CN105949360A - Flame-retardant expandable polystyrene containing flake graphite and body polymerization preparation method thereof - Google Patents

Flame-retardant expandable polystyrene containing flake graphite and body polymerization preparation method thereof Download PDF

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CN105949360A
CN105949360A CN201610368402.6A CN201610368402A CN105949360A CN 105949360 A CN105949360 A CN 105949360A CN 201610368402 A CN201610368402 A CN 201610368402A CN 105949360 A CN105949360 A CN 105949360A
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parts
preparation
graphite
flake graphite
mixture
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张宗卢
徐海
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Rizhao Sanming Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F112/00Homopolymers 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 an aromatic carbocyclic ring
    • C08F112/02Monomers containing only one unsaturated aliphatic radical
    • C08F112/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F112/06Hydrocarbons
    • C08F112/08Styrene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/44Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/16Making expandable particles
    • C08J9/20Making expandable particles by suspension polymerisation in the presence of the blowing agent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/02Halogenated hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2325/00Characterised 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 an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2325/02Homopolymers or copolymers of hydrocarbons
    • C08J2325/04Homopolymers or copolymers of styrene
    • C08J2325/06Polystyrene

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Polymers & Plastics (AREA)
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Abstract

The invention discloses flame-retardant expandable polystyrene containing flake graphite and a body polymerization preparation method thereof, and belongs to the technical field of building external wall heat insulation. The flame-retardant expandable polystyrene containing flake graphite is prepared from the following ingredients in parts by weight: 100 parts of styrene, 1 to 10 parts of flake graphite, 100 to 250 parts of pure water, 0.1 to 1 part of dilauroyl peroxide, 0.05 to 0.1 part of tert-Butyl peroxybenzoate , 0.5 to 1 part of hexabromocyclododecane, 0.1 to 0.5 part of dicumyl peroxide, 0.1 to 0.3 part of dispersing agents, 0.025 to 0.075 part of suspending agents, 1 to 5 parts of universal polystyrene particles, 0.1 to 0.5 part of polyethylene wax and 7 to 10 parts of pentane. According to the preparation method, the styrene and the graphite are subjected to body polymerization for a period of time under the initiator and low-temperature stabilizing conditions; flame retardants are also added; the heat conduction coefficient of a product is reduced; the flame resistant performance of the product is improved; the energy source consumption is reduced.

Description

Fire-retardant expandable polystyrene containing crystalline flake graphite and polymerisation in bulk preparation method thereof
Technical field
The present invention relates to skin heat preservation technology field, a kind of fire-retardant expandability polyphenyl containing crystalline flake graphite Ethylene and the preparation method of polymerisation in bulk thereof.
Background technology
Expandable polystyrene (EPS) be widely applied to because of its characteristic such as excellent heat-insulation and heat-preservation, light weight shock resistance packaging, The fields such as building heat preservation.But common expandable polystyrene has easy firing, during burning, release the shortcomings such as a large amount of black smokes, limit Make its application in building heat preservation field.
Along with people are to the research of expandable polystyrene and improvement, occur in that the fire-retardant expandability polyphenyl with certain fire resistance Ethylene, fire-retardant expandable polystyrene adds the fire retardants such as HBCD because of it and has possessed the feature of self-extinguishment, solves biography The defect that system polystyrene is readily burned, can reach B2 level by fire resistance.But, B2 level still belongs to combustible building materials, Its fire resistance need further to improve.
Chinese patent " CN201410056491.1 " discloses the preparation side of the expandable polystyrene polymer of a kind of graphene-containing Method, Chinese patent " CN201410056479.0 " discloses the system of a kind of fire-retardant expandable polystyrene spherolite containing leafing graphite Preparation Method, above-mentioned two patents all by the method adding graphite-like material in fire-retardant expandable polystyrene, reduce product Heat conductivity and can further improve the anti-flammability of product.
It is added in fire-retardant expandable polystyrene according to natural crystalline flake graphite, can further reduce cost, but, because of For the bad dispersibility of crystalline flake graphite, preparation process can form inhibition, so, never at fire-retardant expandable polystyrene The method of middle interpolation crystalline flake graphite occurs.
Summary of the invention
For above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of fire-retardant expandability polyphenyl second containing crystalline flake graphite Alkene and the preparation method of polymerisation in bulk thereof, this expandable polystyrene low cost, fire resistance is good, and heat conductivity is low;This is prepared Method uses crystalline flake graphite, reduces cost, by polymerisation in bulk, improves graphite dispersibility in the base, reduces polymer The reunion polymerization inhibiting capacity of graphite in system.
The present invention solves the technical scheme that its technical problem taked and includes: the fire-retardant expandable polystyrene containing crystalline flake graphite, bag Include: 100 parts of styrene, 1~10 part of scale graphite, 100~250 parts of pure water, 0.1~1 part of dilauroyl peroxide, 0.05~ 0.1 part of peroxidized t-butyl perbenzoate, 0.5~1 part of HBCD, 0.1~0.5 part of cumyl peroxide, 0.1~ 0.3 part of dispersant, 0.025~0.075 part of suspending agent, 1~5 part of General Purpose Polystyrenre granule, 0.1~0.5 part of Tissuemat E With 7~10 parts of pentanes, above number is by weight.
The present invention solves the technical scheme of its technical problem and also includes: the system of the expandable polystyrene polymerisation in bulk containing crystalline flake graphite Preparation Method, comprises the following steps:
Step 1: weigh by weight 100 parts of styrene, 1~10 part of scale graphite, 100~250 parts of pure water, 0.1~1 Part dilauroyl peroxide, 0.05~0.1 part of peroxidized t-butyl perbenzoate, 0.5~1 part of HBCD, 0.1~0.5 part Cumyl peroxide, 0.1~0.3 part of dispersant, 0.025~0.075 part of suspending agent, 1~5 part of General Purpose Polystyrenre Grain, 0.1~0.5 part of Tissuemat E and 7~10 parts of pentanes;
Step 2: the crystalline flake graphite, dilauroyl peroxide and the General Purpose Polystyrenre granule that step 1 are weighed are put into step 1 and claimed In the styrene taken, heat while stirring, obtain the first mixture;
Step 3: dispersant step 1 weighed and suspending agent add in the pure water that step 1 weighs, and add while stirring Heat, obtains the second mixture;
Step 4: described first mixture is joined in described second mixture, and adds the benzoyl peroxide weighed in step 1 After t-butyl formate, HBCD, cumyl peroxide and Tissuemat E, reaction to particle sinking grain are hard, add The pentane that step 1 weighs, is warming up to more than 115 DEG C and keeps pressure 0.5Mpa~0.8Mpa to react 3~4 hours, having reacted Cheng Hou, is cooled to less than 50 DEG C, is then passed through discharge, washs, is dried, coating, sieves and pack, obtain particle diameter 0.45~ 1.2mm contains the fire-retardant expandable polystyrene particle of graphite.
Further technical scheme is: the mesh number of described crystalline flake graphite is 1000~1500 mesh, and purity is 90~95%.
Further technical scheme is: described dispersant is in tricalcium phosphate, thenardite, silicate, sodium hexameta phosphate One or more mixture being mixed by any ratio.
Further technical scheme is: described suspending agent is triethyl group hexyl phosphoric acid, methyl anyl alcohol, cellulose, polyacrylamide The mixture that one or more in amine are mixed by any ratio.
Further technical scheme is: in step 2, the speed of stirring is 60~150rpm, and heating-up temperature is 65~75 DEG C, instead Answering process is isothermal reaction 1.8~2.5 hours.
Further technical scheme is: in step 3, the speed of stirring is 70~160rpm, and heating-up temperature is 85~95 DEG C.
Further technical scheme is: described General Purpose Polystyrenre granule is high impact polystyrene granule.
Further technical scheme is: in step 4, and the reaction condition that particle sinks and grain is hard is: the temperature strip of 85~95 DEG C React 9~10 hours under part.
Further technical scheme is: in step 4, and after adding pentane, heating rate during intensification is 1~10 DEG C/min.
The invention has the beneficial effects as follows:
1, in the expandable polystyrene of the present invention, with the addition of crystalline flake graphite, crystalline flake graphite aboundresources and low price, permissible Reduce production cost, possessed the feature of self-extinguishment because product adds the fire retardants such as HBCD, after adding graphite, contain There is the anti-flammability expandable polystyrene of graphite, because its strand contains graphite and fire retardant, fire resistance reaches B1 level (difficult Combustion property construction material), graphite has isolation heat energy transmission simultaneously, has the ultrared effect of reflection, therefore can reduce the heat conduction of goods Coefficient, the heat conductivity of obtained finished product, at 0.033W/ (m.k), can greatly reduce the consumption of the energy.
2, in the expandable polystyrene of the present invention, with the addition of General Purpose Polystyrenre (GPPS) granule as stabilizer, can be right Graphite wraps up, and improves graphite dispersibility in the base, and the graphite reunion polymerization inhibiting capacity in polymerization system greatly reduces.
3, the preparation method of the present invention, puts in styrene by crystalline flake graphite, dilauroyl peroxide and General Purpose Polystyrenre granule, Styrene and graphite polymerisation in bulk a period of time under the conditions of initiator and low-temperature stabilization, be equivalent to crystalline flake graphite is carried out pretreatment Processing, complete the mixing of styrene and graphite, styrene by graphite wrap up, with reduce its second stage to be polymerized inhibition shadow Ring.Improving graphite dispersibility in the base, crystalline flake graphite conversion ratio in styrene reaches about 30%, gluing of polymerization system Degree is greatly reduced, uses suspension polymerisation to prepare expandable polystyrene further, the graphite reunion polymerization inhibiting capacity in polymerization system Greatly reduce.
4, the fire retardant polystyrene processing and forming containing graphite prepared by the present invention, the styrofoam obtained uses standard GB8624-2012 Carrying out flame retardant rating test, standard GB/T10294-2008 of employing carries out Determination of conductive coefficients.Result is the stone prepared by the present invention Ink styrofoam flame retardant rating is B1 level, and oxygen index (OI) is 35, and heat conductivity is 0.033W/ (m.k).
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment one:
Fire-retardant expandable polystyrene containing crystalline flake graphite, including: 100 parts of styrene, 6 parts of scale graphites, 250 parts of pure water, 0.3 part of dilauroyl peroxide, 0.1 part of peroxidized t-butyl perbenzoate, 0.8 part of HBCD, 0.3 part of peroxidating two are different Propyl benzene, 0.25 part of dispersant, 0.06 part of suspending agent, 5 parts of General Purpose Polystyrenre granules, 0.5 part of Tissuemat E and 8 part penta Alkane, above number is by weight.
The preparation method of the above-mentioned fire-retardant expandable polystyrene polymerisation in bulk containing crystalline flake graphite, comprises the following steps:
Step 1: weigh 100 parts of styrene, 6 parts of scale graphites, 250 parts of pure water, 0.3 part of peroxidating 12 by weight Acyl, 0.1 part of peroxidized t-butyl perbenzoate, 0.8 part of HBCD, 0.3 part of cumyl peroxide, 0.25 part of phosphoric acid DFP, 0.06 part of cellulose, 5 parts of General Purpose Polystyrenre granules, 0.5 part of Tissuemat E and 8 parts of pentanes;
Step 2: the crystalline flake graphite, dilauroyl peroxide and the General Purpose Polystyrenre granule that step 1 are weighed are put into step 1 and claimed In the styrene taken, under the mixing speed of 100rpm, it is heated to 70 DEG C, and isothermal reaction 2 hours, obtain the first mixture;
Step 3: tricalcium phosphate step 1 weighed and cellulose add in the pure water that step 1 weighs, in the stirring of 150rpm It is warming up to 89 DEG C under speed, obtains the second mixture;
Step 4: described first mixture is joined in described second mixture, and adds the benzoyl peroxide weighed in step 1 T-butyl formate, HBCD, cumyl peroxide and Tissuemat E, react 9.5 hours until particle at 89 DEG C Sink and grain hard after, add the pentane that step 1 weighs, to 118 DEG C and keep pressure 0.6Mpa with the ramp of 9 DEG C/min React 3.5 hours, obtain the fire-retardant expandable polystyrene particle that particle diameter 0.9mm contains graphite.
In the present embodiment, the crystalline flake graphite mesh number used is 1000 mesh, and purity is 92%, and the dispersant used is tricresyl phosphate Calcium, the suspending agent used is cellulose.
Embodiment two:
Fire-retardant expandable polystyrene containing crystalline flake graphite, including: 100 parts of styrene, 8 parts of scale graphites, 230 parts of pure water, 0.5 part of dilauroyl peroxide, 0.08 part of peroxidized t-butyl perbenzoate, 0.7 part of HBCD, 0.5 part of peroxidating two are different Propyl benzene, 0.2 part of dispersant, 0.055 part of suspending agent, 4 parts of General Purpose Polystyrenre granules, 0.4 part of Tissuemat E and 9 part penta Alkane, above number is by weight.
The preparation method of the above-mentioned fire-retardant expandable polystyrene polymerisation in bulk containing crystalline flake graphite, comprises the following steps:
Step 1: weigh 100 parts of styrene, 8 parts of scale graphites, 230 parts of pure water, 0.5 part of peroxidating 12 by weight Acyl, 0.08 part of peroxidized t-butyl perbenzoate, 0.7 part of HBCD, 0.5 part of cumyl peroxide, 0.2 part of dispersion Agent, 0.055 part of suspending agent, 4 parts of General Purpose Polystyrenre granules, 0.4 part of Tissuemat E and 9 parts of pentanes;
Step 2: the crystalline flake graphite, dilauroyl peroxide and the General Purpose Polystyrenre granule that step 1 are weighed are put into step 1 and claimed In the styrene taken, under the mixing speed of 120rpm, it is heated to 68 DEG C, and isothermal reaction 2.2 hours, obtain the first mixing Thing;
Step 3: tricalcium phosphate step 1 weighed and cellulose add in the pure water that step 1 weighs, in the stirring of 160rpm It is warming up to 90 DEG C under speed, obtains the second mixture;
Step 4: described first mixture is joined in described second mixture, and adds the benzoyl peroxide weighed in step 1 T-butyl formate, HBCD, cumyl peroxide and Tissuemat E, react 9.2 hours until particle at 90 DEG C Sink and grain hard after, add the pentane that step 1 weighs, to 120 DEG C and keep pressure 0.7Mpa with the ramp of 10 DEG C/min React 3.3 hours, obtain the fire-retardant expandable polystyrene particle that particle diameter 1.1mm contains graphite.
In the present embodiment, the crystalline flake graphite mesh number used is 1200 mesh, and purity is 93%, and the dispersant used is anhydrous awns Nitre and the mixture of sodium hexameta phosphate, the suspending agent used is triethyl group hexyl phosphoric acid and the mixture of methyl anyl alcohol.
Embodiment three:
Fire-retardant expandable polystyrene containing crystalline flake graphite, including: 100 parts of styrene, 5 parts of scale graphites, 200 parts of pure water, 0.6 part of dilauroyl peroxide, 0.07 part of peroxidized t-butyl perbenzoate, 0.6 part of HBCD, 0.4 part of peroxidating two are different Propyl benzene, 0.15 part of dispersant, 0.07 part of suspending agent, 3.5 parts of General Purpose Polystyrenre granules, 0.35 part of Tissuemat E and 7 parts Pentane, above number is by weight.
The preparation method of the above-mentioned fire-retardant expandable polystyrene polymerisation in bulk containing crystalline flake graphite, comprises the following steps:
Step 1: weigh 100 parts of styrene, 5 parts of scale graphites, 200 parts of pure water, 0.6 part of peroxidating 12 by weight Acyl, 0.07 part of peroxidized t-butyl perbenzoate, 0.6 part of HBCD, 0.4 part of cumyl peroxide, 0.15 part point Powder, 0.07 part of suspending agent, 3.5 parts of General Purpose Polystyrenre granules, 0.35 part of Tissuemat E and 7 parts of pentanes;
Step 2: the crystalline flake graphite, dilauroyl peroxide and the General Purpose Polystyrenre granule that step 1 are weighed are put into step 1 and claimed In the styrene taken, under the mixing speed of 90rpm, it is heated to 68 DEG C, and isothermal reaction 2.3 hours, obtain the first mixture;
Step 3: tricalcium phosphate step 1 weighed and cellulose add in the pure water that step 1 weighs, in the stirring of 140rpm It is warming up to 88 DEG C under speed, obtains the second mixture;
Step 4: described first mixture is joined in described second mixture, and adds the benzoyl peroxide weighed in step 1 T-butyl formate, HBCD, cumyl peroxide and Tissuemat E, react 9.5 hours until particle at 88 DEG C Sink and grain hard after, add the pentane that step 1 weighs, to 116 DEG C and keep pressure 0.6Mpa with the ramp of 7 DEG C/min React 3.8 hours, obtain the fire-retardant expandable polystyrene particle that particle diameter 0.8mm contains graphite.
In the present embodiment, the crystalline flake graphite mesh number used is 1300 mesh, and purity is 91%, and the dispersant used is tricresyl phosphate Calcium and the mixture of silicate, the suspending agent used is the mixture of cellulose and polyacrylamide.
Below by following experimental verification beneficial effects of the present invention, below in experiment, the number related to is by weight:
Test one: the preparation method of polymerisation in bulk in 30L reactor of the fire-retardant expandable polystyrene containing crystalline flake graphite:
Step one, it is that the scale graphite of 1000 mesh, the dilauroyl peroxide of 0.3 part, 5 parts of GPPS granules add by 6 parts of mesh numbers To 100 parts of styrene, under the mixing speed of 100rpm, it is heated to 70 DEG C of also isothermal reaction 2 hours, obtains the first mixing Thing.
Step 2,0.25 part of tricalcium phosphate, 0.06 part of cellulose and polyacrylamide Mixture are added in 250 parts of pure water Under the mixing speed of 150rpm, it is heated to 90 DEG C, obtains the second mixture.
Step 3, the first mixture step one obtained add in the second mixture that step 2 obtains, and add 0.8 part six Bromine cyclododecane, 0.1 part of peroxidized t-butyl perbenzoate, 0.3 part of cumyl peroxide 89-90 DEG C of reaction 9 hours until Particle sinks and grain is hard, adds 0.015 part of cellulose, and closed reactor also adds 8 parts of pentanes intensification speed with 1-10 DEG C/min Rate is warming up to 118 DEG C and keeps pressure 0.5-0.8Mpa to continue reaction 3.5 hours.After having reacted, reactor is cooled to 45 DEG C, Discharge washing is dried, and obtains the flame-proofed polystyrene granule containing graphite of particle diameter 0.45-12.mm.
Experiment two: the preparation method of polymerisation in bulk in 2 cubic metres of reactors of the fire-retardant expandable polystyrene containing crystalline flake graphite:
Step one, by 6 part of 1200 mesh, the scale graphite of purity 95%, the dilauroyl peroxide of 0.3 part, 5 parts of GPPS granules Add to 100 parts of styrene, under the mixing speed of 65rpm, be warming up to 70 DEG C, and constant temperature with the heating rate of 35 DEG C/h React 2 hours, obtain the first mixture.
Step 2,0.3 part of 2000 mesh tricalcium phosphate, 0.05 part of cellulose, 0.01 part of polyacrylamide are added to 200 parts In pure water, under the mixing speed of 70rpm, it is warming up to 90 DEG C with the heating rate of 30 DEG C/h, obtains the second mixture.
Adding in step 3, the first mixture 100min step one obtained in the second mixture that step 2 obtains, sampling is seen Examine normal after, add 1 part of HBCD, 0.1 part of peroxidized t-butyl perbenzoate, 0.3 part of cumyl peroxide, 0.5 Part Tissuemat E react 9 hours at 89-90 DEG C, until particle sinks and grain firmly, add 0.015 part of cellulose, 0.3 part 1000 mesh tricalcium phosphates, closed reactor and add 8 parts of pentanes with the heating rate of 12 DEG C/min be warming up to 122 DEG C and keep pressure Power 0.5-0.8MPa continues reaction 3.5 hours.After having reacted, reactor being cooled to 45 DEG C, discharge washing is dried screening and is coated with Layer is also packed, and obtains the flame-proofed polystyrene granule that particle diameter 0.45-1.22mm contains graphite.
Experiment three: the polymerisation in bulk preparation method in 54 cubic metres of reactors of the fire-retardant expandable polystyrene containing crystalline flake graphite:
Step one, the scale graphite by 6 part of 1200 mesh 95% content, the dilauroyl peroxide of 0.3 part, 5 parts of GPPS granules add Enter to 100 parts of styrene, under the mixing speed of 65rpm, be warming up to 70 DEG C with the heating rate of 35 DEG C/h, and constant temperature is anti- Answer 2 hours, obtain the first mixture.
Step 2,0.3 part of 2000 mesh tricalcium phosphate, 0.05 part of cellulose, 0.01 part of polyacrylamide are added to 200 parts Pure water is warming up to 90 DEG C with the heating rate of 30 DEG C/h under the mixing speed of 70rpm, obtains the second mixture.
Adding in step 3, the first mixture 100min step one obtained in the second mixture that step 2 obtains, sampling is seen Examine normal after, add 1 part of HBCD, 0.1 part of peroxidized t-butyl perbenzoate, 0.3 part of cumyl peroxide, 0.5 Part Tissuemat E react 9 hours at 89-90 DEG C, until particle sinks and grain firmly, add 0.015 part of cellulose, 0.3 part 1000 mesh tricalcium phosphates, closed reactor and add 8 parts of pentanes with the heating rate of 12 DEG C/min be warming up to 122 DEG C and keep pressure Power 0.5-0.8MPa continues reaction 3.5 hours.After having reacted, reactor being cooled to 45 DEG C, discharge washing is dried screening and is coated with Layer is also packed, and obtains the flame-proofed polystyrene granule that particle diameter 0.45-1.22mm contains graphite.
Take the fire retardant polystyrene machine-shaping that 50 kilograms of 0.75-1.1mm prepared by above-mentioned experiment contain crystalline flake graphite respectively, To the styrofoam of a piece 2.8 cubic metres, use target GB8624-2012 to carry out flame retardant rating test, use the world GB/T10294-2008 carries out Determination of conductive coefficients.Result be the graphite polystyrene board flame retardant rating prepared by the present invention be B1 level, Oxygen index (OI) is 35, and heat conductivity is 0.033W/ (m.k).
In the present invention, it is 1000~1500 mesh that crystalline flake graphite preferably employs mesh number, and purity is the graphite of 90~95%;Described divides Powder is not limited to use the material disclosed in embodiment, can use tricalcium phosphate, thenardite, silicate, sodium hexameta phosphate In one or more mixture being mixed by any ratio;Described suspending agent is also not necessarily limited to use the material disclosed in embodiment, One or more in triethyl group hexyl phosphoric acid, methyl anyl alcohol, cellulose, polyacrylamide can be used to be mixed by any ratio Mixture.
In above-described embodiment, the GPPS granule of employing is high impact polystyrene granule.
The foregoing is only presently preferred embodiments of the present invention, be not whole embodiments of the present invention, not in order to limit this Bright, all within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in this Within bright protection domain.
In addition to technical characteristic described in description, remaining technical characteristic is all known to a person skilled in the art technology, in order to highlight this Bright innovative characteristics, above-mentioned technical characteristic does not repeats them here.

Claims (10)

1. the fire-retardant expandable polystyrene containing crystalline flake graphite, is characterized in that, including: 100 parts of styrene, 1~10 part of phosphorus sheet Graphite, 100~250 parts of pure water, 0.1~1 part of dilauroyl peroxide, 0.05~0.1 part of peroxidized t-butyl perbenzoate, 0.5~ 1 part of HBCD, 0.1~0.5 part of cumyl peroxide, 0.1~0.3 part of dispersant, 0.025~0.075 part of suspension Agent, 1~5 part of General Purpose Polystyrenre granule, 0.1~0.5 part of Tissuemat E and 7~10 parts of pentanes, above number is all with weight Meter.
2. the preparation method of the fire-retardant expandable polystyrene polymerisation in bulk containing crystalline flake graphite, is characterized in that, comprise the following steps:
Step 1: weigh by weight 100 parts of styrene, 1~10 part of scale graphite, 100~250 parts of pure water, 0.1~1 Part dilauroyl peroxide, 0.05~0.1 part of peroxidized t-butyl perbenzoate, 0.5~1 part of HBCD, 0.1~0.5 part Cumyl peroxide, 0.1~0.3 part of dispersant, 0.025~0.075 part of suspending agent, 1~5 part of General Purpose Polystyrenre Grain, 0.1~0.5 part of Tissuemat E and 7~10 parts of pentanes;
Step 2: the crystalline flake graphite, dilauroyl peroxide and the General Purpose Polystyrenre granule that step 1 are weighed are put into step 1 and claimed In the styrene taken, heat while stirring, obtain the first mixture;
Step 3: dispersant step 1 weighed and suspending agent add in the pure water that step 1 weighs, and add while stirring Heat, obtains the second mixture;
Step 4: described first mixture is joined in described second mixture, and adds the benzoyl peroxide weighed in step 1 After t-butyl formate, HBCD, cumyl peroxide and Tissuemat E, reaction to particle sinking grain are hard, add The pentane that step 1 weighs, is warming up to more than 115 DEG C and keeps pressure 0.5Mpa~0.8Mpa to react 3~4 hours, having reacted Cheng Hou, is cooled to less than 50 DEG C, obtains the fire-retardant expandable polystyrene particle that particle diameter 0.45~1.2mm contains graphite.
Preparation method the most according to claim 2, is characterized in that, the mesh number of described crystalline flake graphite is 1000~1500 mesh, Purity is 90~95%.
Preparation method the most according to claim 2, is characterized in that, described dispersant be tricalcium phosphate, thenardite, One or more mixture being mixed by any ratio in silicate, sodium hexameta phosphate.
Preparation method the most according to claim 2, is characterized in that, described suspending agent is triethyl group hexyl phosphoric acid, methyl One or more mixture being mixed by any ratio in amylalcohol, cellulose, polyacrylamide.
Preparation method the most according to claim 2, is characterized in that, in step 2, the speed of stirring is 60~150rpm, Heating-up temperature is 65~75 DEG C, and course of reaction is isothermal reaction 1.8~2.5 hours.
Preparation method the most according to claim 2, is characterized in that, in step 3, the speed of stirring is 70~160rpm, Heating-up temperature is 85~95 DEG C.
Preparation method the most according to claim 2, is characterized in that, described General Purpose Polystyrenre granule is high-impact polyphenyl Ethylene granule.
Preparation method the most according to claim 2, is characterized in that, in step 4, and the reaction condition that particle sinks and grain is hard For: react 9~10 hours under the temperature conditions of 85~95 DEG C.
Preparation method the most according to claim 2, is characterized in that, in step 4, after adding pentane, and liter during intensification Temperature speed is 1~10 DEG C/min.
CN201610368402.6A 2016-05-30 2016-05-30 Flame-retardant expandable polystyrene containing flake graphite and body polymerization preparation method thereof Pending CN105949360A (en)

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