CN104974527A - Preparation method and application of organosilicon resin modified polymer foam composite material - Google Patents
Preparation method and application of organosilicon resin modified polymer foam composite material Download PDFInfo
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Abstract
The invention relates to the technical field of organosilicon and aims to solve the inherent problem of inflammability of most of carbon-based polymer foam materials. The invention provides a preparation method and application of an organosilicon resin modified polymer foam composite material. The organosilicon resin modified polymer foam composite material comprises the following components in parts by weight: 10 to 60 parts of a polymer foam material, 30 to 80 parts of organosilicon resin, 0.2 to 2.0 parts of a catalyst and 0 to 8 parts of an inorganic filler. According to the invention, the organosilicon resin is utilized to modify the inflammable polymer foam material, so non-halogen flame-retardancy of the material is realized; meanwhile, the addition of a small amount of the inorganic functional filler can further improve flame-retardant and mechanical performances of the foam composite material; and other functions and characteristics of hydrophobicity, antistatic property and the like are achieved.
Description
Technical field
The present invention relates to a kind of organosilicon technical field, relate in particular to preparation method and the application thereof of the polymer-modified foam materials of a kind of silicone resin.
Background technology
The performances such as density is little owing to having, low thermal conductivity and good sound-absorbing, sound insulation antidetonation, polymer-base foam material has been widely used in the fields such as building, automobile, packaging.With regard to thermoplastic polyurethane and polystyrene rigid foam, in the developed country such as West Europe, North America, be the heat insulation main raw of building heat preservation, the ratio in the share in whole building heat preservation market accounts for 50% always.Due to the inflammableness that most carbon-based polymer foam materials is intrinsic, and the hydrogen cyanide gas containing severe toxicity in combustion processes, can be produced, easily cause big fire rapid spread, the serious personal's injures and deaths easily caused and property damage.Therefore, the flame-retarded of polymeric foamed material has become inevitable trend.But, flame-retarded the used fire retardant overwhelming majority of current polymer foams is halide-containing, some Halogen flame retarded polymeric material can produce objectionable impurities when burning, and the countries such as European Union have started to prohibit the use, and the flame retarding efficiency of more existing halogen-free flame retardantss is lower.
Containing " silicon-oxygen-silicon " structure in silicone resin backbone structure, side chain contains a small amount of organic group, thus it has two-fold advantage that is organic and inorganic materials concurrently, resistance to elevated temperatures, resistance to irradiation and weather-proof ability, in combustion processes, release of heat is little, the amount of being fuming is little, do not discharge toxic gas and have self-extinguishing.Therefore, the fire resistant flame retardant performance of organic particularly silicone resin is much better than carbon back macromolecular material as polypropylene, urethane, epoxy resin etc.Therefore, utilize the polymer-modified foam of organosilicon material can prepare lightweight, flame-proof composite material, and a large amount of obnoxious flavour can not be produced, meet environmental requirement, demonstrate good market application foreground.
Traditional method mainly utilizes fire retardant to add in foam of polymers and realizes its flame retardant effect.Such as, it is brominated Polystyrene or the styrene-butadiene block copolymer of 40-80 weight fraction that Chinese patent CN 201080057444 discloses with bromine content, or tetrabromo-bisphenol compound (TBBPA) produces flame-retardant polymer foam as fire retardant.The Chinese patent being CN201110119867.5 at application number discloses in a kind of flame retardant polyurethane composite material and preparation method, first prepare flame-proof polyol, then flame-proof polyol and commixed type fire retardant are mixed into mixed system, again polyisocyanates is added in mixed system, after reaction, can flame retardant polyurethane composite material be obtained.Expansible black lead is coated polystyrene pre-expanded particles surface by nearest Chinese patent CN201110148602, and then prepares flame-retardant anti-dropping molded polystyrene (EPS) foam materials.In addition; disclose with methyl blocking polydimethylsiloxane as matrix in Chinese patent CN201010291205; add organic-inorganic filler and a kind of transparent flame-proof organosilicon coating liquid prepared by fire retardant, meet the requirement of actual photovoltaic and LED industry circuit card coating protection.But, adopt the method adding organic or inorganic fire retardant to prepare flame-proofed polymer material, there is the weak points such as flame retarding efficiency is not high, products of combustion is poisonous.
Summary of the invention
For solving the intrinsic flammability problems of most carbon-based polymer foam materials, the present invention proposes preparation method and the application thereof of the polymer-modified foamed composite of a kind of silicone resin, the present invention utilizes silicone resin to carry out modification combustible polymers foam materials, realizes the halogen-free flameproof of such material; Simultaneously by adding a small amount of inorganic functional fillers, the fire-retardant and mechanical property of foamed composite can be improved further, and give other functions as the characteristic such as hydrophobic, antistatic.
The present invention is achieved by the following technical solutions: the preparation method of the polymer-modified foamed composite of a kind of silicone resin, and the polymer-modified foamed composite of described silicone resin is made up of following component, and the weight part of each component is:
Polymer foams 10 ~ 60,
Silicone resin 30 ~ 80,
Catalyzer 0.2 ~ 2.0,
Mineral filler 0 ~ 8.
As preferably, the polymer-modified foamed composite of described silicone resin is made up of following component, and the weight part of each component is:
Polymer foams 10 ~ 60,
Silicone resin 55 ~ 70,
Catalyzer 0.5 ~ 1.0;
Mineral filler 2 ~ 6.
As preferably, polymer foams is selected from the one in polyurethane foam, melamine foamed plastic, polystyrene foam, polypropylene foam, polyethylene terephthalate foam, polyvinyl chloride foam, polyethylene and silicon rubber foam.
As preferably, described silicone resin be selected from the methyl silicon resin or methyl phenyl silicone resin with different side chain and molecular weight one or more.
As preferably, catalyzer is selected from polyetheramine, one or more in N, N-dimethyl benzylamine, benzoyl oxide, phenylformic acid, white lead carbonate, diethylenetriamine, triethylene tetramine, γ-aminopropyl triethoxysilane.
As preferably, mineral filler be selected from aluminium hydroxide, nano silicon, magnesium hydroxide, high heat-resistant boehmite, Z 250, titanium dioxide, barium titanate, graphite, Graphene, nano barium titanate calcium, nano carbon black, carbon nanotube one or more.
The polymer-modified foam composite preparation method for material of described a kind of silicone resin is following steps:
(1) first in silicone resin solution, catalyzer and mineral filler is added, mixed solution is obtained after mixing, the solvent of silicone resin solution can be selected from toluene, dimethylbenzene, hexanaphthene, ethanol, hexamethyldisiloxane, dimethicone mixture, octamethylcyclotetrasiloxane, normal hexane, industrial naptha one or more, the usage quantity of solvent is the amount making solute dissolves.As preferably, the solid content of silicone resin solution is 30 ~ 80%.
(2) polymer foams is joined in mixed solution prepared by step (1), under room temperature, polymer foams is infiltrated in mixed solution, as preferably, by after fully infiltrating to remove the bubble in hole; Be more preferably the bubble at room temperature vacuumizing and remove in hole, room temperature is 20 ~ 25 DEG C.
(3) by the polymer foam composite after infiltrating, put on spin coater, spin coating 2 ~ 8min is carried out in the slow speed of revolution, and as preferably, the rotating speed of spin coater is 300-800 rpm, spin-coating time 3-5min.
(4) polymer foam composite after spin coating being put into baking oven, be cured 2 ~ 12 hours at 60 ~ 160 DEG C, is to get rid of solvent, obtains the polymer-modified foamed composite of silicone resin after cooling.
The present invention is deposited by simple physical or silicone resin is covered the surface of polymer foams by spraying method, the features such as high temperature resistant, fire-retardant, the water tolerance utilizing silicone resin good and weathering resistance give flame retardant resistance and the hydrophobicity of polymer foam composite excellence, and keep its original three-dimensional pore space structure and fundamental property, to realize the flame retardant properties improving such foam materials.
The performances such as the fire-retardant of material and mechanics can be improved further by adding a small amount of mineral filler in silicone resin solution, the polymer-modified foamed composite flame retardant rating of such silicone resin is made to obtain V0 level, the ultimate compression strength of material is also significantly increased, and can give other functional performances of foam materials as good hydrophobic performance and the effect such as antistatic simultaneously.
The application of the polymer-modified foamed composite of silicone resin prepared by preparation method of the present invention in fire protection field.The method preparation technology is easy, easily amplify industrialization, effectively can realize the environment friendly halogen-free fireproof of combustible polymers material, and other functional performances can be realized according to actual needs, have a wide range of applications in fields such as polymer foams fire-retardant fireproofs.
Compared with prior art, the invention has the beneficial effects as follows:
(1) present method preparation technology easy, easily amplify industrialization, effectively can realize the environment friendly halogen-free fireproof of combustible polymers material;
(2) regulation and control of such foam materials flame retardant properties can also be realized by adding other mineral fillers, and the mechanical property that can improve further and waterproof effect.
Accompanying drawing explanation
Fig. 1 is pure polyurethane foamed material body structure surface scanning electron microscope (SEM) photograph in embodiment 2;
Fig. 2 is the scanning electron microscope (SEM) photograph of the polymer-modified foam materials of silicone resin in embodiment 2;
Fig. 3 is the vertical combustion test in embodiment 2, pure polyurethane foamed material being carried out to 10s;
Fig. 4 is that embodiment 2 makes solid content be the combustion testing of the 30s of the silicone resin modified polyurethane foam matrix material that 55% has silicon resin solution to prepare;
Fig. 5 is the test of embodiment 4 vertical combustion.
Embodiment
Below by specific embodiment, the present invention is described in further details.
Embodiment 1
First get methyl silicon resin/toluene solution 30g that solid content is 80wt%, adding q. s. toluene, to be diluted to solid content be 30wt%, then add catalyst n, and mechanically mixing after N-dimethyl benzylamine 0.8g, until evenly obtain mixed solution.Afterwards polystyrene foamed material 36g is immersed in above-mentioned methyl silicon resin/catalyst solution mixed solution, vacuumize the bubble removed in hole under room temperature, make its abundant dip-coating.By polymer-modified for the silicone resin after dip-coating foamed composite, put on spin coater, carry out spin coating (spin-coating time 3min, speed 400rpm).Finally foam materials complete for spin coating is put into baking oven, at 100 DEG C, be cured 8h, after cooling, obtain the polymer-modified foamed composite of silicone resin solidified.
Embodiment 2
First get methyl phenyl silicone resin/cyclohexane solution 40g that solid content is 80%, and add appropriate cyclohexane and be diluted to solid content 55wt%, then add catalyzer polyetheramine (D230) 0.8g and mix and make mixed solution.Afterwards polyurethane foamed material 8g is immersed in above-mentioned mixed solution, vacuumize the bubble removed in hole under room temperature, make its abundant dip-coating.By polymer-modified for the silicone resin after abundant dip-coating foamed composite, put on spin coater, carry out spin coating (spin-coating time 4min, speed 600rpm).Finally foamed composite complete for spin coating is put into baking oven, at 85 DEG C, be cured 10h.The polymer-modified foamed composite of silicone resin solidified is obtained after cooling.
Stuctures and properties before and after foam materials coating characterizes as shown in Figure 1, Figure 2, Figure 3, Figure 4, result shows, by above-mentioned simple preparation technology, silicone resin can be coated in the hole on framework surface of pure polyurethane foam structure by physics equably, defines one deck silicone resin film; During burning, silicone resin thermolysis can form layer of silicon dioxide thin film layer, effectively can completely cut off the contact of polyurethane material and air, realize its environment friendly halogen-free fireproof.
As shown in Figure 3, unmodified polyurethane foamed material all burns completely at 10s, and period is with molten melt drop state combustionmaterial drippage and the generation of a large amount of harmful smoke.Comparatively speaking, as shown in Figure 4, the polyurethane foam through silicone resin modification still keeps not having droplet-like combustionmaterial to drip between the basic configuration main combustion period of foam in 30s, and flame retardant properties is significantly improved, and has excellent hydrophobic performance.
Embodiment 3
First get methyl silicon resin/xylene solution 40g that solid content is 80wt%, directly add catalyzer phenylformic acid 0.2g and mix, make mixed solution.Afterwards polypropylene foam 6g is immersed in above-mentioned mixed solution, vacuumize the bubble removed in hole under room temperature, make its abundant dip-coating.Again by polymer-modified for the silicone resin after abundant dip-coating foamed composite, put on spin coater, carry out spin coating (spin-coating time 5min, speed 800rpm).Finally foamed composite complete for spin coating is put into baking oven, at 110 DEG C, be cured 6h.The polymer-modified foamed composite of silicone resin solidified is obtained after cooling.
The polymer-modified foamed composite of the silicone resin that embodiment 3 obtains has excellent fire-retardant and hydrophobic performance, and its anti-pressure ability is also significantly increased.From putting out after rear 25s lighted by this material, harmful smoke had and obviously weakened, and material integrity is maintained substantially without molten melt drop thing drippage period.According to UL94 vertical combustion testing standard, reach V-1 level flame-retardant standard.
Embodiment 4
First get methyl phenyl silicone resin/ethanolic soln 40g that solid content is 80%, add ethanol in proper amount and 0.88g nano silicon, and add catalyzer diethylenetriamine 0.8 g and mix, make mixed solution.Afterwards polyvinyl chloride foam material 5g is immersed in above-mentioned mixed solution, vacuumize the bubble removed in hole under room temperature, make its abundant dip-coating.Again by polymer-modified for the silicone resin after abundant dip-coating foamed composite, put on spin coater, carry out spin coating (spin-coating time 2min, speed 300rpm).Finally foamed composite complete for spin coating is put into baking oven, at 60 DEG C, be cured 12h.The silicone resin modified polyvinyl chloride foamed composite solidified is obtained after cooling.
If Fig. 5 is the silicone resin modified polyurethane foam matrix material vertical combustion test that embodiment 4 obtains; Result shows: the combustionproperty adding the silicone resin modified polyurethane foam matrix material after a small amount of nano silicon arrives V1 rank; Compared with example 3, the flame in this foam composite fuel combustion process is obviously less, and without molten melt drop thing drippage, and the flue gas of release is also less.In addition, nano silicon adds and can improve material mechanical performance, and its flexural strength improves significantly.
Embodiment 5
First get methyl silicon resin/industrial naptha solution 40g that solid content is 80%, add appropriate industrial naptha and 3.2g aluminium hydroxide, and add catalyzer diethylenetriamine 0.8 g and mix and make mixed solution.Afterwards silicon rubber foam material 4g is immersed in above-mentioned mixed solution, vacuumize the bubble removed in hole under room temperature, make its abundant dip-coating.Again by polymer-modified for the silicone resin after abundant dip-coating foamed composite, put on spin coater, carry out spin coating (spin-coating time 6min, speed 500rpm).Finally foamed composite complete for spin coating is put into baking oven, at 160 DEG C, be cured 2h.The silicone resin modified polyurethane foam matrix material solidified is obtained after cooling.
Result shows: the combustionproperty adding the silicone resin modified polyurethane foam matrix material after 2.0g ultrafine aluminium hydroxide arrives V0 rank; Compare with 4 with preceding embodiment 3, the flame in this foam composite fuel combustion process is obviously less, and without molten melt drop thing drippage, self-extinguishing time is shorter, and without a large amount of release being harmful to cigarette; Filler adds the flexural strength that can improve material simultaneously, and has good hydrophobic performance.
Above-described embodiment is used for explaining and the present invention is described, instead of limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.
Claims (9)
1. a preparation method for the polymer-modified foamed composite of silicone resin, is characterized in that, the polymer-modified foamed composite of described silicone resin is made up of following component, and the weight part of each component is:
Polymer foams 10 ~ 60,
Silicone resin 30 ~ 80,
Catalyzer 0.2 ~ 2.0,
Mineral filler 0 ~ 8.
2. the preparation method of the polymer-modified foamed composite of a kind of silicone resin according to claim 1, it is characterized in that, polymer foams is selected from the one in polyurethane foam, melamine foamed plastic, polystyrene foam, polypropylene foam, polyethylene terephthalate foam, polyvinyl chloride foam, polyethylene and silicon rubber foam.
3. the preparation method of the polymer-modified foamed composite of a kind of silicone resin according to claim 1, it is characterized in that, described silicone resin be selected from the methyl silicon resin or methyl phenyl silicone resin with different side chain and molecular weight one or more.
4. the preparation method of the polymer-modified foamed composite of a kind of silicone resin according to claim 1, it is characterized in that, catalyzer is selected from polyetheramine, one or more in N, N-dimethyl benzylamine, benzoyl oxide, phenylformic acid, white lead carbonate, diethylenetriamine, triethylene tetramine, γ-aminopropyl triethoxysilane.
5. the preparation method of the polymer-modified foamed composite of a kind of silicone resin according to claim 1, it is characterized in that, mineral filler be selected from aluminium hydroxide, nano silicon, magnesium hydroxide, high heat-resistant boehmite, Z 250, titanium dioxide, barium titanate, graphite, Graphene, nano barium titanate calcium, nano carbon black, carbon nanotube one or more.
6. the preparation method of the polymer-modified foamed composite of a kind of silicone resin according to any one of claim 1 to 5, is characterized in that, preparation method is following steps:
(1) first in silicone resin solution, add catalyzer and mineral filler, after mixing, obtain mixed solution;
(2) polymer foams is joined in mixture prepared by step (1), under room temperature, polymer foams is infiltrated in mixed solution;
(3) by the polymer foam composite after infiltration, put on spin coater, spin coating 2 ~ 8min is carried out in the slow speed of revolution;
(4) polymer foam composite after spin coating is put into baking oven, at 60 ~ 160 DEG C, be cured 2 ~ 12 hours, after cooling, obtain the polymer-modified foamed composite of silicone resin.
7. the preparation method of the polymer-modified foamed composite of a kind of silicone resin according to claim 6, it is characterized in that, the solvent of silicone resin solution can be selected from toluene, dimethylbenzene, hexanaphthene, ethanol, hexamethyldisiloxane, dimethicone mixture, octamethylcyclotetrasiloxane, normal hexane, industrial naptha one or more.
8. the preparation method of the polymer-modified foamed composite of a kind of silicone resin according to claim 6, is characterized in that, in step (3), the rotating speed of spin coater is 300-800 rpm.
9. the application of the polymer-modified foamed composite of silicone resin in fire protection field prepared of the preparation method of the polymer-modified foamed composite of a kind of silicone resin as claimed in claim 1.
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