CN105566670B - Aqueous-phase suspending comminution granulation based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient and products thereof - Google Patents

Aqueous-phase suspending comminution granulation based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient and products thereof Download PDF

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CN105566670B
CN105566670B CN201510963752.2A CN201510963752A CN105566670B CN 105566670 B CN105566670 B CN 105566670B CN 201510963752 A CN201510963752 A CN 201510963752A CN 105566670 B CN105566670 B CN 105566670B
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polystyrene
fire
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CN105566670A (en
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李建芬
闫俊涛
宋光森
王春蕾
周晓荣
范国枝
王梅
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Wuhan Polytechnic University
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    • C08J2439/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
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Abstract

The invention belongs to the high-valued recycling fields of waste polystyrol foam material, and in particular to a kind of aqueous-phase suspending comminution granulation based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient and products thereof.It forms oil phase with inorganic organic gradient cooperative flame retardant thermal-insulating system, organic solvent and deposed polystyrene material, Aqueous dispersions medium is formed with surfactant, inorganic organic synergistic suspending agent and deionized water, under mechanical agitation, aqueous-phase suspending granulation makes oil phase drop, and steadily suspended dispersed is in an aqueous medium, heating steams the curing that organic solvent realizes gradient flame retardant polystyrene beads, and gradient fire retardant polystyrene thermal insulation board is obtained through pentane filling and foaming.For the present invention using waste and old polystyrol as raw material, physical recovering method simultaneously prepares the fire-retardant expandable polystyrene (EPS) bead of gradient, waste utilization, while improves its gradient flame retardant property and heat insulation, organic solvent can be recycled, environmentally friendly, is easy to industrialized production.

Description

Water based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient Phase suspension comminution granulation and products thereof
Technical field
The invention belongs to the high-valued recycling fields of waste polystyrol foam material, and in particular to one kind is based on useless polyphenyl Vinyl material prepares aqueous-phase suspending comminution granulation of the fire-retardant expandable polystyrene (EPS) bead of gradient and products thereof.
Background technology
Polystyrol foam material (Expanded polystyrene abbreviation EPS) is by steaming by expandable polystyrene Vapour foaming obtains, and has excellent adiabatic heat-insulation, sound insulation, shockproof, light, ageing-resistant and corrosion-resistant etc. performances, extensively For building exterior wall heat preserving field and packaging industry.EPS products are non-degradable, without putrefaction, typically disposable, tight after discarding Heavily contaminated environment, post processing cost height and complex process.Therefore, the resource recycling and height of waste polystyrol foam material Value, which recycles, has very important society, environment and economic benefit.
National house and town and country construction portion, national quality supervision and check quarantine general bureau, which combine, has issued national standard《Building Design fire safety rules》GB50016~2014 were implemented from 1 day May in 2015, this anti-flammability to architecture exterior wall insulating materials Higher requirement can be proposed.At present, the anti-flammability of polystyrol foam material mainly adds organic halogen containing flame-retardant, organic Fire retardant effect is good, and fire retardant, which decomposes, when playing fire retardation generates a kind of non-ignitable hydrogen halide, dilution oxygen and A kind of barrier property protective film is formed in polymer surfaces, the chain reaction for inhibiting burning carries out.But hydrogen halide has toxicity, Once fire occurs, the people to die in fire is many times because breathing is to toxic gas death by suffocation rather than is scorched to death. Increase organic fire-retardant dosage by excessive come to further improve the way of the anti-flammability of polystyrol foam material be EPS industries It does not advocate, not only increases production cost, but also with toxicity ruins the environment.With reference to inorganic combustion inhibitor nontoxic property and The high flame retardant of organic fire-retardant can reduce the use of organic fire-retardant using inorganic-organic compound flame retardant to a certain extent It measures and improves flame retardant effect, at present, research inorganic-organic hybrid fire retardant systems are a big main flow directions of flame retardant area.
At present, the EPS that gives up is recycled mainly to be recycled using solvent method, as Chinese invention patent CN100335539C is disclosed A kind of method of solvent reclamation recycling waste polystyrene foam plastic, using citrus seed oil dissolved polystyrene foam, adds in orange For the precipitating reagents such as 1~5 times of alcohols of oil volume or ethers through vacuum filtration, the polystyrene after filtering adds in orange oil body again 1~5 times of long-pending alcohols or ethers precipitating reagent carry out second and precipitate, and are filtered by vacuum to obtain irregular polystyrene group again Aggressiveness takes out filtered solution and adds in isometric water extraction twice, and being eventually adding auxiliary agent makes solvent and precipitating reagent separated, returns Solvent is received, which uses Nantural non-toxic solvent citrus seed oil, and citrus seed oil is of high cost, and recovery process is extremely complex, it is necessary to add in alcohol Class or ethers precipitating reagent and auxiliary agent distill extremely complex difficult realization, and cost recovery is higher, and obtained regenerated polystyrene is Irregular aggregate, and performance and added value without improving polystyrene, are unfavorable for industrial applications, such as follow-up profit With, it is necessary to through melting extrusion technique and cutting prilling.Chinese invention patent CN101230152B discloses a kind of useless polyphenyl The preparation method of ethylene micron order soccer star's particle, waste old polystyrene foamed plastic is dissolved in organic solvent formed it is organic Phase, then organic phase and the water dissolved with surfactant are mixed, by mechanical agitation with adding in surfactant high speed shear Emulsification forms microemulsion, then microemulsion is added in precipitating reagent, and by relenting, precipitating reagent synergistic effect prepares micron order ball Star solid particle, the invention prepare micron polystyrene by the way that microemulsion is added in precipitating reagent, and the precipitating reagent used is The solvent to dissolve each other with organic solvent and water although having recycled micron polystyrene, generates a large amount of water, has in the invention The mixed solution of solvent and precipitating reagent is difficult to separate, and does not mention and how to handle these waste liquids, is solving waste and old polystyrol Secondary pollution is brought while pollution again, cost is higher, and what is obtained is 9~120 microns of polystyrene particle, is not had Its new performance is assigned, also without application value.Foregoing invention technology simply recycles polystyrene material, and of high cost, technique is multiple It is miscellaneous, secondary pollution is generated, does not assign recycling polystyrene material new function and performance, product is nor the pearl of mm size Grain, does not improve the added value of deposed polystyrene resource recycling, and application prospect is remote, is unfavorable for industrialization promotion with answering With.
The content of the invention
It is fire-retardant based on deposed polystyrene material preparation gradient in view of the deficiencies of the prior art, the present invention provides one kind Aqueous-phase suspending comminution granulation of expandable polystyrene (EPS) bead and products thereof.Method is with lipophile inorganic combustion inhibitor, organic fire-retardant Inorganic-organic gradient cooperative flame retardant thermal-insulating system, organic solvent and deposed polystyrene material composition oil phase with insulation agent composition, Aqueous dispersions medium is formed with surfactant, inorganic-organic synergy suspending agent and deionized water, on mechanical stirring, surface Under activating agent and inorganic-organic synergy suspending agent collective effect, aqueous-phase suspending granulation makes oil phase drop steadily be dispersed in suspension within In aqueous media, it is warming up to organic solvent boiling temperature and steams the curing that organic solvent realizes gradient flame retardant polystyrene beads, That is what the curing of the distillation of organic solvent and gradient flame retardant polystyrene beads was synchronously realized, then, impregnate and prepare in pentane The fire-retardant expandable polystyrene bead of gradient is obtained, foaming processing can obtain gradient fire retardant polystyrene thermal insulation board.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of aqueous-phase suspending comminution granulation based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient, Comprise the following steps:
1) inorganic-organic gradient cooperative flame retardant thermal-insulating system is built
The modification of 1a) inorganic fire-retarded-thermal-insulating system
100~400ml of deionized water is sequentially added in a reservoir, and 1.0~3.0g of polyvinylpyrrolidone after dissolving, adds Enter 2.0~4.0g of nano-sized magnesium hydroxide, 2.0~4.0g of nano-aluminum hydroxide, 2.0~4.0g of nano-zinc borate, ammonium polyphosphate 2.0 ~4.0g, 2.0~4.0g of hydrotalcite, 2.0~4.0g of insulation agent, 5~15min of ultrasonic disperse, mechanical agitation, rotating speed 150~ 350rpm, heating water bath are warming up to 60~85 DEG C, add in 1.0~4.0g hydrophobic modification agent, react 0.5~1.5h, are taken out after cooling Filter and simultaneously washed with ethyl alcohol, obtained after dry loose shape lipophile it is inorganic fire-retarded-thermal-insulating system.
The hydrophobic modification agent is any one in oleic acid, polyethylene glycol phosphate or polypropylene glycol phosphate.
The insulation agent is superfine graphite, and powder footpath is 0.5~10um, and graphite has typical infrared radiation reflecting The effect of, can effective reflective thermal radiation, change the direction of heat transfer, improve the heat insulation effect of material.
1b) the preparation of inorganic-organic gradient cooperative flame retardant thermal-insulating system
It is 3 by weight:1, weighing step 1a) lipophile for preparing is inorganic fire-retarded-organic resistance of thermal-insulating system and equivalent It fires agent to add in dry-powder mixer, 15~50rpm of drum rotation speed, 5~10min of incorporation time can be uniformly mixed, is loose Shape powder obtains inorganic-organic gradient cooperative flame retardant~thermal-insulating system.
The organic fire-retardant is compound for any one in hexabromocyclododecane or deca-BDE or both
2) aqueous-phase suspending comminution granulation prepares the fire-retardant expandable polystyrene (EPS) bead of gradient
2a) organic phase:100~200ml of organic solvent is added in four round flask, adds in inorganic-organic gradient association With fire-retardant~1.0~8.0g of thermal-insulating system, mechanical agitation is uniformly dispersed, and then adds in deposed polystyrene 15~80g of material, dissolving 5~20min of ultrasonic disperse afterwards makes inorganic-organic gradient cooperative flame retardant thermal-insulating system be uniformly dispersed in polystyrene solution, obtains To organic phase.
The organic solvent is any one in ethyl acetate or chloroform;
The deposed polystyrene material is arbitrary in waste polystyrol foam material or deposed polystyrene injected plastics material It is a kind of;
2b) water phase:In the flask of overhead type mechanical agitator and distilling apparatus is installed, addition deionized water 150~ 500ml and mass concentration are 0.1~0.5% 1.0~10.0ml of aqueous surfactant solution, are added inorganic by 0.1~1.0g The inorganic-organic that suspending agent and the polymer suspension agent aqueous solution that 4.0~10.0ml mass concentrations are 2.0~6.0% form increases Suspending agent is imitated, 5~10min of mechanical agitation obtains water phase.
The surfactant is selected from anionic surfactant sodium dodecylbenzene sulfonate, anion surfactant ten Dialkyl sulfonates, nonionic surfactant nonylphenol polyoxyethylene ether or nonionic surfactant octylphenol polyethylene ethylene oxide Any one in ether.
In the inorganic-organic synergy suspending agent, Inorganic suspending agent is tricalcium phosphate, barium sulfate, talcum powder or kaolin In any one;Polymer suspension agent for hydroxyethyl cellulose, polyacrylate, polyvinyl alcohol, polyvinylpyrrolidone, Any one in carboxymethyl cellulose, gelatin or cellulose ether.
2c) aqueous-phase suspending is granulated:By step 2a) the obtained organic phase is transferred to step 2b) obtain it is described In water phase, mechanical agitation rotating speed is 150~350rpm, in surfactant, inorganic-organic synergy suspending agent and mechanical agitation three Under recast is used, organic phase steadily in an aqueous medium, realize that aqueous-phase suspending is granulated, be warming up to organic solvent boiling point by suspended dispersed Temperature steams the curing that organic solvent realizes gradient flame retardant polystyrene beads, that is, prepares gradient flame retardant polystyrene beads.
2d) foaming agent impregnates:By step 2c) described in gradient flame retardant polystyrene beads be put into pentane foaming agent and soak To get to the fire-retardant expandable polystyrene (EPS) bead of gradient after stain.
2e) pre- hair shaping:The fire-retardant expandable polystyrene (EPS) bead of gradient, which pressurizes to send out to be molded in advance through vapor, obtains gradient association With fire retardant polystyrene heat insulating board.
The present invention also provides the gradient fire retardant polystyrene heat insulating boards being prepared according to the above method.
Gradient fire retardant polystyrene heat insulating board prepared by the present invention, due to being with the addition of the collaboration resistance of inorganic-organic gradient Thermal-insulating system is fired, inorganic-organic fire retardant each plays flame retardant efficiency in different gradient temperatures, and insulation agent graphite powder has piece Shape structure, can starvation and heat transfer, there is good flame retardant property, realize cooperative flame retardant synergy purpose, it is useless in recycling Its gradient flame retardant property is assigned while polystyrene material.In addition, it is added in inorganic-organic gradient cooperative flame retardant thermal-insulating system There is the superfine graphite powder of the heat-insulated factor, graphite powder excellent reflection infrared ray characteristic causes gradient fire retardant polystyrene to foam Material has preferable heat preservation and insulation, and therefore, the present invention prepares gradient fire retardant polystyrene expanded material, has excellent resistance Performance and heat insulation effect are fired, realizes the recycling of deposed polystyrene material and the double goal of high-valued recycling, for White foam garbage problem is solved to have very important significance.The invention is physical recovering method technique, and process is simple, You Jirong Agent can be recycled, at low cost, and the fire-retardant expandable polystyrene (EPS) bead granular diameter of gradient prepared by the recycling of aqueous-phase suspending comminution granulation is equal One, its flame retardant property and heat preservation and insulation can be improved, it is environmentally friendly, it is easy to industrialized production and application.
Description of the drawings
Fig. 1 is the optics for the fire-retardant expandable polystyrene (EPS) bead of gradient that the preparation method provided according to the present invention obtains Photo.
Fig. 2 is the light that the preparation method provided according to the present invention obtains gradient cooperative flame retardant polystyrene heat insulating board Learn photo.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and illustrated embodiment is served only for explaining the present invention, It is not intended to limit the scope of the present invention.
Embodiment 1
1) inorganic-organic gradient cooperative flame retardant thermal-insulating system is built
The modification of 1a) inorganic fire-retarded-thermal-insulating system
Deionized water 150ml, polyvinylpyrrolidone 1.2g are sequentially added in a reservoir, after dissolving, add in nanometer hydrogen-oxygen Change magnesium 2.0g, nano-aluminum hydroxide 2.0g, nano-zinc borate 2.0g, ammonium polyphosphate 2.0g, hydrotalcite 2.0g, average grain diameter 5um Graphite insulation agent 2.0g, ultrasonic disperse 8min, mechanical agitation, rotating speed 180rpm, heating water bath is warming up to 73 DEG C, adds in 2.0g Hydrophobic modification agent polyethylene glycol phosphate reacts 1.0h, filters after cooling and is washed with ethyl alcohol, and loose shape parent is obtained after dry Oiliness is inorganic fire-retarded-thermal-insulating system.
1b) the preparation of inorganic-organic gradient cooperative flame retardant thermal-insulating system
It is 3 by weight:1, weighing step 1a) lipophile for preparing is inorganic fire-retarded-organic resistance of thermal-insulating system and equivalent Agent hexabromocyclododecane is fired to add in dry-powder mixer, drum rotation speed 20rpm, incorporation time 6min can be uniformly mixed, Loose shape powder obtains inorganic-organic gradient cooperative flame retardant thermal-insulating system.
2) aqueous-phase suspending comminution granulation prepares the fire-retardant expandable polystyrene (EPS) bead of gradient
2a) organic phase:Ethyl acetate 100ml is added in four round flask, adds in inorganic-organic gradient cooperative flame retardant Thermal-insulating system 4.0g, mechanical agitation are uniformly dispersed, and then add in waste polystyrol foam material 35g, ultrasonic disperse after dissolving 8min makes inorganic-organic gradient cooperative flame retardant thermal-insulating system be uniformly dispersed in polystyrene solution, obtains organic phase.
2b) water phase:In the flask of overhead type mechanical agitator and distilling apparatus is installed, deionized water 300ml is added in It is 0.15% nonylphenol polyoxyethylene ether aqueous solution 5.0ml with mass concentration, adds by 0.4g Inorganic suspending agent tricalcium phosphates With 5.0ml mass concentrations be 3.0% polyvinyl alcohol water solution form inorganic-organic synergy suspending agent, mechanical agitation 6min Obtain water phase.
2c) aqueous-phase suspending is granulated:By step 2a) the obtained organic phase is transferred to step 2b) obtain it is described In water phase, mechanical agitation rotating speed is 250rpm, in three recast of surfactant, inorganic-organic synergy suspending agent and mechanical agitation Under, organic phase steadily in an aqueous medium, realize that aqueous-phase suspending is granulated, be warming up to 77 DEG C and steam organic solvent by suspended dispersed It realizes the curing of gradient flame retardant polystyrene beads, that is, prepares gradient flame retardant polystyrene beads.
2d) foaming agent impregnates:By step 2c) described in gradient flame retardant polystyrene beads be put into pentane foaming agent and soak To get to the fire-retardant expandable polystyrene (EPS) bead of gradient after stain.
2e) pre- hair shaping:The fire-retardant expandable polystyrene (EPS) bead of gradient, which pressurizes to send out to be molded in advance through vapor, obtains gradient association With fire retardant polystyrene heat insulating board.
Embodiment 2
1) inorganic-organic gradient cooperative flame retardant thermal-insulating system is built
The modification of 1a) inorganic fire-retarded-thermal-insulating system
Deionized water 150ml, polyvinylpyrrolidone 1.5g are sequentially added in a reservoir, after dissolving, add in nanometer hydrogen-oxygen Change magnesium 3.0g, nano-aluminum hydroxide 3.0g, nano-zinc borate 3.0g, ammonium polyphosphate 3.0g, hydrotalcite 3.0g, average grain diameter 5um Graphite insulation agent 3.0g, ultrasonic disperse 10min, mechanical agitation, rotating speed 200rpm, heating water bath is warming up to 75 DEG C, adds in 2.4g hydrophobic modification agent oleic acid reacts 1.0h, filters after cooling and is washed with ethyl alcohol, obtained after dry loose shape lipophile without Machine is fire-retardant-thermal-insulating system.
1b) the preparation of inorganic-organic gradient cooperative flame retardant thermal-insulating system
It is 3 by weight:1, weighing step 1a) lipophile for preparing is inorganic fire-retarded-organic resistance of thermal-insulating system and equivalent It fires agent deca-BDE to add in dry-powder mixer, drum rotation speed 25rpm, incorporation time 8min can be uniformly mixed, are crisp Loose shape powder obtains inorganic-organic gradient cooperative flame retardant thermal-insulating system.
2) aqueous-phase suspending comminution granulation prepares the fire-retardant expandable polystyrene (EPS) bead of gradient
2a) organic phase:Chloroform 130ml is added in four round flask, it is heat-insulated to add in inorganic-organic gradient cooperative flame retardant System 6.0g, mechanical agitation are uniformly dispersed, and then add in waste polystyrol foam material 65g, ultrasonic disperse 10min after dissolving, Inorganic-organic gradient cooperative flame retardant thermal-insulating system is made to be uniformly dispersed in polystyrene solution, obtains organic phase.
2b) water phase:In the flask of overhead type mechanical agitator and distilling apparatus is installed, deionized water 300ml is added in Be 0.2% nonylphenol polyoxyethylene ether aqueous solution 5.0ml with mass concentration, add by 0.6g Inorganic suspending agents tricalcium phosphate and The inorganic-organic synergy suspending agent that the polyvinyl alcohol water solution that 5.0ml mass concentrations are 4.5% forms, mechanical agitation 8min are Obtain water phase.
2c) aqueous-phase suspending is granulated:By step 2a) the obtained organic phase is transferred to step 2b) obtain it is described In water phase, mechanical agitation rotating speed is 240rpm, in three recast of surfactant, inorganic-organic synergy suspending agent and mechanical agitation Under, organic phase steadily in an aqueous medium, realize that aqueous-phase suspending is granulated, be warming up to 61 DEG C and steam organic solvent by suspended dispersed It realizes the curing of gradient flame retardant polystyrene beads, that is, prepares gradient flame retardant polystyrene beads.
2d) foaming agent impregnates:By step 2c) described in gradient flame retardant polystyrene beads be put into pentane foaming agent and soak To get to the fire-retardant expandable polystyrene (EPS) bead of gradient after stain.
2e) pre- hair shaping:The fire-retardant expandable polystyrene (EPS) bead of gradient, which pressurizes to send out to be molded in advance through vapor, obtains gradient association With fire retardant polystyrene heat insulating board.
Embodiment 3
1) inorganic-organic gradient cooperative flame retardant thermal-insulating system is built
The modification of 1a) inorganic fire-retarded-thermal-insulating system
Deionized water 350ml, polyvinylpyrrolidone 2.5g are sequentially added in a reservoir, after dissolving, add in nanometer hydrogen-oxygen Change magnesium 4.0g, nano-aluminum hydroxide 4.0g, nano-zinc borate 4.0g, ammonium polyphosphate 4.0g, hydrotalcite 4.0g, average grain diameter 5um Graphite insulation agent 4.0g, ultrasonic disperse 13min, mechanical agitation, rotating speed 280rpm, heating water bath is warming up to 76 DEG C, adds in 4.0g hydrophobic modification agent oleic acid reacts 1.2h, filters after cooling and is washed with ethyl alcohol, obtained after dry loose shape lipophile without Machine is fire-retardant-thermal-insulating system.
1b) the preparation of inorganic-organic gradient cooperative flame retardant thermal-insulating system
It is 3 by weight:1, weighing step 1a) lipophile for preparing is inorganic fire-retarded-organic resistance of thermal-insulating system and equivalent It fires agent deca-BDE to add in dry-powder mixer, drum rotation speed 30rpm, incorporation time 10min can be uniformly mixed, are crisp Loose shape powder obtains inorganic-organic gradient cooperative flame retardant thermal-insulating system.
2) aqueous-phase suspending comminution granulation prepares the fire-retardant expandable polystyrene (EPS) bead of gradient
2a) organic phase:Ethyl acetate 120ml is added in four round flask, adds in inorganic-organic gradient cooperative flame retardant Thermal-insulating system 7.0g, mechanical agitation are uniformly dispersed, and then add in deposed polystyrene injected plastics material 70g, ultrasonic disperse after dissolving 15min makes inorganic-organic gradient cooperative flame retardant thermal-insulating system be uniformly dispersed in polystyrene solution, obtains organic phase.
2b) water phase:In the flask of overhead type mechanical agitator and distilling apparatus is installed, deionized water 360ml is added in Be 0.2% sodium dodecyl benzene sulfonate aqueous solution 5.0ml with mass concentration, add by 0.6g Inorganic suspending agents tricalcium phosphate and The inorganic-organic synergy suspending agent that the hydroxyethyl cellulose aqueous solution that 5.0ml mass concentrations are 6.0% forms, mechanical agitation 8min obtains water phase.
2c) aqueous-phase suspending is granulated:By step 2a) the obtained organic phase is transferred to step 2b) obtain it is described In water phase, mechanical agitation rotating speed is 280rpm, in three recast of surfactant, inorganic-organic synergy suspending agent and mechanical agitation Under, organic phase steadily in an aqueous medium, realize that aqueous-phase suspending is granulated, be warming up to 77 DEG C and steam organic solvent by suspended dispersed It realizes the curing of gradient flame retardant polystyrene beads, that is, prepares gradient flame retardant polystyrene beads.
2d) foaming agent impregnates:By step 2c) described in gradient flame retardant polystyrene beads be put into pentane foaming agent and soak To get to the fire-retardant expandable polystyrene (EPS) bead of gradient after stain.
2e) pre- hair shaping:The fire-retardant expandable polystyrene (EPS) bead of gradient, which pressurizes to send out to be molded in advance through vapor, obtains gradient association With fire retardant polystyrene heat insulating board.
Effect example
As being the fire-retardant expandable polystyrene (EPS) bead of gradient that the preparation method provided according to the present invention obtains in Fig. 1. The bead that as we know from the figure prepared by the present invention is ball-type appearance, due to being added in inorganic-organic gradient cooperative flame retardant thermal-insulating system Insulation agent superfine graphite powder, therefore obtained bead is black beads, average grain diameter about 1.1mm, particle diameter distribution is more uniform, grain Footpath size is controllable.
If Fig. 2 is the preparation method provided according to the present invention obtains gradient cooperative flame retardant polystyrene heat insulating board Optical photograph, heat insulating board are gray appearance, and mouldability is preferable.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and Within principle, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention.

Claims (6)

1. a kind of aqueous-phase suspending comminution granulation based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient, It is characterized in that, comprises the following steps:
1) inorganic-organic gradient cooperative flame retardant thermal-insulating system is built
The modification of 1a) inorganic fire-retarded-thermal-insulating system
1.0~3.0g of 100~400ml of deionized water and polyvinylpyrrolidone is sequentially added in a reservoir, and after dissolving, addition is received 2.0~4.0g of rice magnesium hydroxide, 2.0~4.0g of nano-aluminum hydroxide, 2.0~4.0g of nano-zinc borate, ammonium polyphosphate 2.0~ 4.0g, 2.0~4.0g of hydrotalcite and insulation agent 2.0~4.0g, 5~15min of ultrasonic disperse, mechanical agitation, rotating speed 150~ 350rpm, heating water bath are warming up to 60~85 DEG C, add in 1.0~4.0g hydrophobic modification agent, react 0.5~1.5h, are taken out after cooling Filter, and is washed with ethyl alcohol, obtained after dry loose shape lipophile it is inorganic fire-retarded-thermal-insulating system;
1b) the preparation of inorganic-organic gradient cooperative flame retardant thermal-insulating system
It is 3 by weight:1, weighing step 1a) lipophile that is prepared is inorganic fire-retarded-and thermal-insulating system and organic fire-retardant add Enter into dry-powder mixer, 15~50rpm of drum rotation speed, 5~10min of incorporation time can be uniformly mixed, loose shape Powder obtains inorganic-organic gradient cooperative flame retardant thermal-insulating system;
2) aqueous-phase suspending comminution granulation prepares the fire-retardant expandable polystyrene (EPS) bead of gradient
2a) organic phase:Add in 100~200ml of organic solvent in a reservoir, add in 1.0~8.0g step 1b) obtain it is inorganic- Organic gradient cooperative flame retardant thermal-insulating system, mechanical agitation are uniformly dispersed, and then add in deposed polystyrene 15~80g of material, dissolving 5~20min of ultrasonic disperse afterwards makes inorganic-organic gradient cooperative flame retardant thermal-insulating system be uniformly dispersed in polystyrene solution, obtains To organic phase;
2b) water phase:In the flask of overhead type mechanical agitator and distilling apparatus is installed, 150~500ml of deionized water is added in 1.0~10.0ml of aqueous surfactant solution with mass concentration is 0.1~0.5%, adds by the inorganic suspensions of 0.1~1.0g The inorganic-organic synergy that agent and the polymer suspension agent aqueous solution that 4.0~10.0ml mass concentrations are 2.0~6.0% form is hanged Floating agent, 5~10min of mechanical agitation obtain water phase;
2c) aqueous-phase suspending is granulated:By step 2a) the obtained organic phase is transferred to step 2b) in the obtained water phase, machine Tool speed of agitator is 150~350rpm, is warming up to organic solvent boiling temperature and steams organic solvent realization gradient flame-retardant polystyrene Gradient flame retardant polystyrene beads are prepared in the curing of alkene bead;
2d) foaming agent impregnates:By step 2c) described in gradient flame retardant polystyrene beads be put into pentane foaming agent and impregnate Afterwards to get to the fire-retardant expandable polystyrene (EPS) bead of gradient.
2. the water according to claim 1 based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient Phase suspension comminution granulation, it is characterised in that:Step 1a) in, the hydrophobic modification agent is selected from oleic acid, polyethylene glycol phosphate or poly- Any one in propylene glycol phosphate;The insulation agent is superfine graphite powder, and grain size is 0.5~10 μm.
3. the water according to claim 2 based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient Phase suspension comminution granulation, it is characterised in that:Step 1b) in, the organic fire-retardant is in hexabromocyclododecane or deca-BDE Any one or both it is compound.
4. the water according to claim 3 based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient Phase suspension comminution granulation, it is characterised in that:Step 2a) in, the organic solvent is any one in ethyl acetate or chloroform; The deposed polystyrene material is any one in waste polystyrol foam material or deposed polystyrene injected plastics material.
5. the water according to claim 4 based on the fire-retardant expandable polystyrene (EPS) bead of deposed polystyrene material preparation gradient Phase suspension comminution granulation, it is characterised in that:Step 2b) in, the surfactant is selected from anion surfactant dodecyl Benzene sulfonic acid sodium salt, anion surfactant dodecyl sodium sulfate, nonionic surfactant nonylphenol polyoxyethylene ether or non- Any one in ionic surface active agent octyl phenol polyoxyethylene ether;In the inorganic-organic synergy suspending agent, inorganic suspension Agent is any one in tricalcium phosphate, barium sulfate, talcum powder or kaolin;Polymer suspension agent is hydroxyethyl cellulose, gathers Any one in Acrylates, polyvinyl alcohol, polyvinylpyrrolidone, carboxymethyl cellulose or gelatin.
6. a kind of fire-retardant expandable polystyrene (EPS) bead of gradient that method according to any one of claims 1 to 5 is prepared.
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CN108219233A (en) * 2017-12-18 2018-06-29 襄阳华虹高科新材料有限公司 A kind of gradient fire retardant and preparation method thereof
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