: particle diameter: 400-1250 order, water ratio <0.5%, whiteness>=75%).
10. according to the preparation method of the arbitrary described phenolic aldehyde foam thermal insulation material using glass fiber powder and sericite in powder to improve of claim 1-3, it is characterized in that, first resol and suds-stabilizing agent, resol fluidity improver, toughness reinforcing, toughener high-speed stirring are mixed, and then it is even to add whipping agent powerful mixing, finally add reactive acid solidifying agent to mix, be transferred in the mould of preheating, put into 60-70 ° of C baking oven, be incubated foaming in 6-12 hour, slaking 24 hours, the demoulding, obtain product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410618365.0A CN104356592A (en) | 2014-11-06 | 2014-11-06 | Phenolic foam insulation material improved by glass fiber powder and sericite |
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|---|---|---|---|
| CN201410618365.0A CN104356592A (en) | 2014-11-06 | 2014-11-06 | Phenolic foam insulation material improved by glass fiber powder and sericite |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104785707A (en) * | 2015-04-17 | 2015-07-22 | 广西藤县通轩立信化学有限公司 | Phenolic resin for casting |
| CN106349639A (en) * | 2016-08-29 | 2017-01-25 | 广西梧州通轩林产化学有限公司 | Casting phenolic resin and preparation method thereof |
| CN106433015A (en) * | 2016-09-18 | 2017-02-22 | 安徽嘉伟新材料科技有限责任公司 | Hair-reinforced phenolic foam heat-preservation sectional material and preparing method |
| CN109651757A (en) * | 2019-01-02 | 2019-04-19 | 广东明日环保净化有限公司 | A kind of preparation method of high-performance modified phenolic resin cold-storage insulation board |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766243A (en) * | 2012-07-25 | 2012-11-07 | 胡玉 | Room-temperature foamable phenolic resin and method for preparing phenolic foams by same |
| CN103788570A (en) * | 2012-10-31 | 2014-05-14 | 合肥杰事杰新材料股份有限公司 | Modified phenolic foam and preparation method thereof |
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2014
- 2014-11-06 CN CN201410618365.0A patent/CN104356592A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766243A (en) * | 2012-07-25 | 2012-11-07 | 胡玉 | Room-temperature foamable phenolic resin and method for preparing phenolic foams by same |
| CN103788570A (en) * | 2012-10-31 | 2014-05-14 | 合肥杰事杰新材料股份有限公司 | Modified phenolic foam and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104785707A (en) * | 2015-04-17 | 2015-07-22 | 广西藤县通轩立信化学有限公司 | Phenolic resin for casting |
| CN104785707B (en) * | 2015-04-17 | 2017-05-24 | 广西藤县通轩立信化学有限公司 | phenolic resin for casting |
| CN106349639A (en) * | 2016-08-29 | 2017-01-25 | 广西梧州通轩林产化学有限公司 | Casting phenolic resin and preparation method thereof |
| CN106433015A (en) * | 2016-09-18 | 2017-02-22 | 安徽嘉伟新材料科技有限责任公司 | Hair-reinforced phenolic foam heat-preservation sectional material and preparing method |
| CN109651757A (en) * | 2019-01-02 | 2019-04-19 | 广东明日环保净化有限公司 | A kind of preparation method of high-performance modified phenolic resin cold-storage insulation board |
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