CN115959868A - Composite expanded graphite homogeneous plate and preparation method thereof - Google Patents
Composite expanded graphite homogeneous plate and preparation method thereof Download PDFInfo
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- CN115959868A CN115959868A CN202211650476.0A CN202211650476A CN115959868A CN 115959868 A CN115959868 A CN 115959868A CN 202211650476 A CN202211650476 A CN 202211650476A CN 115959868 A CN115959868 A CN 115959868A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000010439 graphite Substances 0.000 title claims abstract description 47
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 69
- 238000003756 stirring Methods 0.000 claims abstract description 61
- 229920006327 polystyrene foam Polymers 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 19
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 19
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 19
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000835 fiber Substances 0.000 claims abstract description 18
- -1 polypropylene Polymers 0.000 claims abstract description 18
- 239000011398 Portland cement Substances 0.000 claims abstract description 17
- 239000004743 Polypropylene Substances 0.000 claims abstract description 16
- 239000003513 alkali Substances 0.000 claims abstract description 16
- 239000004744 fabric Substances 0.000 claims abstract description 16
- 239000003365 glass fiber Substances 0.000 claims abstract description 16
- 229920001155 polypropylene Polymers 0.000 claims abstract description 16
- 239000004816 latex Substances 0.000 claims abstract description 13
- 229920000126 latex Polymers 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000011325 microbead Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 239000002985 plastic film Substances 0.000 claims abstract description 6
- 229920006255 plastic film Polymers 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 41
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 33
- 239000003063 flame retardant Substances 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- 239000004568 cement Substances 0.000 claims description 21
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 238000004132 cross linking Methods 0.000 claims description 17
- IBGBGRVKPALMCQ-UHFFFAOYSA-N 3,4-dihydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1O IBGBGRVKPALMCQ-UHFFFAOYSA-N 0.000 claims description 14
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000013067 intermediate product Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- PCYGLFXKCBFGPC-UHFFFAOYSA-N 3,4-Dihydroxy hydroxymethyl benzene Natural products OCC1=CC=C(O)C(O)=C1 PCYGLFXKCBFGPC-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- TXFOLHZMICYNRM-UHFFFAOYSA-N dichlorophosphoryloxybenzene Chemical compound ClP(Cl)(=O)OC1=CC=CC=C1 TXFOLHZMICYNRM-UHFFFAOYSA-N 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 239000001506 calcium phosphate Substances 0.000 claims description 4
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 4
- 235000011010 calcium phosphates Nutrition 0.000 claims description 4
- 239000007822 coupling agent Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000005187 foaming Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000003892 spreading Methods 0.000 claims description 4
- 230000007480 spreading Effects 0.000 claims description 4
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 4
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract 1
- 239000004793 Polystyrene Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 229920002223 polystyrene Polymers 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 5
- 239000004005 microsphere Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 125000003172 aldehyde group Chemical group 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910001576 calcium mineral Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical class [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004794 expanded polystyrene Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000003469 silicate cement Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a composite expanded graphite homogeneous plate and a preparation method thereof, wherein the composite expanded graphite homogeneous plate comprises the following raw materials in parts by weight: 50-60 parts of modified polystyrene foam particles, 90-100 parts of Portland cement, 40-50 parts of vitrified micro-bead particles, 1.0-2.0 parts of redispersible latex powder, 0.5-1 part of hydroxypropyl methyl cellulose, 0.1-0.3 part of polypropylene fibers and 220-240 parts of water; the preparation steps are as follows: the method comprises the steps of paving a layer of alkali-resistant glass fiber network cloth at the bottom of a mold, mixing and stirring modified polystyrene foam particles, vitrified micro-bead particles and 1/2 mass water, adding portland cement, redispersible latex powder, hydroxypropyl methyl cellulose, polypropylene fibers and residual water, paving the mixture in the mold after continuously stirring, vibrating and compacting, pressing a layer of alkali-resistant glass fiber network cloth on the upper surface, and covering and maintaining the mixture by using a plastic film.
Description
Technical Field
The invention belongs to the technical field of building fireproof materials, and particularly relates to a composite expanded graphite homogeneous plate and a preparation method thereof.
Background
The homogeneous plate is a fireproof heat-insulating material, which is prepared by compounding silicon, calcium minerals, a modifier and expanded polystyrene foam particles, adding other additives, adding water, uniformly stirring, pressing and molding through a mold, and performing maintenance and processing.
The modified fireproof homogeneous plate disclosed in Chinese patent CN114478061B and the production process thereof comprise the following raw materials in parts by weight: 150-200 parts of polystyrene particles, 100-150 parts of portland cement, 15-35 parts of modified hydrotalcite, 30-65 parts of hyperbranched flame retardant, 15-30 parts of binder, 6-15 parts of foaming agent and 15-25 parts of water; this patent makes the even board reach fine flame retardant efficiency through adding self-made fire retardant, but the polystyrene granule is a hydrophobic material, dry polystyrene granule is more difficult for combining with matrix material, lead to the mechanical properties of even board not good, and because polystyrene is flammable, after the burning of catching fire, its position can form the hole, lead to near adjacent polystyrene granule direct exposure in the air, form the continuation of combustion, consequently, how to improve the associativity of polystyrene granule and matrix material, and it is the technical problem that needs to solve at present to overcome the defect that the polystyrene granule is flammable.
Disclosure of Invention
The invention aims to provide a composite expanded graphite homogeneous plate and a preparation method thereof, and aims to solve the problems in the background art.
The purpose of the invention can be realized by the following technical scheme:
a composite expanded graphite homogeneous plate comprises the following raw materials in parts by weight: 50-60 parts of modified polystyrene foam particles, 90-100 parts of Portland cement, 40-50 parts of vitrified micro-bead particles, 1.0-2.0 parts of redispersible latex powder, 0.5-1 part of hydroxypropyl methyl cellulose, 0.1-0.3 part of polypropylene fibers and 220-240 parts of water;
the composite expanded graphite homogeneous plate is prepared by the following steps:
laying a layer of alkali-resistant glass fiber network cloth at the bottom of a mold, coating a release agent on the periphery of the mold, adding the modified polystyrene foam particles, the vitrified micro bubbles and 1/2 mass of water into a stirrer, stirring for 15-30 seconds, adding portland cement, redispersible latex powder, hydroxypropyl methyl cellulose, polypropylene fiber and residual water, continuously stirring for 8-10min, then laying the mixture in the mold, vibrating and compacting, pressing a layer of alkali-resistant glass fiber network cloth on the upper surface, and covering and curing for 5-7 days by using a plastic film to obtain the composite expanded graphite uniform plate.
Further, the modified polystyrene foam particles are prepared by the following steps:
adding sodium hydroxide into 20wt% of isopropanol solution, stirring, adding polyvinyl alcohol, hydroxypropyl methyl cellulose and a crosslinking auxiliary agent, stirring for 1h to obtain a film forming solution, uniformly spraying the film forming solution on the surfaces of the flame-retardant polystyrene foam particles, carrying out heat preservation treatment at 60 ℃ for 10-15min, adding cement, and stirring to coat cement slurry on the surfaces of the flame-retardant polystyrene foam particles to obtain modified polystyrene foam particles;
wherein the dosage ratio of the isopropanol solution, the sodium hydroxide, the polyvinyl alcohol, the hydroxypropyl methyl cellulose and the crosslinking auxiliary agent is 100mL:3.4-4.2g:5.8-6.4g:4.7-5.1g:1.9-3.2g, and the using amount of the film-forming liquid and the cement is 10-15% of the mass of the flame-retardant polystyrene foam.
In order to improve the binding property between the polystyrene foam particles and a matrix, the invention prepares a film-forming solution, the film-forming solution takes hydrophilic polyvinyl alcohol and hydroxypropyl methyl fiber as main materials and is matched with a crosslinking assistant to obtain the modified polystyrene foam particles, under the condition of heating, the film-forming solution is sprayed on the surfaces of the flame-retardant polystyrene foam particles, epoxy groups and aldehyde groups in the crosslinking assistant can react with hydroxyl groups in the structures of the polyvinyl alcohol and the hydroxypropyl methyl fiber to form hydrophilic crosslinked films on the surfaces of the flame-retardant polystyrene foam particles, phosphate groups with a flame-retardant structure are introduced to endow the crosslinked films with flame-retardant property, and finally, the hydrophilicity of the crosslinked films is utilized to combine cement, so that the surfaces of the flame-retardant polystyrene foam particles are coated with cement slurry by stirring to obtain the modified polystyrene foam particles.
Further, the crosslinking assistant is prepared by the following steps:
step S11, adding 3,4-dihydroxybenzaldehyde, triethylamine and THF into a reaction kettle, stirring, dropwise adding a THF solution of phenylphosphoryl dichloride, heating to reflux reaction for 12 hours after dropwise adding, removing THF through rotary evaporation, washing a product with deionized water, and drying to obtain an intermediate product;
wherein, the dosage ratio of 3,4-dihydroxy benzaldehyde, triethylamine and phenyl phosphoryl dichloride is 0.08mol:0.08mol:0.04mol, and obtaining an intermediate containing terminal aldehyde group, phosphate group and phenolic hydroxyl group by utilizing the elimination reaction of hydroxyl group with larger activity of 3,4-dihydroxy benzaldehyde and chlorine of phenyl phosphoryl dichloride;
step S12, adding the intermediate product, potassium hydroxide and DMF into a reaction kettle, stirring and dissolving, then adding epoxy chloropropane, stirring and reacting for 4-5h at 70 ℃ under the protection of nitrogen, cooling to room temperature after the reaction is finished, dropwise adding 40wt% of potassium hydroxide solution, heating to 60 ℃, stirring and reacting for 6h, cooling to room temperature, filtering, and performing rotary evaporation on filtrate to remove DMF to obtain a crosslinking assistant;
wherein the dosage ratio of the intermediate product, the potassium hydroxide, the DMF, the epichlorohydrin and the potassium hydroxide solution is 4.7g:0.56g:100mL of: 0.2mol:8.4g, carrying out HCl elimination reaction on epoxy chloropropane and phenolic hydroxyl of the intermediate product 1 to introduce an epoxy group, and obtaining the crosslinking assistant containing the epoxy group, phosphate group, aldehyde group and benzene ring structure.
Further, the flame retardant polystyrene foam particles are prepared by the following steps:
step S21, adding a coupling agent KH-570 ethanol solution with the mass fraction of 4% into an expandable graphite ethanol solution with the mass fraction of 2%, stirring and reacting for 2-4h at 80 ℃, centrifugally washing, and drying at 60 ℃ to obtain modified expandable graphite, wherein the volume ratio of the KH-570 ethanol solution to the expandable graphite ethanol solution is 1:100;
step S22, adding the modified expandable graphite and styrene into a reaction kettle, adding benzoyl peroxide under stirring, stirring for 2 hours at 80 ℃, adding an aqueous solution of a dispersing agent, heating to 95 ℃, stirring for reaction for 5-10 hours, adding pentane, reacting at 120 ℃, 0.7-0.9MPa at constant temperature for 4-6 hours, cooling, discharging, washing, drying, foaming and forming to obtain the flame-retardant polystyrene foam particles, wherein the mass ratio of the aqueous solution of the modified expandable graphite, the styrene, the benzoyl peroxide and the dispersing agent to the pentane is 2-4:100:3:100-120:50, the water solution of the dispersing agent is prepared from polyvinyl alcohol, active calcium phosphate and deionized water according to the mass ratio of 0.3:1.5-2:100, the components are mixed.
In order to overcome the problem that polystyrene foam particles are flammable, the invention starts from a polystyrene preparation source, styrene and modified expandable graphite are used as polymerization monomers to prepare polystyrene foam particles doped with graphite, and expandable graphite is introduced to improve the mechanical strength of the polystyrene foam particles and endow the polystyrene foam particles with flame retardant property.
Furthermore, the Portland cement is P.042.5 cement, and the length of the polypropylene fiber is 5-15mm.
Further, the weight of the alkali-resistant glass fiber mesh cloth is 125g/m 2 。
The invention has the beneficial effects that:
the invention uses modified polystyrene foam particles, silicate cement, vitrified microsphere particles and redispersible latex powder as main materials to prepare the homogeneous plate, which not only has good heat preservation performance, but also has excellent mechanical property and flame retardant property.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A flame retardant polystyrene foam particle made by the steps of:
step S21, adding 5mL of coupling agent KH-570 ethanol solution with the mass fraction of 4% into 500mL of expandable graphite ethanol solution with the mass fraction of 2%, stirring and reacting for 2h at 80 ℃, centrifugally washing, and drying at 60 ℃ to obtain modified expandable graphite with the particle size of below 200 meshes;
step S22, adding 2g of modified expandable graphite and 100g of styrene into a reaction kettle, adding 3g of benzoyl peroxide under stirring, stirring for 2h at 80 ℃, adding 100mL of aqueous solution of a dispersing agent, heating to 95 ℃, stirring for reaction for 5h, adding 50g of pentane, heating to 120 ℃, and carrying out 0.7MPa, carrying out constant-temperature reaction for 4h, cooling, discharging, washing, drying, and carrying out foaming molding to obtain the flame-retardant polystyrene foam particles, wherein the aqueous solution of the dispersing agent is prepared from polyvinyl alcohol, active calcium phosphate and deionized water according to a mass ratio of 0.3:1.5: 100.
Example 2
A flame retardant polystyrene foam particle made by the steps of:
step S21, adding 5mL of coupling agent KH-570 ethanol solution with the mass fraction of 4% into 500mL of expandable graphite ethanol solution with the mass fraction of 2%, stirring and reacting for 4h at 80 ℃, centrifugally washing, and drying at 60 ℃ to obtain modified expandable graphite with the particle size of below 200 meshes;
step S22, adding 4g of modified expandable graphite and 100g of styrene into a reaction kettle, adding 3g of benzoyl peroxide under stirring, stirring for 2 hours at 80 ℃, adding 120mL of aqueous solution of a dispersing agent, heating to 95 ℃, stirring for reaction for 10 hours, adding 50g of pentane, 120 ℃, 0.9MPa, reacting for 6 hours at constant temperature, cooling, discharging, washing, drying, foaming and forming to obtain the flame-retardant polystyrene foam particles, wherein the aqueous solution of the dispersing agent is prepared from polyvinyl alcohol, active calcium phosphate and deionized water according to a mass ratio of 0.3:2: 100.
Example 3
A modified polystyrene foam particle made by the steps of:
adding 3.4g of sodium hydroxide into 100mL of a 20wt% isopropanol solution, stirring, adding 5.8g of polyvinyl alcohol, 4.7g of hydroxypropyl methyl cellulose and 1.9g of crosslinking aid, stirring for 1h to obtain a film-forming solution, uniformly spraying the film-forming solution on the surface of the flame-retardant polystyrene foam particles, carrying out heat preservation treatment at 60 ℃ for 10min, adding cement, stirring to coat the surface of the flame-retardant polystyrene foam particles with cement slurry, and obtaining modified polystyrene foam particles, wherein the using amount of the film-forming solution and the cement is 10% of the mass of the flame-retardant polystyrene foam.
The crosslinking assistant is prepared by the following steps:
step S11, adding 0.08mol of 3, 4-dihydroxybenzaldehyde, 0.08mol of triethylamine and 110mL of THF into a reaction kettle, stirring, dropwise adding 70mL of THF solution containing 0.04mol of phenylphosphoryl dichloride, heating to reflux reaction for 12 hours after dropwise adding is finished, removing THF through rotary evaporation, washing a product with deionized water, and drying to obtain an intermediate product;
and S12, adding 4.7g of intermediate product, 0.56g of potassium hydroxide and 100mL of DMF into a reaction kettle, stirring and dissolving, adding 0.2mol of epoxy chloropropane, stirring and reacting at 70 ℃ for 4h under the protection of nitrogen, cooling to room temperature after the reaction is finished, dropwise adding 8.4g of 40wt% potassium hydroxide solution, heating to 60 ℃, stirring and reacting for 6h, cooling to room temperature, filtering, and performing rotary evaporation on filtrate to remove DMF to obtain the crosslinking aid.
Example 4
A modified polystyrene foam particle made by the steps of:
adding 4.2g of sodium hydroxide into 100mL of a 20wt% isopropanol solution, stirring, adding 6.4g of polyvinyl alcohol, 5.1g of hydroxypropyl methyl cellulose and 3.2g of crosslinking aid, stirring for 1h to obtain a film-forming solution, uniformly spraying the film-forming solution on the surface of the flame-retardant polystyrene foam particles, carrying out heat preservation treatment at 60 ℃ for 15min, adding cement, stirring to coat the surface of the flame-retardant polystyrene foam particles with cement slurry, and obtaining modified polystyrene foam particles, wherein the using amount of the film-forming solution and the cement is 15% of the mass of the flame-retardant polystyrene foam.
The crosslinking assistant is prepared by the following steps:
step S11, adding 0.08mol of 3, 4-dihydroxybenzaldehyde, 0.08mol of triethylamine and 110mL of THF into a reaction kettle, stirring, dropwise adding 70mL of THF solution containing 0.04mol of phenylphosphoryl dichloride, heating to reflux reaction for 12 hours after dropwise adding is finished, removing THF through rotary evaporation, washing a product with deionized water, and drying to obtain an intermediate product;
and S12, adding 4.7g of intermediate product, 0.56g of potassium hydroxide and 100mL of DMF into a reaction kettle, stirring and dissolving, adding 0.2mol of epoxy chloropropane, stirring and reacting at 70 ℃ for 5h under the protection of nitrogen, cooling to room temperature after the reaction is finished, dropwise adding 8.4g of 40wt% potassium hydroxide solution, heating to 60 ℃, stirring and reacting for 6h, cooling to room temperature, filtering, and performing rotary evaporation on filtrate to remove DMF to obtain the crosslinking aid.
Comparative example 1
A modified polystyrene foam particle made by the steps of:
adding 6.4g of polyvinyl alcohol and 5.1g of hydroxypropyl methyl cellulose into 100mL of water, stirring for 1h to obtain a film-forming solution, uniformly spraying the film-forming solution on the surface of the flame-retardant polystyrene foam particles, stirring for 15min, adding cement, and stirring to coat the surface of the flame-retardant polystyrene foam particles with cement slurry to obtain modified polystyrene foam particles, wherein the using amounts of the film-forming solution and the cement are 15% of the mass of the flame-retardant polystyrene foam.
Example 5
A composite expanded graphite homogeneous plate comprises the following raw materials in parts by weight: 50 parts of modified polystyrene foam particles, 90 parts of Portland cement, 40 parts of vitrified microsphere particles, 1.0 part of redispersible latex powder, 0.5 part of hydroxypropyl methyl cellulose, 0.1 part of polypropylene fibers and 220 parts of water in example 3;
the composite expanded graphite homogeneous plate is prepared by the following steps:
laying a layer of alkali-resistant glass fiber network cloth at the bottom of a mold, coating a release agent on the periphery of the mold, adding modified polystyrene foam particles, vitrified micro-bead particles and 1/2 mass of water into a stirrer, stirring for 15 seconds, adding portland cement, redispersible latex powder, hydroxypropyl methyl cellulose, polypropylene fibers and residual water, continuously stirring for 8 minutes, laying the mixture in the mold, vibrating for compacting, pressing a layer of alkali-resistant glass fiber network cloth on the upper surface, covering and maintaining for 5 days by using a plastic film, and obtaining the composite expanded graphite homogeneous plate.
Wherein the Portland cement is P.042.5 cement, the polypropylene fiber length is 5-15mm, and the alkali-resistant glass fiber mesh cloth weight is 125g/m 2 。
Example 6
A composite expanded graphite homogeneous plate comprises the following raw materials in parts by weight: 55 parts of modified polystyrene foam particles, 95 parts of Portland cement, 45 parts of vitrified microsphere particles, 1.6 parts of redispersible latex powder, 0.8 part of hydroxypropyl methyl cellulose, 0.2 part of polypropylene fibers and 230 parts of water in example 3;
the composite expanded graphite homogeneous plate is prepared by the following steps:
spreading a layer of alkali-resistant glass fiber network cloth at the bottom of the mold, coating a release agent on the periphery of the mold, adding the modified polystyrene foam particles, the vitrified micro-bead particles and 1/2 mass of water into a stirrer, stirring for 20 seconds, adding portland cement, redispersible latex powder, hydroxypropyl methyl cellulose, polypropylene fibers and residual water, continuously stirring for 9 minutes, spreading the mixture into the mold, vibrating for compacting, pressing a layer of alkali-resistant glass fiber network cloth on the upper surface, and covering and maintaining for 6 days by using a plastic film to obtain the composite expanded graphite homogeneous plate.
Wherein the Portland cement is P.042.5 cement, the polypropylene fiber length is 5-15mm, and the alkali-resistant glass fiber mesh cloth has a weight of 125g/m 2 。
Example 7
A composite expanded graphite homogeneous plate comprises the following raw materials in parts by weight: 60 parts of modified polystyrene foam particles, 100 parts of portland cement, 50 parts of vitrified microsphere particles, 2.0 parts of redispersible latex powder, 1 part of hydroxypropyl methyl cellulose, 0.3 part of polypropylene fibers and 240 parts of water in example 4;
the composite expanded graphite homogeneous plate is prepared by the following steps:
laying a layer of alkali-resistant glass fiber network cloth at the bottom of a mold, coating a release agent on the periphery of the mold, adding modified polystyrene foam particles, vitrified micro-bead particles and 1/2 mass of water into a stirrer, stirring for 30 seconds, adding portland cement, redispersible latex powder, hydroxypropyl methyl cellulose, polypropylene fibers and residual water, continuously stirring for 10 minutes, laying the mixture in the mold, vibrating for compacting, pressing a layer of alkali-resistant glass fiber network cloth on the upper surface, covering and maintaining for 7 days by using a plastic film, and obtaining the composite expanded graphite homogeneous plate.
Wherein the Portland cement is P.042.5 cement, the polypropylene fiber length is 5-15mm, and the alkali-resistant glass fiber mesh cloth weight is 125g/m 2 。
Comparative example 2
In comparison with example 5, the modified polystyrene foam particles of example 5 were replaced with the material of example 1, and the rest of the raw materials and the preparation process were the same as those of example 5.
Comparative example 3
In comparison with example 5, the modified polystyrene foam particles of example 5 were replaced with the material of comparative example 1, and the remaining raw materials and preparation process were the same as those of example 5.
The homogeneous plates prepared in examples 5-7 and comparative examples 2-3 are subjected to performance tests, the compressive strength is detected according to GB/T5486-2008, the thermal conductivity is detected according to GB/T10294-2008, the combustion grade of the plate is detected according to GB8624-2012, and the test results are shown in Table 1:
TABLE 1
| Item | Example 5 | Example 6 | Example 7 | Comparative example 2 | Comparative example 3 |
| Compressive strength (MPa) | 1.42 | 1.56 | 1.78 | 0.92 | 1.31 |
| Thermal conductivity (W/(m. K) | 0.022 | 0.020 | 0.019 | 0.034 | 0.024 |
| Grade of combustion | Class A | Class A | Class A | Class B1 | Class B1 |
As can be seen from Table 1, compared with comparative examples 2 to 3, the homogeneous plates prepared in examples 5 to 7 have good thermal insulation performance, and good mechanical properties and flame retardant properties.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The composite expanded graphite homogeneous plate is characterized by comprising the following raw materials in parts by weight: 50-60 parts of modified polystyrene foam particles, 90-100 parts of Portland cement, 40-50 parts of vitrified micro-bead particles, 1.0-2.0 parts of redispersible latex powder, 0.5-1 part of hydroxypropyl methyl cellulose, 0.1-0.3 part of polypropylene fibers and 220-240 parts of water;
the modified polystyrene foam particles are prepared by the following steps:
adding sodium hydroxide into 20wt% of isopropanol solution, stirring, adding polyvinyl alcohol, hydroxypropyl methyl cellulose and a crosslinking assistant, stirring for 1h to obtain a film forming solution, uniformly spraying the film forming solution on the surfaces of the flame-retardant polystyrene foam particles, carrying out heat preservation treatment at 60 ℃ for 10-15min, adding cement, and stirring to coat cement slurry on the surfaces of the flame-retardant polystyrene foam particles to obtain the modified polystyrene foam particles.
2. The composite expanded graphite homogeneous plate as set forth in claim 1, wherein the amount ratio of isopropyl alcohol solution, sodium hydroxide, polyvinyl alcohol, hydroxypropylmethyl cellulose and crosslinking aid is 100mL:3.4-4.2g:5.8-6.4g:4.7-5.1g:1.9-3.2g, and the using amount of the film-forming liquid and the cement is 10-15% of the mass of the flame-retardant polystyrene foam.
3. The composite expanded graphite homogeneous sheet according to claim 1, wherein the crosslinking assistant is prepared by the steps of:
step S11, adding 3,4-dihydroxybenzaldehyde, triethylamine and THF into a reaction kettle, stirring, dropwise adding a THF solution of phenylphosphoryl dichloride, and after dropwise adding, carrying out reflux reaction for 12 hours to obtain an intermediate product;
and S12, adding the intermediate product, potassium hydroxide and DMF into a reaction kettle, stirring and dissolving, adding epoxy chloropropane, stirring and reacting for 4-5h at 70 ℃ under the protection of nitrogen, cooling to room temperature after the reaction is finished, dropwise adding 40wt% of potassium hydroxide solution, heating to 60 ℃, stirring and reacting for 6h, cooling to room temperature, filtering, and performing rotary evaporation on filtrate to remove DMF to obtain the crosslinking assistant.
4. The composite expanded graphite homogeneous plate as set forth in claim 3, wherein 3,4-dihydroxybenzaldehyde, triethylamine and phenylphosphoryl dichloride are used in a ratio of 0.08mol:0.08mol:0.04mol.
5. The composite expanded graphite homogeneous plate as set forth in claim 3, wherein the amount ratio of the intermediate product, potassium hydroxide, DMF, epichlorohydrin and potassium hydroxide solution is 4.7g:0.56g:100mL of: 0.2mol:8.4g.
6. A composite expanded graphite homogeneous sheet according to claim 1, wherein the flame-retardant polystyrene foam particles are produced by the steps of:
step S21, adding a coupling agent KH-570 ethanol solution with the mass fraction of 4% into an expandable graphite ethanol solution with the mass fraction of 2%, stirring and reacting for 2-4h at 80 ℃, centrifuging, washing and drying to obtain modified expandable graphite;
and S22, adding the modified expandable graphite and styrene into a reaction kettle, adding benzoyl peroxide while stirring, stirring for 2 hours at the temperature of 80 ℃, adding an aqueous solution of a dispersing agent, heating to 95 ℃, stirring for reaction for 5-10 hours, adding pentane, reacting at the temperature of 120 ℃ and under the pressure of 0.7-0.9MPa for 4-6 hours at a constant temperature, cooling, discharging, washing, drying, foaming and forming to obtain the flame-retardant polystyrene foam particles.
7. A composite expanded graphite homogeneous plate according to claim 6, wherein the volume ratio of KH-570 ethanol solution to expandable graphite ethanol solution is 1:100.
8. the composite type expanded graphite homogeneous plate according to claim 6, wherein the mass ratio of the aqueous solution of the modified expandable graphite, the styrene, the benzoyl peroxide, the dispersing agent and the pentane is 2-4:100:3:100-120:50, the water solution of the dispersing agent is prepared from polyvinyl alcohol, active calcium phosphate and deionized water according to the mass ratio of 0.3:1.5-2: 100.
9. The method for producing a composite expanded graphite homogeneous sheet according to claim 1, comprising the steps of:
spreading a layer of alkali-resistant glass fiber network cloth at the bottom of the mold, coating a release agent on the periphery of the mold, adding the modified polystyrene foam particles, the vitrified micro-bead particles and 1/2 mass of water into a stirrer, adding portland cement, redispersible latex powder, hydroxypropyl methyl cellulose, polypropylene fibers and residual water after stirring, spreading the mixture in the mold after continuously stirring, vibrating and compacting, pressing a layer of alkali-resistant glass fiber network cloth on the upper surface, covering and maintaining the mixture by using a plastic film for 5-7 days, and obtaining the composite expanded graphite uniform plate.
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| CN1673166A (en) * | 2004-03-22 | 2005-09-28 | 常州市宇乔建材科技有限公司 | Heat insulating mortar powder and its prepn process |
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| CN1673166A (en) * | 2004-03-22 | 2005-09-28 | 常州市宇乔建材科技有限公司 | Heat insulating mortar powder and its prepn process |
| CN102391588A (en) * | 2011-05-26 | 2012-03-28 | 中国科学院过程工程研究所 | High-flame-retardant low-smoke-density polystyrene foam compound heat insulating material and preparation method thereof |
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