CN105419140A - Building heat preservation material with excellent fireproof performance - Google Patents

Building heat preservation material with excellent fireproof performance Download PDF

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Publication number
CN105419140A
CN105419140A CN201610049174.6A CN201610049174A CN105419140A CN 105419140 A CN105419140 A CN 105419140A CN 201610049174 A CN201610049174 A CN 201610049174A CN 105419140 A CN105419140 A CN 105419140A
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graphene
section
mass ratio
polystyrene
compound
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郑舒元
郑力华
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SHENZHEN MT FLOURING CARBIDE TECHNOLOGY Co Ltd
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SHENZHEN MT FLOURING CARBIDE TECHNOLOGY Co Ltd
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Priority to CN201610049174.6A priority Critical patent/CN105419140A/en
Publication of CN105419140A publication Critical patent/CN105419140A/en
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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
    • C08L25/00—Compositions 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; Compositions of derivatives of such polymers
    • C08L25/02—Homopolymers or copolymers of hydrocarbons
    • C08L25/04—Homopolymers or copolymers of styrene
    • C08L25/06—Polystyrene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • 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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a building heat preservation material with excellent fireproof performance. The building heat preservation material is prepared from a mixture of graphene, zirconia, alumina and polystyrene; a mass ratio between the total mass of graphene-zironia-alumna and the mass of the polystyrene is preferably (1 to 6) to (1 to 8). Compared with the prior art, the building heat preservation material disclosed by the invention has better flame retardancy and low smoke density, is toxity-free and pollution-free, has a higher fireproof grade and accords with an environment protection requirement.

Description

A kind of building thermal insulation material of fire resistance excellence
Technical field
The present invention relates to a kind of material of construction, particularly relate to a kind of lagging material for building.
Background technology
In the art, widely used lagging material is Expandable Polystyrene (EPS).Polystyrene, molecular formula is C 8h 8, be mainly used in foaming, be used as insulation, heat insulation, shockproof and wrapping material.Foamed polystyrene is shaped to spherical granules, is foam, and this foam wt is light, and heat-proof quality is good, adds in cement material and mixes with cement, dry and can prepare building light-weight material, have insulation, fire prevention, the performances such as waterproof.But due to polystyrene have inflammable, the amount of being fuming is large, dropping is many, after burning in the feature such as amorphous viscous liquid, burning grade is not high, does not meet the requirement that present materials for wall fire-protection rating is higher.In addition, in heat-preserving wall prepared by polystyrene in early days and cement mixing, also there is mixing uneven, or the peeling etc. that in long-time body of wall, water loss causes, limit polystyrene applying in warming plate.
In order to better use polystyrene to manufacture warming plate, play the advantage of its good heat insulating, the compound insulating material that people make after have developed and being mixed with polystyrene by various inorganic or organic materials.At the initial stage, in order to improve the flame retardant properties of polystyrene thermal insulation plate, people add organic fire-retardant and play flame retardant effect in Expandable Polystyrene (EPS).Organic fire-retardant comprises halogen containing flame-retardant, such as hexabromocyclododecane, TDE, decabromodiphynly oxide etc., but owing to can produce a large amount of smog when halogen containing flame-retardant burns, does not reach environmental requirement, is unsuitable for its big area and uses.
Afterwards, people, using expanded graphite as fire retardant, obtained foamable polystyrene particle after it being mixed with polystyrene, improved flame retardant resistance, heat retaining property and intensity after compression molding.Wherein expansible black lead is coated on the surface of polystyrene foaming granule as fire retardant, not containing organic fire-retardant, the method has good effect to the flame retardant resistance improving polystyrene, but its shortcoming is, fire-retardant principle due to expansible black lead produces when meeting fire to expand, thus carbonization is fire-retardant, but the skeleton of coating layer can destroy by expanded graphite in expansion carbonization process, can produce powder phenomenon-tion; Secondly, micronic dust, particulate and slag-off phenomenon can be produced during expansion, even also produce Mars, not meet national associated safety regulation, there is potential safety hazard.
Except the component comprised in the matrix material mixed with polystyrene research, people also study at the special coating of surface-coated one deck of matrix material, thus strengthen its flame retardant properties further.In a kind of polystyrene foam composite heat insulatant thermal insulation material, adopt resol and expansible black lead, capsule red phosphorus, nano-aluminum hydroxide as coating, by the compression molding behind expandable polystyrene particle surface of this applying coating.But because red phosphorus can generate Vanadium Pentoxide in FLAKES when burning, and the Vanadium Pentoxide in FLAKES moisture content absorbed further in air can become phosphoric acid, produces corrosion to matrix building materials; In addition, during preparation need using after resol and other mixing material stir in high-speed mixer as paint in polystyrene foaming granule, due to the curing characteristics of resol, in actual production, after the preparation time is slightly long, coating is easily solidified into block, cannot continue to use, cause loss too large, improve production cost.
Along with technical development, people have developed in another kind of polystyrene foam composite heat insulatant thermal insulation material, adopt phenolic aldehyde or furane resin as the method for external phase compound Expandable Polystyrene (EPS), combine phenolic aldehyde or the good flame retardant properties of furane resin and polystyrene good heat-insulating property, it is a kind of solution preferably, but also existing defects in actual applications, because the conjugation of polystyrene is inadequate, causes its intensity to reduce; Due to free monomers such as fire-retardant, phenol, toxicity is large aborning, organic volatile is many, brings pollution to environment, affects the health of staff.In a kind of organic polystyrene foamed lagging material of the same type, wherein with vinyl acetate resin as functional skin layer, then compound add fire retardant make flame-retardant polystyrene.The shortcoming of this material is that polyvinyl acetate must adopt dissolve with methanol to become solution, and due to the easy adhesion of granules of polystyrene, must spray ethylene glycol stripper polystyrene just can be made to become independently particle when stirring; Meanwhile, because polyvinyl acetate does not have when heating or add solidifying agent and curable performance, thus the addition of fire retardant is limited, and product can produce deterioration when molded, cannot in conjunction with or curing molding; In addition, during production, use poisonous, inflammable methyl alcohol, ethylene glycol volatile, also have disadvantageous effect to the health of staff and environment.
For the deficiencies in the prior art, those skilled in the art wish to research and develop polystyrene compound insulating material that flame retardant properties is good, Environmental Safety, cost are low and preparation method thereof.
Summary of the invention
The invention discloses a kind of building thermal insulation material and manufacture method thereof of fire resistance excellence, this material has better flame retardant properties and low smoke density compared to existing technology, and nontoxic pollution-free has higher fire-protection rating, meets environmental requirement.
Fire-retardant heat insulation plate of the present invention comprises the compound of Graphene, zirconium white, aluminum oxide and polystyrene, and the gross weight of Graphene-Zirconia-alumina and the mass ratio of polystyrene are preferably 1:6 ~ 1:8.
Further, resol and solidifying agent is also comprised; The mass ratio of compound and resol is 25:1 ~ 28:1; The mass ratio of resol and solidifying agent is 3:1 ~ 4:1; Wherein, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid.
Further, also topcoating is comprised; Described coating comprises aluminium hydroxide, zirconium white, Graphite Powder 99, laterite, breeze, ceramics powder.In above-mentioned coating, the parts by weight of each component are: aluminium hydroxide 20, zirconium white 40, Graphite Powder 99 5, laterite 20, breeze 5, ceramics powder 10.
The manufacture method of fire-retardant heat insulation plate of the present invention, comprises the following steps:
One, prepare Graphene, comprise the steps:
(1) expanded graphite is prepared.Wherein, first graphite oxide is placed in crucible, then retort furnace is heated to certain temperature, crucible is put into after retort furnace after held for some time, crucible is taken out, obtained expanded graphite.Wherein, the heating rate of heating muffle stove is preferably 10 ~ 15 DEG C/min, preferably retort furnace is heated to 1000 ~ 1100 DEG C, and the soaking time of crucible in retort furnace is preferably 3 ~ 5min.
(2) expanded graphite is scattered in water, ultrasonic after adding polystyrene sphere aqueous dispersions, obtained expanded graphite-polystyrene composite dispersion liquid; Wherein, the mass ratio of expanded graphite and water is 1:1 ~ 1:2, and the mass ratio of expanded graphite and polystyrene sphere aqueous dispersions is 80:1 ~ 60:1, the preferred 2h ~ 3h of ultrasonic time;
(3) by expanded graphite-polystyrene composite dispersion liquid suction filtration in nickel foam, load had the nickel foam of expanded graphite-polystyrene to be placed in the mixing solutions of hydrazine hydrate and ammoniacal liquor after drying, after reaction, get Graphene-polystyrene base material; Wherein, the speed of suction filtration is preferably 3 ~ 4L/s, drying temperature preferably 50 ~ 60 DEG C, and time of drying is 10 ~ 13h preferably, and hydrazine hydrate and ammoniacal liquor volume ratio are 1:5 ~ 1:10, and temperature of reaction is preferably at 80 ~ 85 DEG C;
(4) Graphene-polystyrene base material is warming up to 600 ~ 650 DEG C in vacuum tube furnace, take out after insulation 2 ~ 3h, wherein, temperature rise rate is preferably 3 ~ 4 DEG C/min, obtains Graphene.
Two, Graphene-Zirconia-alumina matrix material is prepared;
(1) mixed with aluminic acid ammonia by the Graphene obtained in step one, ball milling is Graphene-aluminic acid ammonia matrix material; Wherein, the mass ratio of Graphene and aluminic acid ammonia is preferably 1:1-3:1; Adopt ball mill to matrix material ball milling, the rotating speed of ball milling is preferably 200-280rpm;
(2) above-mentioned Graphene-aluminic acid ammonia matrix material is heated to 800-950 DEG C, is incubated under nitrogen protection, lowers the temperature, obtain Graphene-alumina compound; Wherein, can carry out heating, be incubated and lower the temperature in tube furnace, the temperature rise rate of heating be 5-10 DEG C/min, and soaking time is 2-4h, is then down to room temperature, adopts the mode of Temperature fall.
(3) mixed with nano zircite by Graphene-alumina compound, ball milling obtains Graphene-Zirconia-alumina matrix material; Wherein, the mass ratio of Graphene-alumina compound and nano zircite is preferably 3:1-4:1; The rotational speed of ball-mill of ball mill is preferably 300-350rpm.
Three, fire-retardant heat insulation compound is prepared;
(1) Graphene-Zirconia-alumina matrix material is mixed with polystyrene after making solution; Wherein, in Graphene-Zirconia-alumina aqueous solution, the mass ratio of Graphene-Zirconia-alumina and water is 1:20 ~ 1:25; The mass ratio of Graphene-Zirconia-alumina and polystyrene is preferably 1:6 ~ 1:8;
(2) in above-mentioned mixing solutions, add resol and solidifying agent, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid; In mixing solutions, the mass ratio of compound and resol is 25:1 ~ 28:1; The mass ratio of resol and solidifying agent is 3:1 ~ 4:1.The physical strength of the sheet material of the fire-retardant heat insulation plate obtained outward in this ratio ranges is not good.Wherein the mass percentage of sulfuric acid is 97%, and the mass percentage of phosphoric acid is 38%; The mass ratio of water and sulfuric acid is 2:1 ~ 3:1; The mass ratio of water and phosphoric acid is 1.5:1 ~ 2:1; Obtain fire-retardant heat insulation compound.
Four, fire-retardant heat insulation plate is prepared;
(1) in the first twin screw extruder, melt-mixed material is obtained; Compound is added in the first twin screw extruder, obtain the compound of melting.Wherein, the work area in the first twin screw extruder is divided into seven sections: the first to the 3rd section is intensification melt zone, and the 4th to the 5th section is that melting is pressurizeed mixing district, and six to SECTOR-SEVEN section is the mixing district of high pressure-temperature.Wherein, the first zone temperatures 120 DEG C; Second section 150 DEG C; 3rd section 170 DEG C, pressure 3Mpa; 4th zone temperatures 190 DEG C, pressure 8MPa; 5th zone temperatures 210 DEG C, pressure 11Mpa; 6th zone temperatures 220 DEG C, pressure 18MPa, SECTOR-SEVEN section temperature 200 DEG C, pressure 22Mpa.
(2) at the SECTOR-SEVEN section end of the first screw extrusion press, in the compound of melting, supercritical carbon dioxide fluid is added; The mass ratio of supercritical carbon dioxide fluid and compound is about 80:1 ~ 90:1, filling pressure 24MPa.
(3) compound of melting is carried out part mixing; Homogenizing barrier and releasing tube is provided with between first twin screw extruder outlet and the second screw extrusion press the 9th section.Partial blend enters the front end of Section Eight section by the squeezing passage between Section Eight Duan Yu nine section of the second screw extrusion press, after enter the 9th section by the screw extruding of Section Eight section; Partial blend enters the 9th section of the second screw extrusion press by homogenizing barrier and releasing tube, advances through screw extruding; Thus it is mixing to realize part.Wherein, the mass ratio entering the melt-mixed material of Section Eight section and the 9th section is 1:1.
(4) mixture particle is obtained by the second screw machine forcing machine; Second screw extrusion press is divided into five sections, is Section Eight Duan Zhi Twelve-section respectively.Section Eight Duan Zhi ten section is cooling decompression district; 11 section is dynamic mixing district, and Twelve-section is static mixing district.Wherein, Section Eight section temperature 150 DEG C, pressure 16MPa, the 9th zone temperatures 70 DEG C, pressure 20MPa, the tenth zone temperatures 50 DEG C, pressure 15MPa; 11 zone temperatures 40 DEG C, pressure 13MPa; Twelve-section temperature 80 DEG C, pressure 10Mpa.At Twelve-section end, extrusion die is installed, the temperature in die head region 90 DEG C, pressure 8Mpa.
(5) fire-retardant heat insulation plate is made with compound particles.
According to another implementation of the invention, the present invention is before making fire-retardant heat insulation plate with compound particles, first compound particles is mixed with a coating, stirring makes coating evenly be coated on particle surface, again the compound particles being coated with coating is made fire-retardant heat insulation plate, because this coating has well fire-retardant, low cigarette effect, therefore, further increase the fire-protection rating of fire-retardant heat insulation plate, and meet environmental requirement.
Flame-retardant low-smoke coating of the present invention, comprises the component of following weight parts: aluminium hydroxide 15 ~ 25, zirconium white 35 ~ 45, Graphite Powder 99 3 ~ 7, laterite 15 ~ 25, breeze 4 ~ 6, ceramics powder 8 ~ 12.
The method preparing this Flame-retardant low-smoke coating is, by the aluminium hydroxide of said components, zirconium white, Graphite Powder 99, laterite, breeze, ceramics powder, polystyrene, epoxy resin, dimethylaminopropylamine mixing, melting mixing coating is obtained by twin screw extruder, extrude, compressing tablet, air-cooled, abrasive dust, sieve, obtain Flame-retardant low-smoke coating.Then, compound particles is mixed with this coating, tensio-active agent, stir, make coating evenly be coated on particle surface, finally make fire-retardant heat insulation plate with the compound particles being coated with coating.
Embodiment
The manufacture method of fire-retardant heat insulation plate disclosed by the invention, comprises the following steps:
One, prepare Graphene, comprise the steps:
(1) expanded graphite is prepared.Wherein, first graphite oxide is placed in crucible, then retort furnace is heated to certain temperature, crucible is put into after retort furnace after held for some time, crucible is taken out, obtained expanded graphite.Wherein, the heating rate of heating muffle stove is preferably 10 ~ 15 DEG C/min, preferably retort furnace is heated to 1000 ~ 1100 DEG C, and the soaking time of crucible in retort furnace is preferably 3 ~ 5min.
(2) expanded graphite is scattered in water, ultrasonic after adding polystyrene sphere aqueous dispersions, obtained expanded graphite-polystyrene composite dispersion liquid; Wherein, the mass ratio of expanded graphite and water is 1:1 ~ 1:2, and the mass ratio of expanded graphite and polystyrene sphere aqueous dispersions is 80:1 ~ 60:1, the preferred 2h ~ 3h of ultrasonic time;
(3) by expanded graphite-polystyrene composite dispersion liquid suction filtration in nickel foam, load had the nickel foam of expanded graphite-polystyrene to be placed in the mixing solutions of hydrazine hydrate and ammoniacal liquor after drying, after reaction, get Graphene-polystyrene base material; Wherein, the speed of suction filtration is preferably 3 ~ 4L/s, drying temperature preferably 50 ~ 60 DEG C, and time of drying is 10 ~ 13h preferably, and hydrazine hydrate and ammoniacal liquor volume ratio are 1:5 ~ 1:10, and temperature of reaction is preferably at 80 ~ 85 DEG C;
(4) Graphene-polystyrene base material is warming up to 600 ~ 650 DEG C in vacuum tube furnace, take out after insulation 2 ~ 3h, wherein, temperature rise rate is preferably 3 ~ 4 DEG C/min, obtains Graphene.
Grapheme material is that a kind of monolayer carbon atom is through sp 2the novel material of bi-dimensional cellular shape structure that what hydridization was tightly packed have, thickness is 0.335nm only.Since the scientist of Univ Manchester UK in 2004 prepares single-layer graphene, Graphene has received the extensive concern of scientific circles and industry member.Graphene has excellent chemical stability and thermodynamic stability, and outstanding physicals and mechanical property.
The present invention adds Graphene in fire-retardant heat insulation plate, and because graphite is natural inert substance, fusing point is up to 3600 degrees Celsius, powdered graphite can cover on combustion boundary, play the effect of isolated air, and Graphene has larger specific surface area, a small amount of interpolation can be achieved the goal.Be combined with polystyrene foaming granule by Graphene, once be ignited, polystyrene burns generates gaseous volatilization, and Graphene then can form the film of one deck densification, covers isolated air on combustion boundary, plays extraordinary flame retardant effect.Reach the requirement of fire prevention A level.And the fire-retardant heat insulation plate intensity made also is significantly improved.
Two, Graphene-Zirconia-alumina matrix material is prepared;
(1) mixed with aluminic acid ammonia by the Graphene obtained in step one, ball milling is Graphene-aluminic acid ammonia matrix material; Wherein, the mass ratio of Graphene and aluminic acid ammonia is preferably 1:1-3:1; Adopt ball mill to matrix material ball milling, the rotating speed of ball milling is preferably 200-280rpm;
(2) above-mentioned Graphene-aluminic acid ammonia matrix material is heated to 800-950 DEG C, is incubated under nitrogen protection, lowers the temperature, obtain Graphene-alumina compound; Wherein, can carry out heating, be incubated and lower the temperature in tube furnace, the temperature rise rate of heating be 5-10 DEG C/min, and soaking time is 2-4h, is then down to room temperature, adopts the mode of Temperature fall.
(3) mixed with nano zircite by Graphene-alumina compound, ball milling obtains Graphene-Zirconia-alumina matrix material; Wherein, the mass ratio of Graphene-alumina compound and nano zircite is preferably 3:1-4:1; The rotational speed of ball-mill of ball mill is preferably 300-350rpm.
Zirconium white chemical property torpescence, and there is the character of high-melting-point and low thermal coefficient of expansion, make it become important high temperature material.Its relative density 5.6 ~ 6.9, due to the pyrochemistry stable in properties of zirconium white itself, corrosion-resistant, anti-oxidant, anti-thermal shock, non-volatile, pollution-free, is good a kind of refractory materials.
Aluminum oxide possesses fire performance, has the feature of porousness, high degree of dispersion simultaneously, has very large surface-area, and its micropore is evenly distributed, proper pore size, and tap density is little, good mechanical property, has good absorption property and excellent thermostability.
The present invention better plays its flame-retarding characteristic to make Graphene and zirconium white, the porousness utilizing aluminum oxide to possess and adsorptivity, in conjunction with after give full play to the advantage of three, make the Flame-retardant low-smoke warming plate finally made have good fire resistance, meet fire protection requirement; And flue gas is very low, environmental pollution reduces greatly, meets environmental requirement.
In the present invention, the mass ratio of preferred Graphene and aluminic acid ammonia is 1:1-3:1; The mass ratio of Graphene-alumina compound and nano zircite is 3:1-4:1; Can, by each proportioning in Graphene, zirconium white, alumina composite material, the flame retardant effect of the fire-retardant heat insulation plate finally made be made to reach best thus.
Three, fire-retardant heat insulation compound is prepared;
(1) Graphene-Zirconia-alumina matrix material is mixed with polystyrene after making solution; Wherein, in Graphene-Zirconia-alumina aqueous solution, the mass ratio of Graphene-Zirconia-alumina and water is 1:20 ~ 1:25; The mass ratio of Graphene-Zirconia-alumina and polystyrene is preferably 1:6 ~ 1:8; Be less than this ratio, when not increasing flame retardant properties, heat insulation effect can decline to a great extent; Be greater than this ratio, fire resistance will be a greater impact, and can not reach fire protection requirement.
(2) in above-mentioned mixing solutions, add resol and solidifying agent, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid; The mass ratio of mixing solutions and resol is 25:1 ~ 28:1; The mass ratio of resol and solidifying agent is 3:1 ~ 4:1.The physical strength of the sheet material of the fire-retardant heat insulation plate obtained outward in this ratio ranges is not good.Wherein the mass percentage of sulfuric acid is 97%, and the mass percentage of phosphoric acid is 38%; The mass ratio of water and sulfuric acid is 2:1 ~ 3:1; The mass ratio of water and phosphoric acid is 1.5:1 ~ 2:1; Obtain fire-retardant heat insulation compound.
Four, fire-retardant heat insulation plate is prepared;
(1) in the first twin screw extruder, melt-mixed material is obtained; Compound is added in the first twin screw extruder, obtain the compound of melting.Wherein, the work area in the first twin screw extruder is divided into seven sections: the first to the 3rd section is intensification melt zone, and the 4th to the 5th section is that melting is pressurizeed mixing district, and six to SECTOR-SEVEN section is the mixing district of high pressure-temperature.Wherein, the first zone temperatures 120 ~ 130 DEG C; Second section 150 ~ 160 DEG C; 3rd section 170 ~ 180 DEG C, pressure 3 ~ 4Mpa; 4th zone temperatures 190 ~ 200 DEG C, pressure 8 ~ 9MPa; 5th zone temperatures 210 ~ 220 DEG C, pressure 11 ~ 12Mpa; 6th zone temperatures 220 ~ 230 DEG C, pressure 18 ~ 19MPa, SECTOR-SEVEN section temperature 200 ~ 210 DEG C, pressure 22 ~ 23Mpa.Because matrix material of the present invention includes the component all not identical with conventional flame retardant warming plate, therefore the temperature of each section, pressure also must have adaptive innovation in an extruder, also obtain the warming plate material of performance the best.
(2) at the SECTOR-SEVEN section end of the first screw extrusion press, in the compound of melting, supercritical carbon dioxide fluid is added; The mass ratio of supercritical carbon dioxide fluid and compound is about 80:1 ~ 90:1, filling pressure 24MPa.
(3) compound of melting is carried out part mixing; Homogenizing barrier and releasing tube is provided with between first twin screw extruder outlet and the second screw extrusion press the 9th section.Partial blend enters the front end of Section Eight section by the squeezing passage between Section Eight Duan Yu nine section of the second screw extrusion press, after enter the 9th section by the screw extruding of Section Eight section; Partial blend enters the 9th section of the second screw extrusion press by homogenizing barrier and releasing tube, advances through screw extruding; Thus it is mixing to realize part.Wherein, the mass ratio entering the melt-mixed material of Section Eight section and the 9th section is 1:1.
(4) mixture particle is obtained by the second screw machine forcing machine; Second screw extrusion press is divided into five sections, is Section Eight Duan Zhi Twelve-section respectively.Section Eight Duan Zhi ten section is cooling decompression district; 11 section is dynamic mixing district, and Twelve-section is static mixing district.Wherein, Section Eight section temperature 150 ~ 160 DEG C, pressure 16 ~ 17MPa, the 9th zone temperatures 70 ~ 80 DEG C, pressure 20 ~ 21MPa, the tenth zone temperatures 50 ~ 60 DEG C, pressure 15 ~ 16MPa; 11 zone temperatures 40 ~ 50 DEG C, pressure 13 ~ 14MPa; Twelve-section temperature 80 ~ 90 DEG C, pressure 10 ~ 11Mpa.At Twelve-section end, extrusion die is installed, the temperature in die head region 90 ~ 100 DEG C, pressure 8 ~ 9Mpa.Unlike the prior art, it is applicable to above-mentioned matrix material of the present invention specially, is suitable for manufacturing the warming plate material obtaining performance the best for above-mentioned disclosed temperature, pressure range.
Some is had to the special building of requirements at the higher level, compound particles before making fire-retardant heat insulation plate with compound particles, first can mix with a coating, makes paint in particle surface by the present invention.Flame-retardant low-smoke coating of the present invention, comprises the component of following weight parts: aluminium hydroxide 15 ~ 25, zirconium white 35 ~ 45, Graphite Powder 99 3 ~ 7, laterite 15 ~ 25, breeze 4 ~ 6, ceramics powder 8 ~ 12.Preferably, the component of following weight parts is comprised: aluminium hydroxide 20, zirconium white 40, Graphite Powder 99 5, laterite 20, breeze 5, ceramics powder 10.
The method preparing this Flame-retardant low-smoke coating is, by the aluminium hydroxide of said components, zirconium white, Graphite Powder 99, laterite, breeze, ceramics powder, polystyrene, epoxy resin, dimethylaminopropylamine mixing, melting mixing coating is obtained by twin screw extruder, extrude, compressing tablet, air-cooled, abrasive dust, sieve, obtain coating.
Mixed with coating, tensio-active agent by warming plate material, be stirred to coating evenly, the mass ratio of warming plate material and coating is 1:1.2 ~ 1:1.4, obtains parcel warming plate particulate material, then compression molding.Tensio-active agent is preferably silicone.
The present invention is directed to above-mentioned polystyrene flame-retardant thermal insulation material, in order to the building demand of special dimension, develop above-mentioned composite coating, as the coated material on polystyrene foam particles surface, with solve further Polystyrene heat insulation material inflammable, melt drip, height such as to be fuming at the problem.This coating can improve the resistance to temp effect of lagging material further, uses simple, can direct spraying in base material, favorable anti-corrosion effect, cost is low.
(5) fire-retardant heat insulation plate is made with compound particles.
Embodiment 1:
The manufacture method of the fire-retardant heat insulation plate of this embodiment is as follows:
One, prepare Graphene, comprise the steps:
(1) expanded graphite is prepared.Wherein, first graphite oxide is placed in crucible, then retort furnace is heated to certain temperature, crucible is put into after retort furnace after held for some time, crucible is taken out, obtained expanded graphite.Wherein, the heating rate of heating muffle stove is 10 DEG C/min, retort furnace is heated to 1000 DEG C, and the soaking time of crucible in retort furnace is 3min.
(2) expanded graphite is scattered in water, ultrasonic after adding polystyrene sphere aqueous dispersions, obtained expanded graphite-polystyrene composite dispersion liquid; Wherein, the mass ratio of expanded graphite and water is 1:2, and the mass ratio of expanded graphite and polystyrene sphere aqueous dispersions is 60:1, ultrasonic time 2.2h;
(3) by expanded graphite-polystyrene composite dispersion liquid suction filtration in nickel foam, load had the nickel foam of expanded graphite-polystyrene to be placed in the mixing solutions of hydrazine hydrate and ammoniacal liquor after drying, after reaction, get Graphene-polystyrene base material; Wherein, the speed of suction filtration is 3L/s, drying temperature 60 DEG C, time of drying 11h, hydrazine hydrate and ammoniacal liquor volume ratio are 1:6, and temperature of reaction is at 80 DEG C;
(4) Graphene-polystyrene base material is warming up to 650 DEG C in vacuum tube furnace, takes out after insulation 2h, obtain Graphene.
Two, Graphene-Zirconia-alumina matrix material is prepared;
(1) mixed with aluminic acid ammonia by the Graphene obtained in step one, ball milling is Graphene-aluminic acid ammonia matrix material; Wherein, the mass ratio of Graphene and aluminic acid ammonia is 1:1;
(2) above-mentioned Graphene-aluminic acid ammonia matrix material is heated to 900 DEG C, is incubated under nitrogen protection, lowers the temperature, obtain Graphene-alumina compound; Carry out heating, be incubated and lower the temperature in tube furnace, the temperature rise rate of heating is 8 DEG C/min, and soaking time is 2h, and then Temperature fall is down to room temperature.
(3) mixed with nano zircite by Graphene-alumina compound, ball milling obtains Graphene-Zirconia-alumina matrix material; Wherein, the mass ratio of Graphene-alumina compound and nano zircite is 3:1; The rotational speed of ball-mill of ball mill is 350rpm.
Three, fire-retardant heat insulation compound is prepared;
(1) Graphene-Zirconia-alumina matrix material is mixed with polystyrene after making solution; Wherein, in Graphene-Zirconia-alumina aqueous solution, the mass ratio of Graphene-Zirconia-alumina and water is 1:20; The mass ratio of Graphene-Zirconia-alumina and polystyrene is 1:6;
(2) in above-mentioned mixing solutions, add resol and solidifying agent, the mass ratio of mixing solutions and resol is 25:1; The mass ratio of resol and solidifying agent is 4:1.
Four, fire-retardant heat insulation plate is prepared;
(1) in the first twin screw extruder, melt-mixed material is obtained; Compound is added in the first twin screw extruder, obtain the compound of melting.Wherein, the work area in the first twin screw extruder is divided into seven sections: the first zone temperatures 120 DEG C; Second section 150 DEG C; 3rd section 170 DEG C, pressure 3Mpa; 4th zone temperatures 190 DEG C, pressure 8MPa; 5th zone temperatures 210 DEG C, pressure 11Mpa; 6th zone temperatures 220 DEG C, pressure 18MPa, SECTOR-SEVEN section temperature 200 DEG C, pressure 22Mpa.
(2) at the SECTOR-SEVEN section end of the first screw extrusion press, in the compound of melting, supercritical carbon dioxide fluid is added; The mass ratio of supercritical carbon dioxide fluid and compound is about 90:1, filling pressure 24MPa.
(3) compound of melting is carried out part respectively by the Section Eight section of the second screw machine and the 9th section mixing; The mass ratio entering the melt-mixed material of Section Eight section and the 9th section is 1:1.
(4) mixture particle is obtained by the second screw machine forcing machine; Second screw extrusion press is divided into five sections, Section Eight section temperature 150 DEG C, pressure 16MPa, the 9th zone temperatures 70 DEG C, pressure 20MPa, the tenth zone temperatures 50 DEG C, pressure 15MPa; 11 zone temperatures 40 DEG C, pressure 13MPa; Twelve-section temperature 80 DEG C, pressure 10Mpa.The temperature in the extrusion die region of Twelve-section end 90 DEG C, pressure 9Mpa.
(5) fire-retardant heat insulation plate is made with compound particles.
Embodiment 2:
The manufacture method of the fire-retardant heat insulation plate of the present embodiment is as follows:
One, prepare Graphene, comprise the steps:
(1) graphite oxide is placed in crucible, retort furnace is heated to 1100, heating rate 15 DEG C/min, after being incubated 5min after crucible being put into retort furnace, crucible is taken out, obtained expanded graphite.
(2) expanded graphite is scattered in water, the mass ratio of expanded graphite and water is 1:2, adds polystyrene sphere aqueous dispersions, and the mass ratio of expanded graphite and polystyrene sphere aqueous dispersions is 70:1, ultrasonic 2h, obtained expanded graphite-polystyrene composite dispersion liquid;
(3) by expanded graphite-polystyrene composite dispersion liquid suction filtration in nickel foam, dry dry temperature 60 C, time of drying 12h, the nickel foam of expanded graphite-polystyrene load is had to be placed in the mixing solutions of hydrazine hydrate and ammoniacal liquor, hydrazine hydrate and ammoniacal liquor volume ratio are 1:8, get Graphene-polystyrene base material after reaction;
(4) Graphene-polystyrene base material is warming up to 600 DEG C in vacuum tube furnace, takes out after insulation 2h, obtain Graphene.
Two, Graphene-Zirconia-alumina matrix material is prepared;
(1) mixed with aluminic acid ammonia by the Graphene obtained in step one, the mass ratio of Graphene and aluminic acid ammonia is preferably 2:1, and ball milling is Graphene-aluminic acid ammonia matrix material, and the rotating speed of ball milling is preferably 250rpm;
(2) above-mentioned Graphene-aluminic acid ammonia matrix material is heated to 800-950 DEG C, the temperature rise rate of heating is that 5-10 DEG C/min is incubated 2h, Temperature fall under nitrogen protection, obtains Graphene-alumina compound;
(3) mixed with nano zircite by Graphene-alumina compound, the mass ratio of Graphene-alumina compound and nano zircite is 3:1-; Ball milling, the rotational speed of ball-mill of ball mill is 350rpm, obtains Graphene-Zirconia-alumina matrix material.
Three, fire-retardant heat insulation compound is prepared;
(1) Graphene-Zirconia-alumina matrix material is mixed with polystyrene after making solution; Wherein, in Graphene-Zirconia-alumina aqueous solution, the mass ratio of Graphene-Zirconia-alumina and water is 1:20; The mass ratio of Graphene-Zirconia-alumina and polystyrene is preferably 1:6;
(2) in above-mentioned mixing solutions, add resol and solidifying agent, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid; The mass ratio of mixing solutions and resol is 25:1 ~ 28:1; The mass ratio of resol and solidifying agent is 3:1 ~ 4:1.
Four, fire-retardant heat insulation plate is prepared;
(1) in the first twin screw extruder, melt-mixed material is obtained; Compound is added in the first twin screw extruder, obtain the compound of melting.Wherein, in the work area in the first twin screw extruder, the first zone temperatures 130 DEG C; Second section 160 DEG C; 3rd section 180 DEG C, pressure 4Mpa; 4th zone temperatures 200 DEG C, pressure 9MPa; 5th zone temperatures 220 DEG C, pressure 12Mpa; 6th zone temperatures 230 DEG C, 19MPa, SECTOR-SEVEN section temperature 210 DEG C, pressure 23Mpa.
(2) at the SECTOR-SEVEN section end of the first screw extrusion press, in the compound of melting, supercritical carbon dioxide fluid is added; The mass ratio of supercritical carbon dioxide fluid and compound is about 90:1, filling pressure 24MPa.
(3) compound of melting is carried out part at the 8th and the 9th section of the second screw extrusion press mixing; The mass ratio entering the melt-mixed material of Section Eight section and the 9th section is 1:1.
(4) mixture particle is obtained by the second screw machine forcing machine; In second screw extrusion press, Section Eight section temperature 160 DEG C, pressure 17MPa, the 9th zone temperatures 80 DEG C, pressure 21MPa, the tenth zone temperatures 60 DEG C, pressure 16MPa; 11 zone temperatures 50 DEG C, pressure 14MPa; Twelve-section temperature 90 DEG C, pressure 11Mpa.At Twelve-section end, extrusion die is installed, the temperature in die head region 100 DEG C, pressure 9Mpa.
(5) fire-retardant heat insulation plate is made with compound particles.
Embodiment 3:
The manufacture method of the fire-retardant heat insulation plate of this embodiment is as follows:
One, prepare Graphene, comprise the steps:
(1) graphite oxide is placed in crucible, then retort furnace is heated to 1100 DEG C, heating rate is 12 DEG C/min, after being incubated 4min, is taken out by crucible after crucible being put into retort furnace, obtained expanded graphite.
(2) expanded graphite is scattered in water, the mass ratio of expanded graphite and water is 1:2, adds polystyrene sphere aqueous dispersions, and the mass ratio of expanded graphite and polystyrene sphere aqueous dispersions is 70:1, ultrasonic 2h, obtained expanded graphite-polystyrene composite dispersion liquid;
(3) by expanded graphite-polystyrene composite dispersion liquid suction filtration in nickel foam, the speed of suction filtration is 4L/s, dry, drying temperature 60 DEG C, time of drying 11h, the mixing solutions having the nickel foam of expanded graphite-polystyrene to be placed in hydrazine hydrate and ammoniacal liquor load reacts, and hydrazine hydrate and ammoniacal liquor volume ratio are 1:5 ~ 1:10, and temperature of reaction is preferably at 80 ~ 85 DEG C; Get Graphene-polystyrene base material;
(4) Graphene-polystyrene base material is warming up to 650 DEG C in vacuum tube furnace, temperature rise rate is 4 DEG C/min, takes out, obtain Graphene after insulation 3h.
Two, Graphene-Zirconia-alumina matrix material is prepared;
(1) mixed with aluminic acid ammonia by Graphene, mass ratio is 1:1-3:1; Ball milling is Graphene-aluminic acid ammonia matrix material; The rotating speed of ball milling is 260rpm;
(2) above-mentioned Graphene-aluminic acid ammonia matrix material is heated to 900 DEG C, temperature rise rate is 10 DEG C/min, is incubated 3h, Temperature fall under nitrogen protection, obtains Graphene-alumina compound;
(3) mixed with nano zircite by Graphene-alumina compound, the mass ratio of Graphene-alumina compound and nano zircite is 4:1; Ball milling obtains Graphene-Zirconia-alumina matrix material; The rotational speed of ball-mill of ball mill is preferably 330rpm.
Three, fire-retardant heat insulation compound is prepared;
(1) Graphene-Zirconia-alumina matrix material is mixed with polystyrene after making solution; The mass ratio of Graphene-Zirconia-alumina and water is 1:20; The mass ratio of Graphene-Zirconia-alumina and polystyrene is 1:8;
(2) in above-mentioned mixing solutions, add resol and solidifying agent, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid; The mass ratio of mixing solutions and resol is 25:1; The mass ratio of resol and solidifying agent is 3:1.Wherein the mass percentage of sulfuric acid is 97%, and the mass percentage of phosphoric acid is 38%; The mass ratio of water and sulfuric acid is 3:1; The mass ratio of water and phosphoric acid is 2:1; Obtain fire-retardant heat insulation compound.
Four, fire-retardant heat insulation plate is prepared;
(1) in the first twin screw extruder, melt-mixed material is obtained; Compound is added in the first twin screw extruder, obtain the compound of melting.Wherein, the work area in the first twin screw extruder is divided into seven sections: the first zone temperatures 120 DEG C; Second section 150 DEG C; 3rd section 170 DEG C, pressure 3Mpa; 4th zone temperatures 190 DEG C, pressure 8MPa; 5th zone temperatures 210 DEG C, pressure 11Mpa; 6th zone temperatures 220 DEG C, pressure 18MPa, SECTOR-SEVEN section temperature 200 DEG C, pressure 22Mpa.
(2) at the SECTOR-SEVEN section end of the first screw extrusion press, in the compound of melting, supercritical carbon dioxide fluid is added; The mass ratio of supercritical carbon dioxide fluid and compound is about 90:1, filling pressure 24MPa.
(3) compound of melting is carried out part respectively by the Section Eight section of the second screw machine and the 9th section mixing; The mass ratio entering the melt-mixed material of Section Eight section and the 9th section is 1:1.
(4) mixture particle is obtained by the second screw machine forcing machine; Second screw extrusion press is divided into five sections, Section Eight section temperature 150 DEG C, pressure 16MPa, the 9th zone temperatures 70 DEG C, pressure 20MPa, the tenth zone temperatures 50 DEG C, pressure 15MPa; 11 zone temperatures 40 DEG C, pressure 13MPa; Twelve-section temperature 80 DEG C, pressure 10Mpa.The temperature in the extrusion die region of Twelve-section end 90 DEG C, pressure 9Mpa.
(5) fire-retardant heat insulation plate is made with compound particles.
Embodiment 4:
The manufacture method of the fire-retardant heat insulation plate of the present embodiment is as follows:
One, prepare Graphene, comprise the steps:
(1) graphite oxide is placed in crucible, retort furnace is heated to 1100, heating rate 15 DEG C/min, after being incubated 5min after crucible being put into retort furnace, crucible is taken out, obtained expanded graphite.
(2) expanded graphite is scattered in water, the mass ratio of expanded graphite and water is 1:2, adds polystyrene sphere aqueous dispersions, and the mass ratio of expanded graphite and polystyrene sphere aqueous dispersions is 70:1, ultrasonic 2h, obtained expanded graphite-polystyrene composite dispersion liquid;
(3) by expanded graphite-polystyrene composite dispersion liquid suction filtration in nickel foam, dry dry temperature 60 C, time of drying 12h, the nickel foam of expanded graphite-polystyrene load is had to be placed in the mixing solutions of hydrazine hydrate and ammoniacal liquor, hydrazine hydrate and ammoniacal liquor volume ratio are 1:8, get Graphene-polystyrene base material after reaction;
(4) Graphene-polystyrene base material is warming up to 600 DEG C in vacuum tube furnace, takes out after insulation 2h, obtain Graphene.
Two, Graphene-Zirconia-alumina matrix material is prepared;
(1) mixed with aluminic acid ammonia by the Graphene obtained in step one, the mass ratio of Graphene and aluminic acid ammonia is preferably 2:1, and ball milling is Graphene-aluminic acid ammonia matrix material, and the rotating speed of ball milling is preferably 250rpm;
(2) above-mentioned Graphene-aluminic acid ammonia matrix material is heated to 800-950 DEG C, the temperature rise rate of heating is that 5-10 DEG C/min is incubated 2h, Temperature fall under nitrogen protection, obtains Graphene-alumina compound;
(3) mixed with nano zircite by Graphene-alumina compound, the mass ratio of Graphene-alumina compound and nano zircite is 3:1-; Ball milling, the rotational speed of ball-mill of ball mill is 350rpm, obtains Graphene-Zirconia-alumina matrix material.
Three, fire-retardant heat insulation compound is prepared;
(1) Graphene-Zirconia-alumina matrix material is mixed with polystyrene after making solution; Wherein, in Graphene-Zirconia-alumina aqueous solution, the mass ratio of Graphene-Zirconia-alumina and water is 1:20; The mass ratio of Graphene-Zirconia-alumina and polystyrene is preferably 1:6;
(2) in above-mentioned mixing solutions, add resol and solidifying agent, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid; The mass ratio of mixing solutions and resol is 25:1 ~ 28:1; The mass ratio of resol and solidifying agent is 3:1 ~ 4:1.
Four, fire-retardant heat insulation particle is prepared;
(1) in the first twin screw extruder, melt-mixed material is obtained; Compound is added in the first twin screw extruder, obtain the compound of melting.Wherein, in the work area in the first twin screw extruder, the first zone temperatures 130 DEG C; Second section 160 DEG C; 3rd section 180 DEG C, pressure 4Mpa; 4th zone temperatures 200 DEG C, pressure 9MPa; 5th zone temperatures 220 DEG C, pressure 12Mpa; 6th zone temperatures 230 DEG C, 19MPa, SECTOR-SEVEN section temperature 210 DEG C, pressure 23Mpa.
(2) at the SECTOR-SEVEN section end of the first screw extrusion press, in the compound of melting, supercritical carbon dioxide fluid is added; The mass ratio of supercritical carbon dioxide fluid and compound is about 90:1, filling pressure 24MPa.
(3) compound of melting is carried out part at the 8th and the 9th section of the second screw extrusion press mixing; The mass ratio entering the melt-mixed material of Section Eight section and the 9th section is 1:1.
(4) mixture particle is obtained by the second screw machine forcing machine; In second screw extrusion press, Section Eight section temperature 160 DEG C, pressure 17MPa, the 9th zone temperatures 80 DEG C, pressure 21MPa, the tenth zone temperatures 60 DEG C, pressure 16MPa; 11 zone temperatures 50 DEG C, pressure 14MPa; Twelve-section temperature 90 DEG C, pressure 11Mpa.At Twelve-section end, extrusion die is installed, the temperature in die head region 100 DEG C, pressure 9Mpa.
Five, prepare coating and apply
Component by following weight parts ratio: aluminium hydroxide 20, zirconium white 40, Graphite Powder 99 5, laterite 20, breeze 5, ceramics powder 10 mix, and obtain melting mixing coating, extrude, compressing tablet by twin screw extruder, air-cooled, and abrasive dust, sieves, and obtains coating.
Mixed with coating, silicone by fire-retardant heat insulation particle, be stirred to coating evenly, the mass ratio of warming plate material and coating is 1:1.2, obtains parcel warming plate particulate material, then compression molding, obtained building thermal insulation material.
Embodiment 5:
The manufacture method of the fire-retardant heat insulation plate of the present embodiment is as follows:
One, prepare Graphene, comprise the steps:
(1) graphite oxide is placed in crucible, retort furnace is heated to 1100, heating rate 15 DEG C/min, after being incubated 5min after crucible being put into retort furnace, crucible is taken out, obtained expanded graphite.
(2) expanded graphite is scattered in water, the mass ratio of expanded graphite and water is 1:2, adds polystyrene sphere aqueous dispersions, and the mass ratio of expanded graphite and polystyrene sphere aqueous dispersions is 70:1, ultrasonic 2h, obtained expanded graphite-polystyrene composite dispersion liquid;
(3) by expanded graphite-polystyrene composite dispersion liquid suction filtration in nickel foam, dry dry temperature 60 C, time of drying 12h, the nickel foam of expanded graphite-polystyrene load is had to be placed in the mixing solutions of hydrazine hydrate and ammoniacal liquor, hydrazine hydrate and ammoniacal liquor volume ratio are 1:8, get Graphene-polystyrene base material after reaction;
(4) Graphene-polystyrene base material is warming up to 600 DEG C in vacuum tube furnace, takes out after insulation 2h, obtain Graphene.
Two, Graphene-Zirconia-alumina matrix material is prepared;
(1) mixed with aluminic acid ammonia by the Graphene obtained in step one, the mass ratio of Graphene and aluminic acid ammonia is preferably 2:1, and ball milling is Graphene-aluminic acid ammonia matrix material, and the rotating speed of ball milling is preferably 250rpm;
(2) above-mentioned Graphene-aluminic acid ammonia matrix material is heated to 800-950 DEG C, the temperature rise rate of heating is that 5-10 DEG C/min is incubated 2h, Temperature fall under nitrogen protection, obtains Graphene-alumina compound;
(3) mixed with nano zircite by Graphene-alumina compound, the mass ratio of Graphene-alumina compound and nano zircite is 3:1-; Ball milling, the rotational speed of ball-mill of ball mill is 350rpm, obtains Graphene-Zirconia-alumina matrix material.
Three, fire-retardant heat insulation compound is prepared;
(1) Graphene-Zirconia-alumina matrix material is mixed with polystyrene after making solution; Wherein, in Graphene-Zirconia-alumina aqueous solution, the mass ratio of Graphene-Zirconia-alumina and water is 1:20; The mass ratio of Graphene-Zirconia-alumina and polystyrene is preferably 1:6;
(2) in above-mentioned mixing solutions, add resol and solidifying agent, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid; The mass ratio of mixing solutions and resol is 25:1 ~ 28:1; The mass ratio of resol and solidifying agent is 3:1 ~ 4:1.
Four, fire-retardant heat insulation particle is prepared;
(1) in the first twin screw extruder, melt-mixed material is obtained; Compound is added in the first twin screw extruder, obtain the compound of melting.Wherein, in the work area in the first twin screw extruder, the first zone temperatures 130 DEG C; Second section 160 DEG C; 3rd section 180 DEG C, pressure 4Mpa; 4th zone temperatures 200 DEG C, pressure 9MPa; 5th zone temperatures 220 DEG C, pressure 12Mpa; 6th zone temperatures 230 DEG C, 19MPa, SECTOR-SEVEN section temperature 210 DEG C, pressure 23Mpa.
(2) at the SECTOR-SEVEN section end of the first screw extrusion press, in the compound of melting, supercritical carbon dioxide fluid is added; The mass ratio of supercritical carbon dioxide fluid and compound is about 90:1, filling pressure 24MPa.
(3) compound of melting is carried out part at the 8th and the 9th section of the second screw extrusion press mixing; The mass ratio entering the melt-mixed material of Section Eight section and the 9th section is 1:1.
(4) mixture particle is obtained by the second screw machine forcing machine; In second screw extrusion press, Section Eight section temperature 160 DEG C, pressure 17MPa, the 9th zone temperatures 80 DEG C, pressure 21MPa, the tenth zone temperatures 60 DEG C, pressure 16MPa; 11 zone temperatures 50 DEG C, pressure 14MPa; Twelve-section temperature 90 DEG C, pressure 11Mpa.At Twelve-section end, extrusion die is installed, the temperature in die head region 100 DEG C, pressure 9Mpa.
Five, prepare coating and apply
Component by following weight parts ratio: aluminium hydroxide 20, zirconium white 43, Graphite Powder 99 7, laterite 18, breeze 4, ceramics powder 8 mix, and obtain melting mixing coating, extrude, compressing tablet by twin screw extruder, air-cooled, and abrasive dust, sieves, and obtains coating.
Mixed with coating, silicone by fire-retardant heat insulation particle, be stirred to coating evenly, the mass ratio of warming plate material and coating is 1:1.2, obtains parcel warming plate particulate material, then compression molding, obtained building thermal insulation material.
Below in conjunction with some fire-retardant heat insulation plates conventional in prior art as comparative example, these warming plates are made by method as follows, as shown in table 1, while the technical parameter of the above embodiment of the present invention is shown, list the technical parameter of comparative example, for reference.
Comparative example 1:
This comparative example manufacture comprises the warming plate of graphite and polystyrene, is made by following steps:
Being added by Expandable Polystyrene (EPS) in prefoaming machine, by steam heating, is particulate state by Expandable Polystyrene (EPS) foaming; Expandable polystyrene particle after foaming is carried out slaking;
Expandable polystyrene particle is added in stirred vessel, then adds carbon black or graphite, the two uniform stirring is become compound, carbon black or graphite are evenly wrapped up expandable polystyrene particle; Wherein the ratio of carbon black is 0.2% of the expandable polystyrene particle weight after foaming; The ratio of graphite is 2% of the expandable polystyrene particle weight after foaming;
The compound of the expandable polystyrene particle be stirred and carbon black or graphite is transported in forming machine fixed-type.
Comparative example 2:
This comparative example is a kind of polystyrene foam composite heat insulatant thermal insulation material, comprises the following steps:
With 100 parts of resol for base-material, 10 parts of expansible black leads and capsule red phosphorus is added respectively under stirring, add 10 parts of solidifying agent and 10 parts of whipping agents and 5 parts of tensio-active agents, be stirred to and be uniformly dispersed, obtain the polymer-based carbon coating being dispersed with anti-flaming function component, wherein the mass ratio of expansible black lead and capsule red phosphorus is 1:1;
Get the polystyrene foam particles of pre-frothing as base-material, then above-mentioned polymer-based carbon coating is added, wherein, the base-material of polystyrene foam particles and the mass ratio of polymer-based carbon coating are 1:2, be stirred to coating evenly, obtain coated composite polystyrene foam beads material, then will obtain coated composite polystyrene foam beads material joins in steam heat compression mould, and Feng Mo, passes into high-pressure water vapor to 0.05MPa, and after pressurize 45s, release, after cooling, die sinking, discharging, obtains high-flame-retardant low-smoke-density polystyrene foam compound heat insulating material.
Comparative example 3:
This comparative example manufactures a kind of Polystyrene heat insulation material, and preparation method comprises the following steps:
First prepare properties-correcting agent, it comprises the component by following parts by weight: silicate 40 parts, methacrylic acid 3 parts, Graphene 1 part, polyoxyethylene nonylphenol ether 1 part, sulfonation polyoxyethylene glycol 1 part, 10 parts, water.
After being mixed by the material of said components, get 1 part according to parts by weight, get foam materials 10 parts, together enter mixer batch mixing, under the continuous stirring of the agitating vane of mixer, stir 2 hours, properties-correcting agent on foam materials, is dried stand-by by uniform application.
Get the above-mentioned foam materials handled well, according to the ratio of volume ratio 1.5:1, with cement mixing, mix post-drying, make lagging material.
Table 1
The building thermal insulation material of a kind of fire resistance excellence disclosed by the invention and manufacture method thereof, this material has better flame retardant properties and low smoke density compared to existing technology, and nontoxic pollution-free has higher fire-protection rating, meets environmental requirement.
The present invention adds Graphene in lagging material, due to the inert substance that graphite is natural, fusing point is up to 3600 degrees Celsius, powdered graphite can cover on combustion boundary, play the effect of isolated air, and Graphene has larger specific surface area, a small amount of interpolation can be achieved the goal, and plays extraordinary flame retardant effect.Reach the requirement of fire prevention A level.
The present invention adds zirconium white at lagging material, due to the pyrochemistry stable in properties of zirconium white itself, corrosion-resistant, anti-oxidant, anti-thermal shock, non-volatile, pollution-free, is good a kind of refractory materials.
The present invention adds aluminum oxide at lagging material, because aluminum oxide possesses fire performance, there is the feature of porousness, high degree of dispersion simultaneously, there is very large surface-area, its micropore is evenly distributed, proper pore size, and tap density is little, good mechanical property, has good absorption property and excellent thermostability.
Graphene, zirconium white, aluminum oxide combine with specified proportion by the present invention, in conjunction with after give full play to the advantage of three, make the Flame-retardant low-smoke warming plate finally made have good fire resistance, meet fire protection requirement; And flue gas is very low, environmental pollution reduces greatly, meets environmental requirement.
In the present invention, the ratio of Graphene-Zirconia-alumina and polystyrene makes its flame retardant properties and heat-insulating property reach balance, there will not be obvious short slab, outside this proportioning, its heat insulation effect will be made to decline or fire resistance will be a greater impact.
Because matrix material of the present invention includes the component all not identical with conventional flame retardant warming plate, the temperature of each section, pressure carry out adaptive innovation in an extruder, give full play to the advantage of component, be not subject to the restriction of manufacturing condition simultaneously, finally obtain the warming plate material of performance the best.
Invention also discloses other the very important point, lagging material of the present invention, before making fire-retardant heat insulation plate with compound particles, first compound particles is mixed with a coating, stirring makes coating evenly be coated on particle surface, again the compound particles being coated with coating being made fire-retardant heat insulation plate, because this coating has well fire-retardant, low cigarette effect, is a kind of A level fire-retardant heat-insulation material meeting environmental protection A grade standard.
The present invention also can have other various embodiments; when not deviating from the present invention's spirit and essence thereof; those of ordinary skill in the art are when making various corresponding change and distortion according to the present invention, but these change accordingly and are out of shape the protection domain that all should belong to the claim appended by the present invention.

Claims (6)

1. a lagging material, comprises the compound of Graphene, zirconium white, aluminum oxide and polystyrene, and the gross weight of Graphene-Zirconia-alumina and the mass ratio of polystyrene are 1:6 ~ 1:8;
Further, lagging material also comprises resol and solidifying agent; The mass ratio of compound and resol is 25:1 ~ 28:1; The mass ratio of resol and solidifying agent is 3:1 ~ 4:1; Wherein, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid.
2. lagging material as claimed in claim 1, it is characterized in that, the manufacture method of this lagging material comprises the following steps:
Prepare Graphene:
(11) expanded graphite is prepared; Wherein, first graphite oxide is placed in crucible, then retort furnace is heated to certain temperature, crucible is put into after retort furnace after held for some time, crucible is taken out, obtained expanded graphite;
(12) expanded graphite is scattered in water, ultrasonic after adding polystyrene sphere aqueous dispersions, obtained expanded graphite-polystyrene composite dispersion liquid; Wherein, the mass ratio of expanded graphite and water is 1:1 ~ 1:2, and the mass ratio of expanded graphite and polystyrene sphere aqueous dispersions is 80:1 ~ 60:1;
(13) by expanded graphite-polystyrene composite dispersion liquid suction filtration in nickel foam, load had the nickel foam of expanded graphite-polystyrene to be placed in the mixing solutions of hydrazine hydrate and ammoniacal liquor after drying, after reaction, get Graphene-polystyrene base material;
(14) Graphene-polystyrene base material is warming up to 600 ~ 650 DEG C in vacuum tube furnace, takes out after insulation 2 ~ 3h, obtain Graphene;
Prepare Graphene-Zirconia-alumina matrix material;
(21) mixed with aluminic acid ammonia by the Graphene obtained in step one, ball milling is Graphene-aluminic acid ammonia matrix material; Wherein, the mass ratio of Graphene and aluminic acid ammonia is preferably 1:1-3:1;
(22) above-mentioned Graphene-aluminic acid ammonia matrix material is heated to 800-950 DEG C, is incubated under nitrogen protection, lowers the temperature, obtain Graphene-alumina compound;
(23) mixed with nano zircite by Graphene-alumina compound, ball milling obtains Graphene-Zirconia-alumina matrix material; Wherein, the mass ratio of Graphene-alumina compound and nano zircite is preferably 3:1-4:1;
Prepare fire-retardant heat insulation compound;
(31) Graphene-Zirconia-alumina matrix material is mixed with polystyrene after making solution; Wherein, in Graphene-Zirconia-alumina aqueous solution, the mass ratio of Graphene-Zirconia-alumina and water is 1:20 ~ 1:25; The mass ratio of Graphene-Zirconia-alumina and polystyrene is preferably 1:6 ~ 1:8;
(32) in above-mentioned mixing solutions, add resol and solidifying agent, solidifying agent is the mixture of water, sulfuric acid and phosphoric acid, obtains fire-retardant heat insulation compound;
Prepare fire-retardant heat insulation plate;
(41) in the first twin screw extruder, melt-mixed material is obtained; Compound is added in the first twin screw extruder, obtain the compound of melting;
(42) at the SECTOR-SEVEN section end of the first screw extrusion press, in the compound of melting, supercritical carbon dioxide fluid is added; The mass ratio of supercritical carbon dioxide fluid and compound is about 80:1 ~ 90:1, filling pressure 24Mpa;
(43) compound of melting is carried out part in the Section Eight section of the second screw machine and the 9th section mixing; Wherein, the mass ratio entering the melt-mixed material of Section Eight section and the 9th section is 1:1;
(44) mixture particle is obtained by the second screw machine forcing machine;
(45) lagging material is made with compound particles.
3. lagging material as claimed in claim 2, it is characterized in that, in step (22), carry out heating, be incubated and lower the temperature in tube furnace, the temperature rise rate of heating is 5-10 DEG C/min, and soaking time is 2-4h, then Temperature fall.
4. lagging material as claimed in claim 2, it is characterized in that, in step (32), in mixing solutions, the mass ratio of compound and resol is 25:1 ~ 28:1; The mass ratio of resol and solidifying agent is 3:1 ~ 4:1; Wherein the mass percentage of sulfuric acid is 97%, and the mass percentage of phosphoric acid is 38%; The mass ratio of water and sulfuric acid is 2:1 ~ 3:1; The mass ratio of water and phosphoric acid is 1.5:1 ~ 2:1.
5. lagging material as claimed in claim 2, it is characterized in that, in step (41), the work area in the first twin screw extruder is divided into seven sections: the first zone temperatures 120 DEG C; Second section 150 DEG C; 3rd section 170 DEG C, pressure 3Mpa; 4th zone temperatures 190 DEG C, pressure 8MPa; 5th zone temperatures 210 DEG C, pressure 11Mpa; 6th zone temperatures 220 DEG C, pressure 18MPa, SECTOR-SEVEN section temperature 200 DEG C, pressure 22Mpa.
6. lagging material as claimed in claim 2, it is characterized in that, in step (44), the second screw extrusion press is divided into five sections, is Section Eight Duan Zhi Twelve-section respectively, Section Eight section temperature 150 DEG C, pressure 16MPa, the 9th zone temperatures 70 DEG C, pressure 20MPa, tenth zone temperatures 50 DEG C, pressure 15MPa; 11 zone temperatures 40 DEG C, pressure 13MPa; Twelve-section temperature 80 DEG C, pressure 10Mpa.
CN201610049174.6A 2016-01-25 2016-01-25 Building heat preservation material with excellent fireproof performance Withdrawn CN105419140A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106883526A (en) * 2017-04-28 2017-06-23 惠生新材料研究院（深圳）有限公司 Nanometer fireproof polystyrene foam plate and preparation method thereof
CN107746564A (en) * 2017-09-22 2018-03-02 山东汇星科技开发有限公司 A kind of GPES composite plastics warming plate and its preparation technology
CN107759243A (en) * 2017-10-31 2018-03-06 广西旭腾实业集团有限公司 One kind is based on graphene and stone material foamed wall slab and preparation method thereof
CN108976922A (en) * 2018-05-23 2018-12-11 苏州牛麦田新材料科技有限公司 A kind of fire resistant special type coating and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103555151A (en) * 2013-10-28 2014-02-05 安徽明都电气有限公司 Temperature-resistant corrosion-preventing mixed resin powder coating
CN104163421A (en) * 2014-07-27 2014-11-26 北京工业大学 Preparation method of three-dimensional flocculent graphene substrate material and application
KR101494289B1 (en) * 2014-08-20 2015-02-17 전남대학교산학협력단 Polymer electrolyte composite, method for producing the same and energy storage comprising the polymer electrolyte composite
CN104861323A (en) * 2015-05-26 2015-08-26 黑龙江省黑钻极光新能源科技有限公司 Non-combustible graphene polystyrene foamed insulation board as well as preparation method and application thereof
CN105174818A (en) * 2015-09-10 2015-12-23 孟红琳 Preparation method of graphene modified slurry heat insulation material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103555151A (en) * 2013-10-28 2014-02-05 安徽明都电气有限公司 Temperature-resistant corrosion-preventing mixed resin powder coating
CN104163421A (en) * 2014-07-27 2014-11-26 北京工业大学 Preparation method of three-dimensional flocculent graphene substrate material and application
KR101494289B1 (en) * 2014-08-20 2015-02-17 전남대학교산학협력단 Polymer electrolyte composite, method for producing the same and energy storage comprising the polymer electrolyte composite
CN104861323A (en) * 2015-05-26 2015-08-26 黑龙江省黑钻极光新能源科技有限公司 Non-combustible graphene polystyrene foamed insulation board as well as preparation method and application thereof
CN105174818A (en) * 2015-09-10 2015-12-23 孟红琳 Preparation method of graphene modified slurry heat insulation material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
杜科选等: "《铝电解和铝合金铸造生产与安全》", 31 May 2012, 冶金工业出版社 *
郭秉臣: "《非织造技术产品开发》", 31 July 2009, 中国纺织出版社 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106883526A (en) * 2017-04-28 2017-06-23 惠生新材料研究院（深圳）有限公司 Nanometer fireproof polystyrene foam plate and preparation method thereof
CN106883526B (en) * 2017-04-28 2018-06-08 惠生新材料研究院（深圳）有限公司 Nanometer fireproof polystyrene foam plate and preparation method thereof
CN107746564A (en) * 2017-09-22 2018-03-02 山东汇星科技开发有限公司 A kind of GPES composite plastics warming plate and its preparation technology
CN107759243A (en) * 2017-10-31 2018-03-06 广西旭腾实业集团有限公司 One kind is based on graphene and stone material foamed wall slab and preparation method thereof
CN108976922A (en) * 2018-05-23 2018-12-11 苏州牛麦田新材料科技有限公司 A kind of fire resistant special type coating and preparation method thereof

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