CN102863706A - Polystyrene/thermosetting resin syntactic foam and method for preparing same - Google Patents
Polystyrene/thermosetting resin syntactic foam and method for preparing same Download PDFInfo
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- CN102863706A CN102863706A CN2012103110593A CN201210311059A CN102863706A CN 102863706 A CN102863706 A CN 102863706A CN 2012103110593 A CN2012103110593 A CN 2012103110593A CN 201210311059 A CN201210311059 A CN 201210311059A CN 102863706 A CN102863706 A CN 102863706A
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Abstract
The invention discloses polystyrene/thermosetting resin syntactic foam and a method for preparing the same, and belongs to the field of flame retardant materials. The formula of the syntactic foam comprises expandable polystyrene, resin monomers or prepolymers and a curing agent. The invention also discloses a method for preparing the syntactic foam. The preparation method comprises the following steps of: pre-foaming the expandable polystyrene particles to obtain polystyrene beads; and uniformly coating the polystyrene beads with the curing agent-contained resin monomers or prepolymers, and curing the polystyrene beads to obtain the syntactic foam. The syntactic foam can fundamentally solve the problem that the polystyrene is combusted and drips, has a high flame retardant property, and is low in cost and excellent in performance, so that the syntactic foam becomes a new selection for exterior wall heat-insulating materials.
Description
Technical field
The present invention relates to a kind of polystyrene/thermosetting resin syntactic foam and preparation method thereof, belong to the fire retardant material field.
Background technology
Polystyrene foamed plastics is take polystyrene resin as main body, and the additives such as adding whipping agent are made, and it is to use at present maximum a kind of cushioning materials.It has unicellular structure, and water-absorbent is little, and good water resisting property is arranged; Density is little, is generally 0.015~0.03; Physical strength is good, and shock-absorbing capacity is excellent; Processibility is good, is easy to molded; Tint permanence is good, and thermal adaptability is strong, the advantages such as radioresistance excellence, and also dimensional precision is high, even structure.In addition, polystyrene foamed plastics is inexpensive, is the external-wall heat-insulation material of present global usage quantity maximum.
But polystyrene foamed plastics very easily burns, and burning produces a large amount of dense smokes, and drippage when burning easily, accelerates fire spread, brings very big hidden danger to security against fire.Therefore, improve the combustibility of polystyrene foamed plastics, improve the security of polystyrene foamed plastics, become in the industry study hotspot and emphasis.
At present, the flame resistant method of polystyrene foamed plastics mainly comprises two large classes: the one, and adopt the way of adding fire retardant to realize that the method is comparatively simple and practical; The 2nd, with flame-retardant monomer and styrene copolymerizedly obtain intrinsically flame retarded polystyrene, directly foaming or obtain with the polystyrene blend foaming, the method technique is comparatively complicated, and majority only rests on the scientific research stage.
As at first proposing the method that preparation contains the polystyrene foamed plastics (EPS) of graphite granule among patent US6130265, the US6340713, described EPS has self-extinguishing, can be by the B2 level of DIN4102 combustion test.Patent US6444714 has introduced the method for preparing Halogen EPS, and the EPS that obtains can reach DIN4102 combustion test B1 or B2 level.In addition, point out in the US Patent No. 6420442 that it is 20 ~ 200kg/m that the composite use of 1% ~ 12% expanded graphite and phosphorus flame retardant (red phosphorus or triphenylphosphate) can obtain density
3The fire-retardant EPS of self-extinguishing type.The combustibility of the equal p-poly-phenyl vinylic foam of aforesaid method has larger improvement, has improved the fire safety performance, but all is difficult to solve the drippage problem of polystyrene foamed plastics.Recently, Pekinese's external wall energy-saving lagging material forecloses polystyrene foamed plastics, and reason can produce molten drop when burning because of it exactly, and the polystyrene foamed plastics industrial chain faces the industry crisis.
Summary of the invention
Drippage problem when burning for solving polystyrene foamed plastics, and effectively improve its flame retardant properties, the object of the present invention is to provide a kind of polystyrene/thermosetting resin syntactic foam.
The present invention also provides the preparation method of described polystyrene/thermosetting resin syntactic foam.By Expandable Polystyrene (EPS) and thermosetting resin is compound, solve the burning drippage problem of polystyrene foamed plastics, and by adding the way of fire retardant, further improve the combustionproperty of syntactic foam.
The present invention is realized by following technical proposals.
A kind of polystyrene/thermosetting resin syntactic foam, described syntactic foam comprises polystyrene and thermosetting resin, it is as follows to fill a prescription:
Expandable Polystyrene (EPS) 20 ~ 90 weight parts;
Resin monomer or prepolymer 10 ~ 70 weight parts;
Solidifying agent;
Wherein, resin monomer or prepolymer are that 10 ~ 70 weight parts refer to that the solid content in resin monomer or the prepolymer is 10 ~ 70 weight parts.
The selection of solidifying agent and consumption are determined according to the kind of used resin, for the routine of field of polymer technology is selected, such as solidifying agent dilute hydrochloric acid, the dilute sulphuric acid of melmac; The solidifying agent dilute hydrochloric acid of urea-formaldehyde resin, dilute sulphuric acid; The solidifying agent vitriol oil of heat-reactive phenolic resin, toluene sulfonic acide, boric acid; The solidifying agent urotropine of novolac resin; The solidifying agent Tetra hydro Phthalic anhydride of Resins, epoxy, mphenylenediamine;
Also contain auxiliary agent in the prescription of preferred described syntactic foam, described auxiliary agent comprises tensio-active agent (such as tween 80), whipping agent (being used for resol, such as pentamethylene, Skellysolve A, iso-pentane, 141b(one fluorine ethylene dichloride)) and/or fire retardant (such as hexabromocyclododecane, decabromodiphynly oxide, phosphoric acid ester, expanded graphite or triethyl phosphate).
Preferred described resin is in Resins, epoxy, resol, urea-formaldehyde resin, the melmac one or more.
Preferred described Resins, epoxy is in bisphenol f type epoxy resin, tetrabromo-bisphenol type Resins, epoxy, the bisphenol-s epoxy resin one or more.
Preferred described resol is in heat-reactive phenolic resin, novolac resin, the modified phenolic resins one or more.
Preferred described resin monomer or prepolymer are: one or more in epoxy monomer, urea-formaldehyde resin prepolymer, melmac prepolymer, the resol prepolymer.
The preparation method of a kind of polystyrene of the present invention/thermosetting resin syntactic foam, described method steps is as follows:
(1) with after the expandable polystyrene particle pre-frothing, obtains polystyrene bead;
(2) in resin monomer or prepolymer, add solidifying agent, obtain mixture A after mixing;
(3) with after even coating of described polystyrene bead usefulness usefulness mixture A, carry out slaking, obtain polystyrene of the present invention/thermosetting resin syntactic foam.Wherein the preparation method of the monomer of resin or prepolymer is the routine techniques of polymeric material field.
The diameter of styrene beads is 1 ~ 10mm described in the preferred steps (1);
Pre-expansion time is 5 ~ 30min in the preferred steps (1), and temperature is 70 ~ 140 ℃; The curing time is 0 ~ 30min in the step (3), and temperature is 80 ~ 180 ℃.
Preferred described urea-formaldehyde resin prepolymer is obtained at 50 ~ 90 ℃, pH=7.5 ~ 10 time stirring reaction 1 ~ 6h by urea and formaldehyde, and the mol ratio of urea and formaldehyde is 1.5 ~ 4.0:1.
Preferred described melmac prepolymer is obtained at 60 ~ 90 ℃, pH=7.5 ~ 10 time stirring reaction 1 ~ 5h by trimeric cyanamide and formaldehyde, and the mol ratio of trimeric cyanamide and formaldehyde is 2.0 ~ 4.0:1.
The resol prepolymer comprises thermoplasticity and heat-reactive phenolic resin prepolymer, preferred heat-reactive phenolic resin prepolymer wherein, and stirring reaction 1 ~ 6h under 70 ~ 110 ℃, alkaline condition obtains by formaldehyde and phenol, and the mol ratio of formaldehyde and phenol is 1 ~ 2.0:1; The novolac resin prepolymer, stirring reaction 1 ~ 6h under 70 ~ 140 ℃, acidic conditions obtains by formaldehyde and phenol, and the mol ratio of formaldehyde and phenol is 0.5 ~ 1:1.After wherein the novolac resin prepolymer adds solidifying agent, with polystyrene bead blend slaking, can change thermosetting resin into.
Beneficial effect
1. the invention provides a kind of polystyrene/thermosetting resin syntactic foam, described syntactic foam has fundamentally solved the burning drippage of polystyrene.
2. described syntactic foam has higher flame retardant properties, and with low cost, excellent performance is for external-wall heat-insulation material provides new selection.
Embodiment
Below by embodiment, the invention will be further described.Expandable polystyrene particle among the embodiment 1 ~ 7 is the Dalian petrochemical iy produced.
Embodiment 1
(trade mark is R433, and particle diameter is 0.85 ~ 1.40mm), at 80 ℃ of lower pre-frothing 25min, obtains the polystyrene bead that particle diameter is 5 ~ 8mm with universal expandable polystyrene particle.
Formaldehyde solution and the 50mL distilled water of 40g trimeric cyanamide, 60mL 38wt% are added in the there-necked flask, and transferring pH with trolamine is 8 ~ 9, at 70 ℃ of lower reaction 1h, obtains sticky transparent melamine pre-polymer solution, and the solid content of described melamine pre-polymer solution is 43wt%.
Take by weighing above-mentioned melmac prepolymer 30g, regulate pH to 6 with dilute hydrochloric acid, join in the above-mentioned polystyrene bead of 100g that (described polystyrene quality change before and after pre-frothing is very little, can think that the quality of polystyrene bead is the quality of expandable polystyrene particle), join behind the mixing in the mould of 100mm * 100mm * 200mm and fill up compacting, at 110 ℃ of lower slaking 10min, namely get polystyrene/melmac syntactic foam, without drippage, limiting oxygen index(LOI) is 21.1% during described syntactic foam burning.
Embodiment 2
(trade mark F403, particle diameter 0.85 ~ 1.40mm) obtains the polystyrene bead that particle diameter is 5 ~ 7mm at 120 ℃ of lower pre-frothing 5min with fire-retarding foamable polystyrene grain.
18g urea, 60mL 38wt% formaldehyde solution are added in the there-necked flask, and transferring pH with trolamine is 8 ~ 9, at 70 ℃ of lower reaction 2h, gets sticky transparent melamine pre-polymer solution, and the solid content of described melamine pre-polymer solution is 53wt%.
Take by weighing above-mentioned urea-formaldehyde resin prepolymer 50g, regulate pH to 6 ~ 6.5 with dilute hydrochloric acid, join in the above-mentioned polystyrene bead of 50g, join behind the mixing in the mould of 100mm * 100mm * 100mm and fill up compacting, at 160 ℃ of lower slaking 5min, namely get polystyrene/urea-formaldehyde resin syntactic foam, without drippage, limiting oxygen index(LOI) is 26.6% during described syntactic foam burning.
Embodiment 3
(trade mark R436, particle diameter 0.4 ~ 0.7mm) obtain the polystyrene bead of particle diameter 3 ~ 5mm at 110 ℃ of lower pre-frothing 15min with universal expandable polystyrene particle.
Take by weighing the formaldehyde solution 130g of 38wt%, be preheated to 70 ℃ phenol 100g, zinc acetate 1.2g, 30% sodium hydroxide solution 3.5g places in the middle of the 500ml there-necked flask, is warming up to 95 ℃ of reaction 2.5h, be cooled to subsequently 55 ℃, steam except moisture content with pump vacuum, obtain the thermosetting phenolic prepolymer, the solid content of described thermosetting phenolic prepolymer is 90wt%.
Take by weighing above-mentioned heat-reactive phenolic resin prepolymer 70g, add the sulphuric acid soln of 2g 50wt% as solidifying agent, join behind the stirring and evenly mixing in the above-mentioned polystyrene bead of 30g, being added in the mould of 100mm * 100mm * 50mm compacting behind the mixing fills up, at 80 ℃ of lower slaking 30min, namely get the polystyrene/phenolic resin composite porous plastics, without drippage, limiting oxygen index(LOI) is 27.8% during described syntactic foam burning.
Embodiment 4
(trade mark F403, particle diameter 0.85 ~ 1.40mm) obtains the polystyrene bead that particle diameter is 5 ~ 7mm at 100 ℃ of lower pre-frothing 15min with fire-retarding foamable polystyrene grain.
40g trimeric cyanamide, 60mL 38% formaldehyde solution and 50mL distilled water are added in the there-necked flask, and transferring pH with trolamine is 8 ~ 9, at 70 ℃ of lower reaction 1h, gets sticky transparent melamine pre-polymer solution, and the solid content of described melamine pre-polymer solution is 43wt%.
Take by weighing above-mentioned melmac prepolymer 50g, regulate pH to 6 with dilute hydrochloric acid, add again triethyl phosphate fire retardant 20g, then join in the above-mentioned polystyrene bead of 50g, being added to behind the mixing in the withstand voltage mould of 100mm * 100mm * 100mm, is the water vapour foaming slaking 10s of 4kg with pressure, namely gets polystyrene/melmac syntactic foam, without drippage, limiting oxygen index(LOI) is 32.1% during described syntactic foam burning.
Embodiment 5
(trade mark R436, particle diameter 0.4 ~ 0.7mm) obtains the polystyrene bead that particle diameter is 1 ~ 5mm at 110 ℃ of lower pre-frothing 15min with universal expandable polystyrene particle.
40g trimeric cyanamide, 60mL 38% formaldehyde solution and 50mL distilled water are added in the there-necked flask, and transferring pH with trolamine is 8 ~ 9, at 70 ℃ of lower reaction 1h, gets sticky transparent melamine pre-polymer solution, and the solid content of described melamine pre-polymer solution is 43wt%.
Take by weighing melmac prepolymer 40g, regulate pH to 6 with dilute sulphuric acid, adding whipping agent pentamethylene 3g stirs evenly, join in the above-mentioned polystyrene bead of 100g, be added to behind the mixing in the mould of 100mm * 100mm * 200mm, at 100 ℃ of lower foaming slaking 20min, namely get polystyrene/melmac syntactic foam, without drippage, limiting oxygen index(LOI) is 23.5% during described syntactic foam burning.
Embodiment 6
(trade mark R433, particle diameter 0.85 ~ 1.40mm) obtains the polystyrene bead that particle diameter is 5 ~ 8mm at 80 ℃ of lower pre-frothing 25min with universal expandable polystyrene particle.
Heat-obtaining plasticity resol prepolymer (trade mark 2132, prosperous anti-material is melted in the Xinxiang City) 60g, urotropine 6g are dissolved in the 40ml dehydrated alcohol, get the novolac resin ethanolic soln, and the solid content of described novolac resin ethanolic soln is 65wt%.
Take by weighing above-mentioned novolac resin ethanolic soln 17g, join in the above-mentioned polystyrene bead of 90g, carry out air-dry behind the mixing, be added to subsequently in the withstand voltage mould of 100mm * 100mm * 200mm, be the water vapour foaming slaking 15s of 4kg with pressure, namely get polystyrene/melmac syntactic foam, without drippage, limiting oxygen index(LOI) is 23.4% during described syntactic foam burning.
Embodiment 7
(trade mark R436, particle diameter 0.4 ~ 0.7mm) obtains the polystyrene bead that particle diameter is 2 ~ 5mm at 110 ℃ of lower pre-frothing 15min with universal expandable polystyrene particle.
Take by weighing tetrabromo bisphenol-a epoxy resin (Hunan Jia Shengde, trade mark BE5400) 65g, solidifying agent mphenylenediamine 5g, triethyl phosphate 10g, join after the mixing and stirring in the above-mentioned polystyrene bead of 20g, be added to behind the mixing in the withstand voltage mould of 100mm * 100mm * 50mm, be the water vapour foaming slaking 20s of 3kg with pressure, namely get polystyrene/Resins, epoxy syntactic foam, without drippage, limiting oxygen index(LOI) is 31.3% during described syntactic foam burning.
Embodiment 8
(trade mark R433, particle diameter 0.85 ~ 1.40mm) obtains the polystyrene bead that particle diameter is 5 ~ 8mm at 80 ℃ of lower pre-frothing 25min with universal expandable polystyrene particle.
40g trimeric cyanamide, 60mL 38wt% formaldehyde solution and 50mL distilled water are added in the there-necked flask, and transferring pH with trolamine is 8 ~ 9, at 70 ℃ of lower reaction 1h, gets sticky transparent melamine pre-polymer solution, and the solid content of described melamine pre-polymer solution is 43wt%.
18g urea, 60mL 38wt% formaldehyde solution are added in the there-necked flask, and transferring pH with trolamine is 8 ~ 9, at 70 ℃ of lower reaction 2h, gets sticky transparent urea-formaldehyde resin pre-polymer solution, and the solid content of described urea-formaldehyde resin pre-polymer solution is 53wt%.
Take by weighing above-mentioned melmac prepolymer 20g, urea-formaldehyde resin prepolymer 20g, regulate pH to 6 with dilute hydrochloric acid behind the mixing, join in the above-mentioned polystyrene bead of 100g, behind its mixing, be added in 100mm * 100mm * 200mm mould and fill up compacting, at 100 ℃ of lower slaking 15min, namely get polystyrene/melamine/urea-formaldehyde resin syntactic foam, without drippage, limiting oxygen index(LOI) is 23.8% during described syntactic foam burning.
In sum, more than be preferred embodiment of the present invention only, be not for limiting protection scope of the present invention.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. polystyrene/thermosetting resin syntactic foam, it is characterized in that: described syntactic foam comprises polystyrene and thermosetting resin, it is as follows to fill a prescription:
Expandable Polystyrene (EPS) 20 ~ 90 weight parts;
Resin monomer or prepolymer 10 ~ 70 weight parts;
Solidifying agent.
2. a kind of polystyrene according to claim 1/thermosetting resin syntactic foam, it is characterized in that: contain auxiliary agent in the prescription of described syntactic foam, described auxiliary agent comprises tensio-active agent, whipping agent and/or fire retardant.
3. a kind of polystyrene according to claim 1 and 2/thermosetting resin syntactic foam is characterized in that: described resin is in Resins, epoxy, resol, urea-formaldehyde resin, the melmac one or more.
4. a kind of polystyrene according to claim 1 and 2/thermosetting resin syntactic foam, it is characterized in that: described Resins, epoxy is in bisphenol f type epoxy resin, tetrabromo-bisphenol type Resins, epoxy, the bisphenol-s epoxy resin one or more.
5. a kind of polystyrene according to claim 1 and 2/thermosetting resin syntactic foam is characterized in that: described resol is in heat-reactive phenolic resin, novolac resin, the modified phenolic resins one or more.
6. a kind of polystyrene according to claim 1 and 2/thermosetting resin syntactic foam, it is characterized in that: described resin monomer or prepolymer are: one or more in epoxy monomer, urea-formaldehyde resin prepolymer, melmac prepolymer, the resol prepolymer.
7. the preparation method of a kind of polystyrene as claimed in claim 1 or 2/thermosetting resin syntactic foam, it is characterized in that: described method steps is as follows:
(1) with after the expandable polystyrene particle pre-frothing, obtains polystyrene bead;
(2) in resin monomer or prepolymer, add solidifying agent, obtain mixture A after mixing;
(3) with after even coating of described polystyrene bead usefulness mixture A, carry out slaking, obtain described polystyrene/thermosetting resin syntactic foam.
8. the preparation method of a kind of polystyrene according to claim 7/thermosetting resin syntactic foam, it is characterized in that: the diameter of styrene beads is 1 ~ 10mm described in the step (1).
9. the preparation method of a kind of polystyrene according to claim 7/thermosetting resin syntactic foam is characterized in that: pre-expansion time is 5 ~ 30min in the step (1), and temperature is 70 ~ 140 ℃; The curing time is 0 ~ 30min in the step (3), and temperature is 80 ~ 180 ℃.
10. the preparation method of a kind of polystyrene according to claim 7/thermosetting resin syntactic foam is characterized in that:
Described urea-formaldehyde resin prepolymer is obtained at 50 ~ 90 ℃, pH=7.5 ~ 10 time stirring reaction 1 ~ 6h by urea and formaldehyde, and the mol ratio of urea and formaldehyde is 1.5 ~ 4.0:1;
Described melmac prepolymer is obtained at 60 ~ 90 ℃, pH=7.5 ~ 10 time stirring reaction 1 ~ 5h by trimeric cyanamide and formaldehyde, and the mol ratio of trimeric cyanamide and formaldehyde is 2.0 ~ 4.0:1;
The resol prepolymer comprises thermoplasticity and heat-reactive phenolic resin prepolymer, heat-reactive phenolic resin prepolymer wherein, and stirring reaction 1 ~ 6h under 70 ~ 110 ℃, alkaline condition obtains by formaldehyde and phenol, and the mol ratio of trimeric cyanamide and formaldehyde is 1 ~ 2.0:1; The novolac resin prepolymer, stirring reaction 1 ~ 6h under 70 ~ 140 ℃, acidic conditions obtains by formaldehyde and phenol, and the mol ratio of trimeric cyanamide and formaldehyde is 0.5 ~ 1:1.
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