CN106590192A - Fireproof transition metal-loaded polystyrene building material and preparation method thereof - Google Patents
Fireproof transition metal-loaded polystyrene building material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D125/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
- C09D125/02—Homopolymers or copolymers of hydrocarbons
- C09D125/04—Homopolymers or copolymers of styrene
- C09D125/06—Polystyrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers 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
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a fireproof transition metal-loaded polystyrene building material. The polystyrene building material is prepared from the following raw materials in parts by weight: 6-8 parts of zirconium oxychloride, 7-9 parts of nickel chloride, 10-14 parts of graphene oxide, 20-30 parts of styrene, 0.1-0.2 part of benzoyl peroxide, 100-110 parts of polystyrene, 0.6-1 part of aluminum ammonium sulfate, 0.1-0.3 part of calcium naphthenate, 3-4 parts of polyether glycol, 0.6-1 part of 1, 2-dimethylimidazole, 3-4 parts of water and zinc borate, 0.3-1 part of butyl tin mercaptide, 1-2 parts of ammonium polyphosphate, 4-7 parts of talcum powder, and 0.1-0.4 part of butyl oleate. The water, zinc borate, butyl tin mercaptide, ammonium polyphosphate and talcum powder are added, so that the flame retardancy and fire resistance of the finished product can be effectively improved, and the safety of the finished product can be improved.
Description
Technical field
The present invention relates to building material technical field, more particularly to a kind of polystyrene building of fire prevention carrying transition metal
Material and preparation method thereof.
Background technology
Polymer nanocomposites（By polymeric matrix（Continuous phase）With nano-filled dose（Dispersion phase）Composition.Wherein,
The yardstick of nano-filled dose of at least one dimension is less than nanometer.Good dividing is formed in polymeric matrix when nano-filled dose
Dissipate, can significantly improve the performance of nano composite material.Compared to traditional polymer composites, polymer nanocomposite composite wood
The consumption of the filler of material is low, effect is significant；
The performance of polymer nanocomposites is affected by two big factors：Nano-filled dose of dispersibility and nano-filled dose with
Interfacial interaction between polymeric matrix；Dispersibility（Dispersibility refers to dispersion feelings of the nanoparticle in polymeric matrix
Condition.Nanoparticle generally has stronger reunion tendency, and the specific surface area for causing filler reduces, affects between filler and matrix
Surface energy and interfacial interaction, so as to affect the performance of composite, interfacial interaction：Nano-filled dose and polymer
Interfacial interaction between matrix is the key factor for causing changes in material properties, and important to being dispersed with for nanoparticle
Affect.When interfacial interaction is stronger, nanoparticle easily forms good dispersion, and the performance of composite is improved more
Substantially；
Polymer laminar compound nano composite has lot of advantages, and first, dispersion phase is two-dimensional layer nano material, than
Surface area is big；Secondly, two-dimensional layered structure forms lamella blocking effect, can significantly increase material gas barrier property and
Heat stability；Again, many performances can simultaneously be improved；
The fire safety performance of polymeric material is the important topic that polymer grinds the field of making internal disorder or usurp.The fire of polymer
Safety refers to security performance during polymer combustion, mainly discharges, poisons including ignition temperature, the combustion heat
The contents such as the release of property flue gas.Polymer is widely used in the every field of human being's production and life.Most polymers
Main component be carbon and hydrogen, be susceptible to decompose and burn when being heated, belong to combustible material.During polymer combustion, release
Substantial amounts of light, heat and toxic flue gas are released, is the main cause for causing casualties in fire.Improve polymeric material fire peace
The technology of full performance is commonly known as flame-retarded technology；
Improving the method for flame retardance of polymer performance can be divided into two big class, and the first kind is, by MOLECULE DESIGN, to give polymer point
Sub- ignition-proof element or flame retarding construction, so as to improve the fire resistance of polymer；Equations of The Second Kind is by adding fire retardant, so as to improve
The fire resistance of polymeric material.Wherein, Equations of The Second Kind is the wide variety of method of plastics industry, with technology maturation, low cost
And it is easy to process the advantages of.Conventional fire retardant has bromide fire retardant, APP, hydroxide trick, magnesium hydroxide, red phosphorus and three
Poly cyanamid etc..Over nearly 15 years, flame-retardant polymer nano composite material has obtained extensive research.Wherein, polymer laminar without
Machine thing nano composite material, it is only necessary to less addition, you can obtain obvious flame retardant effect, and environmental protection, be considered
One of important developing direction of field of fire-proof technology；
The lamella blocking effect of graphene sheet layer is the heat stability and fire safety for improving graphene/polymer nano composite material
The principal element of performance, and its high-termal conductivity often leads to the reduction of polymer nanocomposites pyrolysis temperature, ignition temperature and carries
Before.But, with regard to the interfacial interaction between Graphene and polymer in GPNC heat stability and fire safety performance is improved
Effect, also clearly do not studied；The high-termal conductivity of Graphene is unfavorable for that it improves polymer thermostable and fire peace
Full performance.The physics and chemical property of Graphene can be changed by surface modification, so as to open up a raising Graphene/polymerization
The technology path of thing nano composite material heat stability and fire safety performance.The research of flame retardance of polymer technical field shows, portion
Divide transition metal that there is the effect of catalyzing and carbonizing and capture free radical, be conducive to improving the heat stability and anti-flammability of polymer
Can, such as, zirconium is acted in the pyrolysis of polymer and combustion process with catalysis carbon-forming, and nickel is not only acted on catalysis carbon-forming,
Also there is the effect of absorption free radical.Therefore, transition metal is supported on Graphene, it is possible to have than simple Graphene
Preferably improve the effect of heat stability and fire safety performance.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of polyphenyl second of fire prevention carrying transition metal
Alkene construction material and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of polystyrene construction material of fire prevention carrying transition metal, it is by made by the raw material of following weight parts：
Zirconium oxychloride 6-8, Nickel dichloride. 7-9, graphene oxide 10-14, styrene 20-30, dibenzoyl peroxide 0.1-0.2,
Polystyrene 100-110, Burnt ammonium alum 0.6-1, calcium naphthenate 0.1-0.3, polyether Glycols 3-4,1,2- methylimidazoles
0.6-1, water and Firebrake ZB 3-4, thiol-butyl tin 0.3-1, APP 1-2, Pulvis Talci 4-7, butyl oleate 0.1-0.4.
A kind of preparation method of the polystyrene construction material of described fire prevention carrying transition metal, comprises the following steps：
（1）Above-mentioned Burnt ammonium alum is added in the deionized water of its weight 30-45 times, is stirred, add above-mentioned water and boron
Sour zinc, APP, it is 65-70 DEG C to rise high-temperature, insulated and stirred 5-10 minute, obtains fire-retardant dispersion liquid；
（2）Above-mentioned 1,2- methylimidazoles are added in the dehydrated alcohol of its weight 10-14 times, are stirred, rise high-temperature
For 51-60 DEG C, above-mentioned calcium naphthenate is added, insulated and stirred 10-20 minute, add the 30-40% of above-mentioned styrene weight, stirring
To room temperature, monomeric polyol dispersion liquid is obtained；
（3）Above-mentioned graphene oxide is added in the deionized water of its weight 200-300 times, supersound process 100-120 minute,
Obtain graphene dispersing solution；
（4）By above-mentioned zirconium oxychloride, Nickel dichloride., Pulvis Talci mixing, in being added to the deionized water of compound weight 70-100 times,
Stir, mix with graphene dispersing solution, fire-retardant dispersion liquid, stir, in being sent to reactor, Deca concentration is 10-
14% ammonia, regulation pH is 10-11, and it is 190-200 DEG C to rise high-temperature, and insulated and stirred 6-7 hour, discharging, sucking filtration will be precipitated
Washing 2-3 time, is dried 20-25 hours at 76-80 DEG C, obtains pretreating graphite alkene；
（5）Above-mentioned pretreating graphite alkene is added in the dimethylformamide of its weight 100-110 times, ultrasonic 1-2 hours are obtained
Amide dispersion liquid；
（6）Remaining styrene is taken, in being added to the dimethylformamide of its weight 17-20 times, stirring reaction 16-20 minute,
Mix with above-mentioned amide dispersion liquid, monomeric polyol dispersion liquid, stir, add above-mentioned dibenzoyl peroxide, be passed through nitrogen,
Insulated and stirred 1-2 hour at 70-75 DEG C, in sending into baking oven, is dried complete, discharging cooling at 120-130 DEG C, obtains polymer and changes
Property Graphene；
（7）By above-mentioned polyether Glycols at 76-80 DEG C insulated and stirred 17-20 minute, add above-mentioned calcium naphthenate, insulated and stirred
3-10 minutes, above-mentioned thiol-butyl tin, polymer modification Graphene are added, stirred to room temperature, obtain pretreatment polymer modification stone
Black alkene；
（8）Above-mentioned pretreatment polymer modification Graphene, polystyrene are mixed, remaining each raw material is added, is stirred, sent into
To in banbury, it is 180-190 DEG C to rise high-temperature, Heat preservation 10-12 minutes, is cooled to room temperature, in sending into vulcanizing press,
Under 190-200 DEG C, 10-15MPa, fine powder is worn in pressurize 3-4 minutes, cooling, obtains final product.
It is an advantage of the invention that：Zirconium oxide and hydroxide that the present invention passes through the monoclinic phase in graphite oxide area load
Nickel, and while graphite oxide is reduced to into Graphene, the heat stability of composite depends on the lamella obstruct of graphene sheet layer
Interfacial interaction between effect and Graphene and polymer, and the basic structure of Graphene is conjugation hexatomic ring, it is and poly-
There is π-π interactions in the phenyl ring in styrene, form good leafing dispersity, effectively raises Graphene and is polymerized
Interfacial interaction between thing, the heat that carrying transition metal can further improve graphite dilute polymer nano composite material is steady
, there is synergistic effect in qualitative and fire safety performance, there is 2 reasons between the zirconium or nickel and graphite coal of the present invention：Zirconium is in polymer
Pyrolysis and combustion process in catalysis carbon-forming effect, can promote material formed protectiveness layer of charcoal, nickel not only have urge
Chemical conversion charcoal effect, also with the effect of absorption free radical；And graphite is dilute with more preferable lamella blocking effect, so as to reduce pyrolysis
The diffusion of product and effusion；Effectively raise the heat stability and fire resistance of finished product；The water and Firebrake ZB of present invention addition,
Thiol-butyl tin, APP, Pulvis Talci etc., can effectively improve the fire-retardant fireproof of finished product, improve the safety of material.
Specific embodiment
A kind of polystyrene construction material of fire prevention carrying transition metal, it is by made by the raw material of following weight parts：
Zirconium oxychloride 6, Nickel dichloride. 7, graphene oxide 10, styrene 20, dibenzoyl peroxide 0.1, polystyrene 100, sulfur
Sour aluminum ammonium 0.6, calcium naphthenate 0.1, the methylimidazole 0.6, water of polyether Glycols 3,1,2 and Firebrake ZB 3, thiol-butyl tin 0.3,
APP 1, Pulvis Talci 4, butyl oleate 0.1.
A kind of preparation method of the polystyrene construction material of described fire prevention carrying transition metal, comprises the following steps：
（1）Above-mentioned Burnt ammonium alum is added in the deionized water of 30 times of its weight, is stirred, add above-mentioned water and boric acid
Zinc, APP, it is 65 DEG C to rise high-temperature, and insulated and stirred 5 minutes obtains fire-retardant dispersion liquid；
（2）Above-mentioned 1,2 methylimidazole is added in the dehydrated alcohol of 10 times of its weight, is stirred, it is 51 to rise high-temperature
DEG C, add above-mentioned calcium naphthenate, insulated and stirred 10 minutes to add the 30% of above-mentioned styrene weight, stir to room temperature, obtain monomer
Alcohol dispersion liquid；
（3）Above-mentioned graphene oxide is added in the deionized water of 200 times of its weight, supersound process 100 minutes obtains Graphene
Dispersion liquid；
（4）By above-mentioned zirconium oxychloride, Nickel dichloride., Pulvis Talci mixing, in being added to the deionized water of 70 times of compound weight, stirring
Uniformly, mix with graphene dispersing solution, fire-retardant dispersion liquid, stir, in being sent to reactor, Deca concentration is 10% ammonia
Water, it is 10 to adjust pH, and it is 190 DEG C to rise high-temperature, insulated and stirred 6 hours, discharging, sucking filtration, by precipitation washing 2 times, at 76 DEG C
It is dried 20 hours, obtains pretreating graphite alkene；
（5）Above-mentioned pretreating graphite alkene is added in the dimethylformamide of 100 times of its weight, ultrasound 1 hour obtains amide point
Dispersion liquid；
（6）Remaining styrene is taken, in being added to the dimethylformamide of 17 times of its weight, stirring reaction 16 minutes is and above-mentioned
Amide dispersion liquid, the mixing of monomeric polyol dispersion liquid, stir, and add above-mentioned dibenzoyl peroxide, nitrogen are passed through, at 70 DEG C
Insulated and stirred 1 hour, in sending into baking oven, is dried complete, discharging cooling at 120 DEG C, obtains polymer modification Graphene；
（7）By above-mentioned polyether Glycols at 76 DEG C insulated and stirred 17 minutes, add above-mentioned calcium naphthenate, insulated and stirred 3 minutes,
Above-mentioned thiol-butyl tin, polymer modification Graphene are added, is stirred to room temperature, obtain pretreatment polymer modification Graphene；
（8）Above-mentioned pretreatment polymer modification Graphene, polystyrene are mixed, remaining each raw material is added, is stirred, sent into
To in banbury, it is 180 DEG C to rise high-temperature, and Heat preservation 10 minutes is cooled to room temperature, in sending into vulcanizing press, 190
DEG C, under 10MPa, fine powder is worn in pressurize 3 minutes, cooling, obtains final product.
Performance test:
Tensile strength（MPa）:11.7；
Elongation at break（%）：78；
Bending strength（MPa）：20.7.
Claims (2)
1. it is a kind of fire prevention carrying transition metal polystyrene construction material, it is characterised in that it is by the original of following weight parts
Made by material：
Zirconium oxychloride 6-8, Nickel dichloride. 7-9, graphene oxide 10-14, styrene 20-30, dibenzoyl peroxide 0.1-0.2,
Polystyrene 100-110, Burnt ammonium alum 0.6-1, calcium naphthenate 0.1-0.3, polyether Glycols 3-4,1,2- methylimidazoles
0.6-1, water and Firebrake ZB 3-4, thiol-butyl tin 0.3-1, APP 1-2, Pulvis Talci 4-7, butyl oleate 0.1-0.4.
2. a kind of preparation method of the polystyrene construction material of fire prevention carrying transition metal as claimed in claim 1, it is special
Levy and be, comprise the following steps：
（1）Above-mentioned Burnt ammonium alum is added in the deionized water of its weight 30-45 times, is stirred, add above-mentioned water and boron
Sour zinc, APP, it is 65-70 DEG C to rise high-temperature, insulated and stirred 5-10 minute, obtains fire-retardant dispersion liquid；
（2）Above-mentioned 1,2- methylimidazoles are added in the dehydrated alcohol of its weight 10-14 times, are stirred, rise high-temperature
For 51-60 DEG C, above-mentioned calcium naphthenate is added, insulated and stirred 10-20 minute, add the 30-40% of above-mentioned styrene weight, stirring
To room temperature, monomeric polyol dispersion liquid is obtained；
（3）Above-mentioned graphene oxide is added in the deionized water of its weight 200-300 times, supersound process 100-120 minute,
Obtain graphene dispersing solution；
（4）By above-mentioned zirconium oxychloride, Nickel dichloride., Pulvis Talci mixing, in being added to the deionized water of compound weight 70-100 times,
Stir, mix with graphene dispersing solution, fire-retardant dispersion liquid, stir, in being sent to reactor, Deca concentration is 10-
14% ammonia, regulation pH is 10-11, and it is 190-200 DEG C to rise high-temperature, and insulated and stirred 6-7 hour, discharging, sucking filtration will be precipitated
Washing 2-3 time, is dried 20-25 hours at 76-80 DEG C, obtains pretreating graphite alkene；
（5）Above-mentioned pretreating graphite alkene is added in the dimethylformamide of its weight 100-110 times, ultrasonic 1-2 hours are obtained
Amide dispersion liquid；
（6）Remaining styrene is taken, in being added to the dimethylformamide of its weight 17-20 times, stirring reaction 16-20 minute,
Mix with above-mentioned amide dispersion liquid, monomeric polyol dispersion liquid, stir, add above-mentioned dibenzoyl peroxide, be passed through nitrogen,
Insulated and stirred 1-2 hour at 70-75 DEG C, in sending into baking oven, is dried complete, discharging cooling at 120-130 DEG C, obtains polymer and changes
Property Graphene；
（7）By above-mentioned polyether Glycols at 76-80 DEG C insulated and stirred 17-20 minute, add above-mentioned calcium naphthenate, insulated and stirred
3-10 minutes, above-mentioned thiol-butyl tin, polymer modification Graphene are added, stirred to room temperature, obtain pretreatment polymer modification stone
Black alkene；
（8）Above-mentioned pretreatment polymer modification Graphene, polystyrene are mixed, remaining each raw material is added, is stirred, sent into
To in banbury, it is 180-190 DEG C to rise high-temperature, Heat preservation 10-12 minutes, is cooled to room temperature, in sending into vulcanizing press,
Under 190-200 DEG C, 10-15MPa, fine powder is worn in pressurize 3-4 minutes, cooling, obtains final product.
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Application publication date: 20170426 |