CN104559044A - Non-corrosive, low-density and high-strength phenolic foam - Google Patents
Non-corrosive, low-density and high-strength phenolic foam Download PDFInfo
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- CN104559044A CN104559044A CN201410842031.1A CN201410842031A CN104559044A CN 104559044 A CN104559044 A CN 104559044A CN 201410842031 A CN201410842031 A CN 201410842031A CN 104559044 A CN104559044 A CN 104559044A
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Abstract
The invention discloses non-corrosive, low-density and high-strength phenolic foam. The phenolic foam is prepared from expendable phenolic resin, a surfactant, a foaming agent, a curing agent and a flame retardant in the mass ratio of 100:(1-10):(1-10):(3-10):(1-10) through foaming and solidification at the temperature of 100-140 DEG C, wherein the used curing agent is a mixture of an organic acid and an inorganic acid in the mass ratio of 1:1, the foaming agent is ammonium carbonate, ammonium hydrogen carbonate or calcium carbonate with particle sizes smaller than or equal to 50 mu m, and the curing agent and the foaming agent have the synergistic effect, so that resin foaming and cross-linking curing are conducted synchronously, and the phenolic foam with the weakly acidic surface is formed; the phenolic foam has low-density and high-strength properties without any toughening agents, so that the flame retardance and the thermal stability of a material are guaranteed; meanwhile, the phenolic foam has the advantages that the consumed time of a preparation method is short, and the phenolic foam is low in cost, non-corrosive, low in environment pollution and the like.
Description
Technical field
The present invention is specifically related to a kind of corrosion-free low-density and high-strength phenol formaldehyde foam.
Background technology
Phenolic foam material is a kind of heat insulating material, it has the excellent feature such as heat-resisting heat insulating ability, flame retardant resistance, fire-resistance flame penetrativity, the low cigarette of low toxicity, performance is obviously better than polyethylene, polystyrene foam and polyurethane foam, is the porous plastics uniquely reaching fire prevention to high buildings standard.In recent years, China's fire disaster accident frequently occurs, and adopting the phenol formaldehyde foam of excellent fireproof performance to replace other inflammable foam, is the great demand of the development of the national economy.The heat preservation fireproofing material that some large public buildings etc. are badly in need of, as: material of construction, piping insulation, and the heat-insulating heat-preserving material etc. that ocean-going freighter, van container and passenger car etc. use, for phenolic foamed plastics brings wide market outlook.
Phenol formaldehyde foam generally adopts physical blowing method to be prepared from, by expandable phenolic resin, tensio-active agent, whipping agent, solidifying agent foamed solidification at 60 ~ 80 DEG C, whipping agent wherein used is methylene dichloride, Skellysolve A etc., and solidifying agent is organic acid (toluene sulfonic acide, Phenylsulfonic acid etc.) and mineral acid (sulfuric acid, hydrochloric acid, phosphoric acid etc.).At present, the main drawback of phenol formaldehyde foam is that intensity is subject to the impact of unit weight very large, the intensity of low unit weight goods is low, fragility large, easily efflorescence, existing method mainly through increase hardener dose and adopt toughening agent modified expandable phenolic resin improve phenol formaldehyde foam intensity, reduce and fall slag rate, make the uniform foam cell of phenol formaldehyde foam fine and smooth simultaneously.Be 100 mass parts in expandable phenolic resin, the addition of solidifying agent is generally 20 ~ 50 parts, and this makes gained phenol formaldehyde foam acidity stronger, and easily produces during metallic contact that acid is permeated, acid corrosion, makes its range of application limited; And most of toughner is all combustible material, modified phenol formaldehyde foam flame retardant properties and thermal stability is caused to decline.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned phenol formaldehyde foam Problems existing, provides a kind of surface in slightly acidic, is not adding under any toughner condition, the low density of flame retardant resistance and Heat stability is good, the phenol formaldehyde foam of high strength simultaneously.
Solving the problems of the technologies described above adopted technical scheme is: this phenol formaldehyde foam is 100:(1 ~ 10 by expandable phenolic resin, tensio-active agent, whipping agent, solidifying agent, fire retardant in mass ratio): (1 ~ 10): (3 ~ 10): (1 ~ 10), is prepared from 100 ~ 140 DEG C of foamed solidifications.
Phenol formaldehyde foam of the present invention is preferably 100:(1 ~ 5 by expandable phenolic resin, tensio-active agent, whipping agent, solidifying agent, fire retardant in mass ratio): (4 ~ 10): (5 ~ 10): (2 ~ 8), are prepared from 100 ~ 140 DEG C of foamed solidifications for 10 minutes.
Phenol formaldehyde foam of the present invention is best is 100:2:6:6:8 by expandable phenolic resin, tensio-active agent, whipping agent, solidifying agent, fire retardant in mass ratio, within 10 minutes, is prepared from 140 DEG C of foamed solidifications.
The viscosity of above-mentioned expandable phenolic resin is 3000 ~ 5000mPas, and it is be prepared from phenol and formaldehyde through polycondensation in the KOH aqueous solution of 50% at massfraction; Solidifying agent is the mass ratio of organic acid and mineral acid is the mixture of 1:1, wherein said mineral acid is any one in sulfuric acid, hydrochloric acid, phosphoric acid, preferred hydrochloric acid, organic acid is any one in oxalic acid, benzene nitric acid, toluene sulfonic acide, Phenylsulfonic acid, naphthene sulfonic acid, preferable methyl Phenylsulfonic acid or Phenylsulfonic acid; Whipping agent is any one in the volatile salt of granularity≤50 μm, bicarbonate of ammonia, calcium carbonate, preferred calcium carbonate; Tensio-active agent is any one in tween-80, polyoxyethylene nonylphenol ether NP-15, polyoxyethylene fatty acid ester A-115, fatty alcohol-polyoxyethylene ether AEO-7, epoxy castor oil.
Beneficial effect of the present invention is as follows:
1, the present invention with mineral acid and organic acid mixing acid for solidifying agent, with calcium carbonate, volatile salt, bicarbonate of ammonia for whipping agent, adopt high temperature foam process, by the synergy between solidifying agent and whipping agent, make resin expandedly synchronously to carry out with crosslinking curing, form surface in weakly acidic phenol formaldehyde foam.
2, the present invention is under the condition of not adding any toughner, has prepared low density, high intensity and high performance phenol formaldehyde foam, ensure that flame retardant resistance and the thermostability of material.
3, the present invention is compared with existing phenol formaldehyde foam, have preparation method consuming time short, cost is low, non-corrosiveness and the advantage such as environmental pollution is little, can be used for the phenol formaldehyde foam preparing high-intensity performance.
Accompanying drawing explanation
Fig. 1 is the photo of phenol formaldehyde foam prepared by embodiment 1.
Fig. 2 is the photo of phenol formaldehyde foam prepared by comparative example 1.
Fig. 3 is the photo of phenol formaldehyde foam prepared by comparative example 2.
Fig. 4 is the photo of phenol formaldehyde foam prepared by embodiment 2.
Embodiment
Below in conjunction with embodiment, the present invention is described in more detail, but protection scope of the present invention is not limited only to these embodiments.
Expandable phenolic resin in following embodiment prepares as follows:
Be the formaldehyde solution of 37% by 94.11g phenol, 178.55g massfraction, 28.1g massfraction be 50% the KOH aqueous solution add in 500mL there-necked flask, wherein the mol ratio of phenol and formaldehyde, KOH is 1:2.2:0.25,90 DEG C are warming up to the temperature rate of 1 DEG C/min, isothermal reaction 120 minutes, then underpressure distillation under-0.09MPa, obtain expandable phenolic resin, testing its viscosity according to GB/T 6680-2003 " measuring method of sizing agent viscosity " is 4000mPas.
The performance test methods of the phenol formaldehyde foam in following embodiment is as follows:
1, flexural strength is tested according to GB/T 8812.2-2007 " mensuration of rigid foam bending property " method.
2, compressive strength is tested according to GB/T 8813-2008 " mensuration of rigid foam compression performance " method.
3, apparent density is according to the test of GB/T 6343-1995 " mensuration of porous plastics and rubber apparent density " method, and according to formula ρ=m/V × 10
6calculate the apparent density of phenol formaldehyde foam, unit is kg/m
3.
4, apparent pH is tested according to GB/T 13528-1992 " assay method of paper and paperboard surface pH value " method.
5, slag rate is fallen according to the test of GB/T 12812-1991 " rigid foam rolling wear test " method, and according to formula f=(m
1-m
2)/m
1× 100% calculate phenol formaldehyde foam fall slag rate; Wherein m
1for testing the quality of front sample, unit is g; m
2for testing the quality of rear sample, unit is g.
Embodiment 1
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 2g polyoxyethylene nonylphenol ether NP-15,6g calcium carbonate, 3g massfraction be 85% phosphate aqueous solution, 3g Phenylsulfonic acid, 8g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 140 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam (see Fig. 1), its flexural strength is 1.7MPa, and compressive strength is 0.256MPa, and apparent density is 43.26kg/m
3, surface pH value is 6.2, and falling slag rate is 5.0%.
Comparative example 1
In embodiment 1, the Skellysolve A of the quality such as calcium carbonate use used is replaced, and other steps are identical with embodiment 1, obtain phenol formaldehyde foam (see Fig. 2), and its flexural strength is 6.1MPa, and compressive strength is 0.335MPa, and apparent density is 119.49kg/m
3, surface p H is 4.5, and falling slag rate becomes 5.6%.
Comparative example 2
In embodiment 1,80 DEG C of foamed solidifications 30 minutes, other steps are identical with embodiment 1, obtain phenol formaldehyde foam (see Fig. 3), and its flexural strength is 3.2MPa, and compressive strength is 0.337MPa, and apparent density is 98.93kg/m
3, surface p H is 4.3, and falling slag rate becomes 8.9%.
Embodiment 2
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 2g polyoxyethylene nonylphenol ether NP-15,6g calcium carbonate, 3g massfraction be 85% phosphate aqueous solution, 3g Phenylsulfonic acid, 8g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 100 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam (see Fig. 4), its flexural strength is 1.4MPa, and compressive strength is 0.154MPa, and apparent density is 42.15kg/m
3, surface p H is 5.9, and falling slag rate is 6.4%.
Embodiment 3
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 5g polyoxyethylene nonylphenol ether NP-15,4g calcium carbonate, 1.5g massfraction be 85% phosphate aqueous solution, 1.5g Phenylsulfonic acid, 10g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 140 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam, its flexural strength is 1.6MPa, and compressive strength is 0.215MPa, and apparent density is 50.45kg/m
3, surface p H is 5.9, and falling slag rate becomes 5.3%.
Embodiment 4
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 1g polyoxyethylene nonylphenol ether NP-15,10g calcium carbonate, 5g massfraction be 85% phosphate aqueous solution, 5g Phenylsulfonic acid, 2g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 140 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam, its flexural strength is 1.8MPa, and compressive strength is 0.282MPa, and apparent density is 56.57kg/m
3, surface p H is 5.6, and falling slag rate becomes 6.5%.
Embodiment 5
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 10g polyoxyethylene nonylphenol ether NP-15,1g calcium carbonate, 2.5g massfraction be 85% phosphate aqueous solution, 2.5g Phenylsulfonic acid, 1g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 140 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam, its flexural strength is 1.8MPa, and compressive strength is 0.228MPa, and apparent density is 50.25kg/m
3, surface p H is 6.2, and falling slag rate becomes 6.5%.
Embodiment 6
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 2g tween-80,6g bicarbonate of ammonia, 3g massfraction be 36% aqueous hydrochloric acid, 3g benzene nitric acid, 8g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 140 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam, its flexural strength is 1.6MPa, and compressive strength is 0.212MPa, and apparent density is 46.58kg/m
3, surface p H is 5.6, and falling slag rate becomes 6.5%.
Embodiment 7
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 2g epoxy castor oil, 6g volatile salt, 3g massfraction be 85% phosphate aqueous solution, 3g naphthene sulfonic acid, 8g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 140 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam, its flexural strength is 1.5MPa, and compressive strength is 0.176MPa, and apparent density is 62.45kg/m
3, surface p H is 5.6, and falling slag rate becomes 6.4%.
Embodiment 8
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 2g fatty alcohol-polyoxyethylene ether AEO-7,2g calcium carbonate, 3g massfraction be 50% aqueous sulfuric acid, 3g toluene sulfonic acide, 8g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 140 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam, its flexural strength is 1.5MPa, and compressive strength is 0.161MPa, and apparent density is 45.34kg/m
3, surface p H is 5.8, and falling slag rate becomes 5.2%.
Embodiment 9
Be the expandable phenolic resin of 4000mPas by 100g viscosity, 2g polyoxyethylene fatty acid ester A-115,6g volatile salt, 3g massfraction be 50% aqueous sulfuric acid, 3g oxalic acid, 8g aluminium hydroxide add beaker, stir, pour mould into, foamed solidification 10 minutes at 140 DEG C, obtain corrosion-free low-density and high-strength phenol formaldehyde foam, its flexural strength is 1.8MPa, and compressive strength is 0.252MPa, and apparent density is 52.34kg/m
3, surface p H is 5.8, and falling slag rate becomes 5.2%.
Claims (5)
1. a corrosion-free low-density and high-strength phenol formaldehyde foam, it is characterized in that: this phenol formaldehyde foam is 100:(1 ~ 10 by expandable phenolic resin, tensio-active agent, whipping agent, solidifying agent, fire retardant in mass ratio): (1 ~ 10): (3 ~ 10): (1 ~ 10), is prepared from 100 ~ 140 DEG C of foamed solidifications;
The viscosity of above-mentioned expandable phenolic resin is 3000 ~ 5000mPas, and it is be prepared from phenol and formaldehyde through polycondensation in the KOH aqueous solution of 50% at massfraction; Solidifying agent is the mass ratio of organic acid and mineral acid is the mixture of 1:1, and wherein said mineral acid is any one in sulfuric acid, hydrochloric acid, phosphoric acid, and organic acid is any one in oxalic acid, benzene nitric acid, toluene sulfonic acide, Phenylsulfonic acid, naphthene sulfonic acid; Whipping agent is any one in the volatile salt of granularity≤50 μm, bicarbonate of ammonia, calcium carbonate; Tensio-active agent is any one in tween-80, polyoxyethylene nonylphenol ether NP-15, polyoxyethylene fatty acid ester A-115, fatty alcohol-polyoxyethylene ether AEO-7, epoxy castor oil.
2. corrosion-free low-density and high-strength phenol formaldehyde foam according to claim 1, it is characterized in that: this phenol formaldehyde foam is 100:(1 ~ 5 by expandable phenolic resin, tensio-active agent, whipping agent, solidifying agent, fire retardant in mass ratio): (4 ~ 10): (5 ~ 10): (2 ~ 8), are prepared from 100 ~ 140 DEG C of foamed solidifications for 10 minutes.
3. corrosion-free low-density and high-strength phenol formaldehyde foam according to claim 1, it is characterized in that: this phenol formaldehyde foam is 100:2:6:6:8 by expandable phenolic resin, tensio-active agent, whipping agent, solidifying agent, fire retardant in mass ratio, within 10 minutes, is prepared from 140 DEG C of foamed solidifications.
4. the corrosion-free low-density and high-strength phenol formaldehyde foam according to claims 1 to 3 any one, is characterized in that: described mineral acid is hydrochloric acid, and organic acid is toluene sulfonic acide or Phenylsulfonic acid.
5. corrosion-free low-density and high-strength phenol formaldehyde foam according to claim 4, is characterized in that: described whipping agent is calcium carbonate.
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| CN201410842031.1A CN104559044A (en) | 2014-12-30 | 2014-12-30 | Non-corrosive, low-density and high-strength phenolic foam |
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| CN201410842031.1A CN104559044A (en) | 2014-12-30 | 2014-12-30 | Non-corrosive, low-density and high-strength phenolic foam |
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Cited By (3)
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| CN107089927A (en) * | 2016-06-02 | 2017-08-25 | 山东理工大学 | With being used as CO2The organic amine salt compounds and its purposes as foaming agent of the anion of donor |
| WO2017206693A1 (en) * | 2016-06-02 | 2017-12-07 | 山东理工大学 | Organic amine salt compound having anions serving as co2 donors and application of same as foaming agent |
| CN108239369A (en) * | 2016-12-27 | 2018-07-03 | 龙岩紫荆创新研究院 | A kind of neutrality phenolic foam and preparation method thereof |
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| CN107089927B (en) * | 2016-06-02 | 2017-11-21 | 山东理工大学 | With as CO2The organic amine salt compounds of the anion of donor and its purposes as foaming agent |
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| RU2708457C1 (en) * | 2016-06-02 | 2019-12-09 | Шаньдун Юниверсити Оф Текнолоджи | Compound with an organic amine salt, having an anion as a co2 donor, and its use as a foaming agent |
| RU2716711C1 (en) * | 2016-06-02 | 2020-03-16 | Шаньдун Юниверсити Оф Текнолоджи | Compound with organic amine salt, having anion as co2 donor and use thereof as foaming agent |
| US11261153B2 (en) | 2016-06-02 | 2022-03-01 | Shandong University Of Technology | Organic amine salt compounds having CO2-donating anions and their use as foaming agent |
| CN108239369A (en) * | 2016-12-27 | 2018-07-03 | 龙岩紫荆创新研究院 | A kind of neutrality phenolic foam and preparation method thereof |
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