CN106146891A - A kind of expansion type flame retardant and the application in polyurethane foam thereof - Google Patents
A kind of expansion type flame retardant and the application in polyurethane foam thereof Download PDFInfo
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- CN106146891A CN106146891A CN201510152115.7A CN201510152115A CN106146891A CN 106146891 A CN106146891 A CN 106146891A CN 201510152115 A CN201510152115 A CN 201510152115A CN 106146891 A CN106146891 A CN 106146891A
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- flame retardant
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Abstract
The invention discloses a kind of expansion type flame retardant and the application in polyurethane foam thereof, expansion type flame retardant is the microcapsule being overmolding to for wall shell with phosphate as capsule-core, with polymer, it uses following technique to be prepared from: solvent is divided into two parts, and the aqueous solution adding emulsifying agent, phosphate and water-soluble polymer reaction monomers in portion carries out mixing to obtain latex A；Another part of solvent adds isocyanates and catalyst, forms emulsion B；Latex A and emulsion B are carried out hybrid reaction with stirring and obtains expansion type flame retardant.The microcapsule that the present invention is overmolding to for wall shell with phosphate as capsule-core, with polymer by interfacial polymerization, when being heated, phosphate is as acid source, foaming agent, the polyureas of cladding or polyurethane are as carbon forming agent, making the microcapsule composition Novel Intumescent Flame Retardant of gained, flame retardant effect highlights, is widely used.
Description
Technical field
The invention belongs to expanded material technical field, be specifically related to a kind of expansion type flame retardant and the application in polyurethane foam thereof.
Background technology
Owing to phosphate has, fusing point is low, phosphorus content is high and carbon containing is few, endothermic decomposition can become Metaphosphoric acid or phosphoric acid when burning, melted at low temperatures produces one layer of vitreous film residual covering, and it is few to give birth to smoke in combustion, therefore can use as fire retardant.As Chinese patent CN103755908A disclose in hard polyurethane foam, add hollow glass micropearl and phosphate simultaneously time, phosphate endothermic decomposition can become Metaphosphoric acid and phosphoric acid when burning, its fusing point is relatively low, one layer of vitreous film residual covering of melted at low temperatures generation, form melted thermal insulation layer again to cover at matrix surface and air exclusion with incombustible hollow glass micropearl, thus reduce the HRR of foamed materials；Its resume combustion can be stoped when covering reaches certain thickness, stop burning to carry out, thus improve the fire resistance of polyurethane foamed material.But, phosphate, owing to having good water solublity, can migrate because being dissolved in water, decompose and lose efficacy so that it is as the miopragia of fire proofing for building.
Additionally, Chinese patent CN102417612A discloses the preparation method of a kind of in-situ modified expansion type flame retardant, the preparation method of a kind of microcapsule-coated ammonium polyphosphate being directed to, select methylolation amino resins as source of the gas, acid catalysis crosslinking curing under the effect of phosphate ester acid, generate phosphate ester melamine salt and then be coated on the surface of APP, improve the resistance to water of expansion type flame retardant.But its preparation method cumbersome, after needing to be sequentially prepared phosphate ester acid, methylolated melamine, coated ammonium polyphosphate prepares expansion type flame retardant again.
Summary of the invention
It is an object of the invention to provide a kind of hydrolysis, be difficult to the expansion type flame retardant of precipitation and the application in polyurethane foam thereof, solve phosphate flame retardants hygroscopic inefficacy in polyurethane foam, the unendurable problem of flame retardant effect.The present invention utilizes interfacial polymerization to wrap up one layer at fire retardant phosphate surface can obtain efficient expansion type flame retardant as the polymer of carbon forming agent, the polyurethane foam jointly prepared with hollow glass micropearl, and flame retardant effect is excellent, and mechanical property is good.
It is an object of the invention to be achieved through the following technical solutions:
A kind of expansion type flame retardant, described expansion type flame retardant is the microcapsule being overmolding to for wall shell with phosphate as capsule-core, with polymer, and it uses following technique to be prepared from:
(1) solvent being divided into two parts, the aqueous solution adding emulsifying agent, phosphate and water-soluble polymer reaction monomers wherein in a solvent mixes, and obtains latex A；The mass ratio of described emulsifying agent, phosphate and water-soluble polymer reaction monomers is 5-15:15-50:15-50；
(2) in another part of solvent, add isocyanates and catalyst carries out mixing dispersion, form emulsion B；Described isocyanates, catalyst and phosphatic mass ratio are 100-150:2-5:15-50；
(3) latex A and emulsion B are mixed with stirring, be slowly heated and be warming up to 50-60 oC, after reaction 1-2h, cooling is centrifugal, and through washing, sucking filtration, be dried to obtain expansion type flame retardant.
In described step (1), emulsifying agent is dodecyl sodium sulfate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, sodium lauryl sulphate, nekal or sorbitol anhydride oleate (Span80).
In described step (1), phosphate is ammonium dihydrogen phosphate, diammonium phosphate, potassium dihydrogen phosphate or ammonium phosphate.
In described step (1), the mass concentration of the aqueous solution of water-soluble polymer reaction monomers is 30-50%, and water-soluble polymer reaction monomers refers to the condensation polymerization monomer of water miscible two or more functional group.
Described condensation polymerization monomer includes ethylene glycol, hexanediol, pentanediol, Polyethylene Glycol, tetramethylolmethane, ethylenediamine, diethyl triamine or trientine.
In described step (2), catalyst is stannous octoate or dibutyl tin laurate.
In described step (2), isocyanates is hexamethylene diisocyanate, isophorone diisocyanate, toluene di-isocyanate(TDI) or methyl diphenylene diisocyanate.
Solvent in described step (1) and (2) is toluene, dimethylbenzene, oxolane or acetone；In described step (1), the quality of solvent is (1-2) with emulsifying agent, the ratio of phosphate quality sum: 1.
It is a further object to provide the application in hard polyurethane foam of the expansion type flame retardant of above-mentioned preparation, expansion type flame retardant and hollow glass micropearl are added as fire retardant for 10-30:15 in mass ratio the hard polyurethane foams being prepared high resistance to compression, highly effective flame-retardant in urethane raw by foam process；Described hollow glass micropearl is to carry out surface modification treatment gained through coupling agent.
Polyurethane foam technique in the present invention is prior art, mainly expansion type flame retardant, hollow glass micropearl are added in polyether polyol, it is stirred at room temperature uniformly, adds water, polysiloxanes and dibutyl tin laurate, triethylene diamine and stir together with triethanolamine to obtain mixture；Add and after isocyanates stirs, be poured into foaming in mould, after ripening, obtain the RPUF that high resistance to compression is fire-retardant.
Its concrete preparation method is as follows:
(1) hollow glass micropearl and coupling agent 3-aminopropyl triethoxysilane in mass ratio 100: 1 are carried out surface modification treatment；
(2) by weight, by expansion type flame retardant 10-30 part, modified hollow glass micropearl 15 parts and polyether polyol 100 parts, it is stirred at room temperature mixing；
(3) adding 3 parts of water in above-mentioned mixed solution, 3 parts of polysiloxanes, 0.5 part of dibutyl tin laurate, 1 part of triethylene diamine and 3 parts of triethanolamine, stir to obtain mixture；
(4) methyl diphenylene diisocyanate (MDI) that 150 parts of isocyano (NCO) mass fractions are 30-33% is added in (3) in mixture, in 25oFoaming in casting mold after stirring under C, and control curing temperature 75oC, after ripening, the demoulding i.e. obtains described high resistance to compression, the RPUF of high fire-retardance.
The present invention uses interfacial polymerization, with phosphate as capsule-core, the polyureas or the polyurethane that generate with water-soluble polymer reaction monomers, emulsifying agent and isocyanates are prepared as water-fast microencapsulated fire retardant for wall shell cladding, water-soluble polymer reaction monomers is possible not only to the compatibility improving phosphate with organic system, and be a kind of carbonization forming agent, the microcapsule compactness of preparation is good, and reaction rate is fast, technique is simple and reaction condition is gentle, can carry out at normal temperatures；Simultaneously compared with traditional method, it is not necessary to add firming agent, reduce production cost.
The invention have the benefit that
1. the preparation technology of the expansion type flame retardant of the present invention uses simply, wraps up the interfacial polymerization that efficiency is high, can be as the polyureas of fire-retardant carbon forming agent or polyurethane at water-soluble flame retardant phosphate surface grafting last layer, and flame retarding efficiency is high, and resistance to water-soluble is good.
2. the expansion type flame retardant that prepared by the present invention is the microcapsule being overmolding to for wall shell with phosphate as capsule-core, with polymer.When being heated, phosphate as carbon forming agent, makes the microcapsule composition Novel Intumescent Flame Retardant of gained as acid source, foaming agent, the polyureas of cladding or polyurethane, and flame retardant effect highlights.
3. the expansion type flame retardant of the present invention and hollow glass micropearl prepare as fire retardant high resistance to compression, the hard polyurethane foams of highly effective flame-retardant have higher anti-flammability and fire-retardant persistency, oxygen index (OI) can reach 24.5-28.5%, mechanical property and thermally-stabilised be improved.
4, expansion type flame retardant prepared by the present invention is because its surface parcel is containing active group, make it good with the polyurethane foam matrix compatibility, water-tolerant will not be separated out, the physical property of foam is had no adverse effect, building, insulation and some require that high special occasions has a wide range of applications to water-fast.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described:
Method of testing in embodiment is as follows:
Rigid foam compression performance is tested according to GB/T 8813-2008, batten size 50 × 50 × 30 mm3.Compression speed is 3 mm/min, and compressive deformation is 15%.Direction of exerting pressure is parallel to abscess prolonging direction.
Limited oxygen index (LOI) is according to ASTM
D2863 standard is tested on HC-2 type oxygen index instrument (Jiangning Instrumental Analysis company of China produces), batten a size of 150 × 10 × 10 mm3。
Vertical combustion (UL-94) is tested: according to standard ASTM D3801-1996, using the CFZ-3 type horizontal vertical burning analyzer that Jiangning analytical tool factory produces, test sample, batten size used is 130 × 13 × 10 mm3
Fire-retardant sample water resistance test: vertical combustion batten is placed in 50oContinuous dipping 120h separately sampled, by sample 70 in the deionized water of C oC baking oven is dried, then tests the vertical combustion performance of sample after soaking among hot water.
HRR (KW/m2) obtained according to ISO5600 standard test by conic heat meter (Stanton Redcroft company of Britain) test.Sample cuts into 100 × 100 × 25
mm3Size.During test, set the radiation heat flux of instrument as 35 kW/m2。
Embodiment
1
(1) by weight, 40g toluene solvant adds 5g dodecyl sodium sulfate, adds 15g ammonium dihydrogen phosphate and 50g quality of glycol concentration is the aqueous solution of 30%, mix homogeneously, obtain latex A.
(2) in 40g toluene, add 2g part stannous octoate and 100g hexamethylene diisocyanate (HDI), be uniformly dispersed, form emulsion B
(3) latex A and emulsion B are stirred lower mixing, be slowly heated and be warming up to 50oC, reacts 1h, and cooling is centrifugal, precipitate through washing, sucking filtration, be dried to obtain efficient expansion type fire retardant.
Embodiment
2
(1) by weight, 50g tetrahydrofuran solvent adds 10g disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, adds the aqueous solution that mass concentration is 40% of 25g diammonium phosphate and 60g Polyethylene Glycol-200, mix homogeneously, obtain latex A.
(2) in 50g oxolane, add 3g dibutyl tin laurate and 100g isophorone diisocyanate (IPDI), be uniformly dispersed, form emulsion B
(3) latex A and emulsion B are stirred lower mixing, be slowly heated and be warming up to 60oC, reacts 2h, and cooling is centrifugal, precipitate through washing, sucking filtration, be dried to obtain efficient expansion type fire retardant.
Embodiment
3
(1) by weight, 100g acetone solvent adds 15g sodium lauryl sulphate, adds the aqueous solution that mass concentration is 50% of 40g dipotassium hydrogen phosphate and 100g pentanediol, mix homogeneously, obtain latex A.
(2) in 100g acetone, add 5g dibutyl tin laurate and 150g toluene di-isocyanate(TDI) (TDI), be uniformly dispersed, form emulsion B
(3) latex A and emulsion B are stirred lower mixing, be slowly heated and be warming up to 60oC, reacts 2h, and cooling is centrifugal, precipitate through washing, sucking filtration, be dried to obtain efficient expansion type fire retardant.
Embodiment
4
(1) by weight, 120g xylene solvent adds 15g sorbitol anhydride oleate (Span80), adds 50g ammonium phosphate and 100g ethylenediamine mass concentration is the aqueous solution of 50%, mix homogeneously, obtain latex A.
(2) in 120g dimethylbenzene, add 5g dibutyl tin laurate and 150g methyl diphenylene diisocyanate (MDI), be uniformly dispersed, form emulsion B
(3) latex A and emulsion B are stirred lower mixing, be slowly heated and be warming up to 60oC, reacts 2h, and cooling is centrifugal, precipitate through washing, sucking filtration, be dried to obtain efficient expansion type fire retardant.
Embodiment
5
(1) by weight, 120g toluene solvant adds 15g dodecyl sodium sulfate, adds 50g ammonium dihydrogen phosphate and 100g Polyethylene Glycol-200 mass concentration is the aqueous solution of 50%, mix homogeneously, obtain latex A.
(2) in 120g toluene, add 5g dibutyl tin laurate and 150g isophorone diisocyanate (IPDI), be uniformly dispersed, form emulsion B
(3) latex A and emulsion B are stirred lower mixing, be slowly heated and be warming up to 60oC, reacts 2h, and cooling is centrifugal, precipitate through washing, sucking filtration, be dried to obtain efficient expansion type fire retardant.
Embodiment
6
Expansion type flame retardant embodiment 5 prepared by following preparation method adds in polyurethane foam plastics raw material as fire retardant, prepares RPUF, specifically comprises the following steps that
(1) hollow glass micropearl and 100: 1 pairs in mass ratio hollow glass micropearls of coupling agent 3-aminopropyl triethoxysilane are carried out surface modification treatment；
(2) weight ratio that modification hollow glass micropearl 15 parts, polyether polyol 100 parts mixing, then according to the form below 1 first account for polyether polyol adds expansion type flame retardant, stirs at room temperature；
(3) adding 3 parts of water in above-mentioned mixed solution, 3 parts of polysiloxanes, 0.5 part of dibutyl tin laurate, 1 part of triethylene diamine and 3 parts of triethanolamine, stir to obtain mixture；
(4) methyl diphenylene diisocyanate (MDI) that 150 parts of isocyano mass fractions are 30-33% is added in said mixture, in 25oFoaming in casting mold after stirring under C, and control curing temperature 75oC, after ripening, the demoulding i.e. obtains described high resistance to compression, the RPUF of high fire-retardance.Then it being carried out mechanical property and combustibility test, result is as shown in table 1 below:
The performance test of table 1 polyurethane foam plastics
| Performance | Comparative example | Example 6-1 | Example 6-2 | Example 6-3 |
| Expansion type flame retardant accounts for weight ratio % of polyether polyol | 0 | 10 | 20 | 30 |
| Compressive strength MPa | 0.308 | 0.478 | 0.516 | 0.498 |
| Oxygen index (OI) % | 20.5 | 24.5 | 27.0 | 28.5 |
| UL-94 | NR | V-0 | V-0 | V-0 |
| Water resistance test UL-94 | NR | V-0 | V-0 | V-0 |
| HRR (KW/m2) | 414 | 78 | 0 | 0 |
Result shows: efficient expansion type fire retardant prepared by the present invention is good with the polyurethane foam system compatibility, improves mechanical property and the fire resistance of polyurethane foamed material.Can be seen that from upper table 1, only add the expansion type flame retardant of the weight ratio 10% accounting for polyether polyol, the polyurethane foamed material of preparation both can be made by UL-94 V-0 rank；And in the middle of the test of taper calorimetric, polyurethane foam articles is 35
KW/m2Sustained radiation under, HRR is 0, it is impossible to be ignited；The water-tolerant of flame retarded rigid foams, soaking 120h in hot water is still V-0 rank.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and apply the present invention.These embodiments obviously easily can be made various amendment by person skilled in the art, and General Principle described herein is applied in other embodiments without through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art should be within protection scope of the present invention according to the announcement of the present invention, the improvement made without departing from scope and amendment.
Claims (9)
1. an expansion type flame retardant, it is characterised in that: described expansion type flame retardant is the microcapsule being overmolding to for wall shell with phosphate as capsule-core, with polymer, and it uses following technique to be prepared from:
(1) solvent being divided into two parts, the aqueous solution adding emulsifying agent, phosphate and water-soluble polymer reaction monomers wherein in a solvent mixes, and obtains latex A；The mass ratio of described emulsifying agent, phosphate and water-soluble polymer reaction monomers is 5-15:15-50:15-50；
(2) in another part of solvent, add isocyanates and catalyst carries out mixing dispersion, form emulsion B；Described isocyanates, catalyst and phosphatic mass ratio are 100-150:2-5:15-50；
(3) latex A and emulsion B are mixed with stirring, be slowly heated and be warming up to 50-60oC, after reaction 1-2h, cooling is centrifugal, and through washing, sucking filtration, be dried to obtain expansion type flame retardant.
A kind of expansion type flame retardant the most according to claim 1, it is characterised in that: in described step (1), emulsifying agent is dodecyl sodium sulfate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, sodium lauryl sulphate, nekal or sorbitol anhydride oleate.
A kind of expansion type flame retardant the most according to claim 1, it is characterised in that: in described step (1), phosphate is ammonium dihydrogen phosphate, diammonium phosphate, potassium dihydrogen phosphate or ammonium phosphate.
A kind of expansion type flame retardant the most according to claim 1, it is characterized in that: in described step (1), the mass concentration of the aqueous solution of water-soluble polymer reaction monomers is 30-50%, water-soluble polymer reaction monomers refers to the condensation polymerization monomer of water miscible two or more functional group.
A kind of expansion type flame retardant the most according to claim 4, it is characterised in that: described condensation polymerization monomer includes ethylene glycol, hexanediol, pentanediol, Polyethylene Glycol, tetramethylolmethane, ethylenediamine, diethyl triamine or trientine.
A kind of expansion type flame retardant the most according to claim 1, it is characterised in that: in described step (2), catalyst is stannous octoate or dibutyl tin laurate.
A kind of expansion type flame retardant the most according to claim 1, it is characterised in that: in described step (2), isocyanates is hexamethylene diisocyanate, isophorone diisocyanate, toluene di-isocyanate(TDI) or methyl diphenylene diisocyanate.
A kind of expansion type flame retardant the most according to claim 1, it is characterised in that: the solvent in described step (1) and step (2) is toluene, dimethylbenzene, oxolane or acetone；In described step (1), the quality of solvent is (1-2) with emulsifying agent, the ratio of phosphate quality sum: 1.
9. the expansion type flame retardant as described in the claim 1-8 application in hard polyurethane foam, it is characterised in that: expansion type flame retardant and hollow glass micropearl are added as fire retardant for 10-30:15 in mass ratio the hard polyurethane foams being prepared high resistance to compression, highly effective flame-retardant in urethane raw by foam process；Described hollow glass micropearl is to carry out surface modification treatment gained through coupling agent.
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| CN201510152115.7A CN106146891A (en) | 2015-04-01 | 2015-04-01 | A kind of expansion type flame retardant and the application in polyurethane foam thereof |
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| CN201510152115.7A CN106146891A (en) | 2015-04-01 | 2015-04-01 | A kind of expansion type flame retardant and the application in polyurethane foam thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2018188508A (en) * | 2017-04-28 | 2018-11-29 | 第一工業製薬株式会社 | Polyol composition, polyurethane resin-formable composition, and composite material |
| CN111978706A (en) * | 2020-07-30 | 2020-11-24 | 四川金象赛瑞化工股份有限公司 | Preparation method for improving mechanical property of polyurethane flame-retardant material |
| CN112088181A (en) * | 2018-03-06 | 2020-12-15 | 巴斯夫聚氨酯特种产品（中国）有限公司 | Formulations comprising thermoplastic polyisocyanate polyaddition products, method for the production thereof and use thereof |
| CN114044940A (en) * | 2021-10-26 | 2022-02-15 | 南京理工大学 | Microencapsulated flame retardant and preparation method thereof |
| CN116638831A (en) * | 2023-06-01 | 2023-08-25 | 常州宏巨电子科技有限公司 | Efficient heat-insulating flame-retardant material between single battery cells |
| CN117247638A (en) * | 2023-10-27 | 2023-12-19 | 六安市金赛特橡塑制品有限公司 | Corrosion-resistant insulating rubber for extra-high voltage transmission line and production process |
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| CN101376811A (en) * | 2008-09-28 | 2009-03-04 | 中国科学技术大学 | Polyurethane microcapsulated inorganic phosphonium flame retardant and preparation thereof |
| CN103333364A (en) * | 2013-06-17 | 2013-10-02 | 青岛科技大学 | Compound intumescent flame retardant (IFR) and application thereof to carrying out flame retardance on polypropylene (PP) and polyurethane (PU) |
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| CN101037498A (en) * | 2006-03-17 | 2007-09-19 | 上海杰事杰新材料股份有限公司 | Microencapsulation reinforced inorganic particle and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2018188508A (en) * | 2017-04-28 | 2018-11-29 | 第一工業製薬株式会社 | Polyol composition, polyurethane resin-formable composition, and composite material |
| CN112088181A (en) * | 2018-03-06 | 2020-12-15 | 巴斯夫聚氨酯特种产品（中国）有限公司 | Formulations comprising thermoplastic polyisocyanate polyaddition products, method for the production thereof and use thereof |
| CN111978706A (en) * | 2020-07-30 | 2020-11-24 | 四川金象赛瑞化工股份有限公司 | Preparation method for improving mechanical property of polyurethane flame-retardant material |
| CN114044940A (en) * | 2021-10-26 | 2022-02-15 | 南京理工大学 | Microencapsulated flame retardant and preparation method thereof |
| CN116638831A (en) * | 2023-06-01 | 2023-08-25 | 常州宏巨电子科技有限公司 | Efficient heat-insulating flame-retardant material between single battery cells |
| CN116638831B (en) * | 2023-06-01 | 2023-11-24 | 常州宏巨电子科技有限公司 | Efficient heat-insulating flame-retardant material between single battery cells |
| CN117247638A (en) * | 2023-10-27 | 2023-12-19 | 六安市金赛特橡塑制品有限公司 | Corrosion-resistant insulating rubber for extra-high voltage transmission line and production process |
| CN117247638B (en) * | 2023-10-27 | 2024-03-22 | 六安市金赛特橡塑制品有限公司 | Corrosion-resistant insulating rubber for extra-high voltage transmission line and production process |
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Application publication date: 20161123 |