CN117186278A - Method for preparing environment-friendly flame-retardant expandable polystyrene - Google Patents
Method for preparing environment-friendly flame-retardant expandable polystyrene Download PDFInfo
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- CN117186278A CN117186278A CN202311241108.5A CN202311241108A CN117186278A CN 117186278 A CN117186278 A CN 117186278A CN 202311241108 A CN202311241108 A CN 202311241108A CN 117186278 A CN117186278 A CN 117186278A
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- expandable polystyrene
- friendly flame
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- graphene oxide
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- 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 title claims abstract description 88
- 239000003063 flame retardant Substances 0.000 title claims abstract description 88
- 229920006248 expandable polystyrene Polymers 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 49
- 239000002270 dispersing agent Substances 0.000 claims abstract description 45
- 238000002360 preparation method Methods 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000004088 foaming agent Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000007599 discharging Methods 0.000 claims abstract description 13
- 239000003999 initiator Substances 0.000 claims description 73
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 65
- 239000003153 chemical reaction reagent Substances 0.000 claims description 46
- 229910021389 graphene Inorganic materials 0.000 claims description 33
- 239000002131 composite material Substances 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 24
- 239000003381 stabilizer Substances 0.000 claims description 23
- 239000002667 nucleating agent Substances 0.000 claims description 22
- 239000004014 plasticizer Substances 0.000 claims description 22
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims description 17
- ILOKQJWLMPPMQU-UHFFFAOYSA-N calcium;oxido(oxo)borane Chemical compound [Ca+2].[O-]B=O.[O-]B=O ILOKQJWLMPPMQU-UHFFFAOYSA-N 0.000 claims description 15
- -1 hexadecyl ester Chemical class 0.000 claims description 15
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 13
- FIYMNUNPPYABMU-UHFFFAOYSA-N 2-benzyl-5-chloro-1h-indole Chemical compound C=1C2=CC(Cl)=CC=C2NC=1CC1=CC=CC=C1 FIYMNUNPPYABMU-UHFFFAOYSA-N 0.000 claims description 11
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 11
- 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 11
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 10
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- 150000001993 dienes Chemical class 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- 239000006260 foam Substances 0.000 claims description 9
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 8
- CRSOQBOWXPBRES-UHFFFAOYSA-N neopentane Chemical compound CC(C)(C)C CRSOQBOWXPBRES-UHFFFAOYSA-N 0.000 claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 7
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 7
- 239000005642 Oleic acid Substances 0.000 claims description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000013067 intermediate product Substances 0.000 claims description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 7
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- 125000002252 acyl group Chemical group 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 4
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 4
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 4
- NOBYOEQUFMGXBP-UHFFFAOYSA-N (4-tert-butylcyclohexyl) (4-tert-butylcyclohexyl)oxycarbonyloxy carbonate Chemical compound C1CC(C(C)(C)C)CCC1OC(=O)OOC(=O)OC1CCC(C(C)(C)C)CC1 NOBYOEQUFMGXBP-UHFFFAOYSA-N 0.000 claims description 3
- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 claims description 3
- 230000002708 enhancing effect Effects 0.000 claims description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 22
- 239000002994 raw material Substances 0.000 description 21
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 20
- 239000001506 calcium phosphate Substances 0.000 description 20
- 229910000389 calcium phosphate Inorganic materials 0.000 description 20
- 235000011010 calcium phosphates Nutrition 0.000 description 20
- 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 description 20
- 239000000047 product Substances 0.000 description 19
- 238000001723 curing Methods 0.000 description 15
- 239000004698 Polyethylene Substances 0.000 description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 description 10
- 239000003822 epoxy resin Substances 0.000 description 10
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 10
- 239000004137 magnesium phosphate Substances 0.000 description 10
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 10
- 229960002261 magnesium phosphate Drugs 0.000 description 10
- 235000010994 magnesium phosphates Nutrition 0.000 description 10
- 229920000647 polyepoxide Polymers 0.000 description 10
- 229920000573 polyethylene Polymers 0.000 description 10
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 10
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 10
- 229910000165 zinc phosphate Inorganic materials 0.000 description 10
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 9
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical group C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 description 9
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 9
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 9
- 238000001914 filtration Methods 0.000 description 9
- 229920003048 styrene butadiene rubber Polymers 0.000 description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 238000010992 reflux Methods 0.000 description 6
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- 239000004793 Polystyrene Substances 0.000 description 4
- 229920002223 polystyrene Polymers 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- RWPGFSMJFRPDDP-UHFFFAOYSA-L potassium metabisulfite Chemical compound [K+].[K+].[O-]S(=O)S([O-])(=O)=O RWPGFSMJFRPDDP-UHFFFAOYSA-L 0.000 description 2
- 229940043349 potassium metabisulfite Drugs 0.000 description 2
- 235000010263 potassium metabisulphite Nutrition 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 2
- 238000010557 suspension polymerization reaction Methods 0.000 description 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229920003064 carboxyethyl cellulose Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000004794 expanded polystyrene Substances 0.000 description 1
- 238000009422 external insulation Methods 0.000 description 1
- 238000010097 foam moulding Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- QYZLKGVUSQXAMU-UHFFFAOYSA-N penta-1,4-diene Chemical compound C=CCC=C QYZLKGVUSQXAMU-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920006327 polystyrene foam Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
Abstract
The application relates to the field of expandable polystyrene synthesis technology, and in particular discloses a method for preparing environment-friendly flame-retardant expandable polystyrene. The method for preparing the environment-friendly flame-retardant expandable polystyrene comprises the following steps: adding pure water, water-based auxiliary materials, styrene and oil-based auxiliary materials into a reaction kettle in sequence, heating and preserving heat through steam, adding a dispersing agent B and a foaming agent after low-temperature polymerization is completed, heating and entering high-temperature polymerization, and cooling and discharging after the polymerization is completed. The preparation method can effectively reduce the pollution to water, thereby being more environment-friendly and more energy-saving.
Description
Technical Field
The application relates to the field of expandable polystyrene synthesis technology, in particular to a method for preparing environment-friendly flame-retardant expandable polystyrene.
Background
The Expandable Polystyrene (EPS) is prepared from pure water, styrene, benzoyl peroxide, tert-butyl peroxybenzoate, pentane, a structure regulator, a flame retardant (methyl octabromoether, brominated SBS) and other raw materials through the steps of stirring, heating, suspension polymerization, washing, screening and the like. The foaming agent-containing expandable polystyrene beads can be subjected to pre-foaming, curing and foam molding to obtain the foam plastic product. Foamed polystyrene foam articles are currently extremely valuable insulating, heat preserving and packaging cushioning materials. The polystyrene foam plastic has low water absorption, excellent heat insulation and dielectric property and high mechanical strength.
The expandable polystyrene products in the current market are influenced by auxiliary material factors such as flame retardant, initiator, stabilizer and the like, most of the products have a plurality of defects such as high residue, low conversion rate, unstable flame retardance and the like, and particularly auxiliary materials which act on the system externally pollute water greatly, such as substances such as sodium dodecyl benzene sulfonate, anhydrous sodium sulfate and the like, so that the sewage treatment cost is high.
Disclosure of Invention
In order to reduce the pollution of auxiliary materials of an external system to water quality in the synthesis process of the expandable polystyrene and reduce the sewage treatment cost, the application provides a method for preparing environment-friendly flame-retardant expandable polystyrene, which adopts the following technical scheme:
a method for preparing environment-friendly flame-retardant expandable polystyrene, comprising the following steps:
s1, adding 110 parts by weight of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.06 to 0.08 weight part of dispersant A,0.0014 to 0.0018 weight part of reagent A and 0.001 to 0.0012 weight part of reagent B;
s2, adding 100 parts by weight of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.25 to 0.55 weight part of initiator A,0.03 to 0.08 weight part of initiator B,0.2 to 0.5 weight part of initiator C,0.6 to 0.9 weight part of flame retardant, 0.2 to 0.6 weight part of plasticizer, 0.005 to 0.008 weight part of stabilizer and 0.1 to 0.2 weight part of nucleating agent;
s3, heating to 88-90 ℃ and reacting for 5-6 hours;
s4, adding 0.2 to 0.3 weight part of dispersant B, and then adding 0.5 to 1.2 weight parts of foaming agent;
s5, heating to 118-130 ℃ and reacting for 2.5-5 hours;
s6, cooling and discharging.
By adopting the technical scheme, the auxiliary materials of the reaction system are changed, so that the system is more stable and more environment-friendly; the material residue after the reaction is reduced, and the sewage treatment is more effective and energy-saving; the polymerization and the impregnation are completed in one kettle, so that the production time is saved and the production period is shortened.
Preferably, the initiator A is one or more of azodiisobutyronitrile, benzoyl peroxide and tert-butyl peroxy-2-ethyl hexyl carbonate.
Preferably, the initiator B is one or more of dicumyl peroxide, bis (4-tert-butylcyclohexyl) peroxydicarbonate and hexadecyl ester.
Preferably, the initiator C is one or more of tert-butyl peroxybenzoate, tert-butyl peroxyneodecanoate and tert-butyl peroxycarbonate-2-ethylhexyl.
Preferably, the foaming agent is one or more of n-pentane, isopentane and neopentane.
Preferably, the reagent A is one or more of polyvinyl alcohol, carboxymethyl cellulose and ethyl cellulose.
Preferably, the reagent B is one of potassium metabisulfite or potassium persulfate.
Preferably, the foaming agent is one or more of n-pentane, isopentane and neopentane.
Preferably, the oily auxiliary material further comprises 0.5-1.5 parts by weight of reinforced modified composite powder, wherein the reinforced modified composite powder comprises modified graphene oxide, calcium metaborate and polyethylene glycol monomethyl ether.
According to the technical scheme, polyethylene glycol monomethyl ether is used as a connecting agent of the modified graphene oxide and the calcium metaborate, and the molecular chain on the surface of the modified graphene oxide and the interlayer structure of the calcium metaborate are utilized, so that the modified graphene oxide and the calcium metaborate are tightly connected, and further the dispersibility of the modified graphene oxide is improved due to the influence of the physical property of the calcium metaborate.
Preferably, the reinforced modified composite powder is prepared by the following steps: mixing and ball milling calcium metaborate and oleic acid mixed with polyethylene glycol monomethyl ether, then adding modified graphene oxide, and continuing mixing and ball milling, thereby enhancing the modified composite powder.
According to the technical scheme, firstly, the oleic acid is used as a medium to enable polyethylene glycol monomethyl ether and calcium metaborate to be gathered, meanwhile, the calcium metaborate is crushed and thinned, and then the modified graphene oxide is added, so that the polyethylene glycol monomethyl ether and the modified graphene oxide are combined in the ball milling process of the crushed and thinned calcium metaborate, and the dispersion performance of the modified graphene oxide is improved.
Preferably, the modified graphene oxide is prepared from graphene oxide, unsaturated fatty acid and conjugated diene.
Through adopting above-mentioned technical scheme, at first with the oxidation graphene with unsaturated fatty acid combines and carries out acyl chlorination to make the compatibility of modified oxidation graphene in oily auxiliary material improve, more be convenient for the dispersion of modified oxidation graphene in oily auxiliary material, then form the oxidation graphene that contains cyclic unsaturated fatty acid through the unsaturated fatty acid on the oxidation graphene and conjugated diene, and then improve the whole stability of modified oxidation graphene when improving oxidation graphene dispersion.
Preferably, the modified graphene oxide is prepared by the following steps: s1, carrying out acyl chlorination reaction on graphene oxide and unsaturated fatty acid to obtain an intermediate product; s2, reacting the intermediate product with conjugated diene to generate final modified graphene oxide.
Through adopting above-mentioned technical scheme, at first carry out unsaturated fatty acid modification to graphene oxide, make its dispersibility in oily auxiliary material promote, then carry out the closed loop to unsaturated fatty acid on the graphene oxide to make unsaturated fatty acid stability on the graphene oxide promote.
Preferably, the expandable polystyrene is used for preparing foam boards, and the preparation steps are as follows: the environment-friendly flame-retardant expandable polystyrene is subjected to pre-expansion, curing and forming processes to prepare the foam board.
In summary, the application has the following beneficial effects:
1. the application uses the more advanced and stable emulsifier to replace the original sodium dodecyl benzene sulfonate, so that the pollution to water is reduced, the suspension polymerization in the early stage is more stable, and the substance residue after the reaction is finished is reduced, thereby reducing the later-stage defoamer, and the sewage treatment is more effective and energy-saving.
2. The preparation method of the application improves the conversion rate, reduces the residual of styrene monomer, ensures that the product structure is more stable, reduces the high-temperature residual monomer from 0.3% to 0.05%, and greatly improves the conversion rate of the product.
3. The preparation method improves the concentration of effective particles from 65% to 75%, and increases the product income.
4. The preparation method of the application eliminates toluene and eliminates residue in the product.
5. In the application, the strength of the prepared plate is preferably improved by adopting the graphene oxide, and meanwhile, the graphene oxide is subjected to double modification, so that the graphene oxide subjected to double modification is uniformly dispersed, and the performance of the plate is more favorably improved.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example
Preparation example 1
The preparation example discloses modified graphene oxide, which is prepared by the following steps:
s1, unsaturated fatty acid functionalized graphene oxide: 0.5g of graphene oxide is taken and dissolved in 150mL of dehydrated DMF solvent, the solution is transferred into a 250mL four-neck flask equipped with a dry tail pipe and a tail gas removing device after being uniformly dispersed, 20mL of acrylic acid, 1mg of hydroquinone polymerization inhibitor and 30mg of triethylamine are added, 30mL of thionyl chloride is slowly added dropwise, magnetic stirring is carried out, nitrogen is introduced to protect acrylic acid and products from self-polymerization, and the solution is subjected to ice bath reaction for 2 hours and then is subjected to room temperature overnight. Filtering to remove a small amount of black insoluble substances after the reaction is finished, washing the filtrate with water to obtain a brown product, depositing the brown product at the bottom, standing, pouring out supernatant, repeatedly washing with water, centrifuging at high speed for 3 times at 10000 revolutions per minute, removing small molecular byproducts and a small amount of self-polymerized acrylic acid which are wrapped in the product, and freeze-drying at-40 ℃ to obtain a brown intermediate product;
s2, conjugated diene stable-curing graphene oxide: into a 50mL round bottom flask was charged 2g of the intermediate prepared in S1, 2g of butadiene and 25mL of anhydrous xylene, a reflux condenser was connected, and heated to reflux at 140℃for 25min. And (5) oscillating the crystals precipitated on the edge of the liquid level, continuing to heat for 5min, and stopping heating. And when the liquid is not refluxed, filtering the liquid through a Buchner funnel which is preheated by the heat, cooling the filtrate, filtering to separate out a solid product, and drying in a vacuum dryer to obtain the modified graphene oxide.
Preparation example 2
The preparation example discloses modified graphene oxide, which is prepared by the following steps:
s1, unsaturated fatty acid functionalized graphene oxide: 0.5g of graphene oxide is taken and dissolved in 150mL of dehydrated DMF solvent, the solution is transferred into a 250mL four-neck flask equipped with a dry tail pipe and a tail gas removing device after being uniformly dispersed, 20mL of linoleic acid, 1mg of hydroquinone polymerization inhibitor and 30mg of triethylamine are added, 30mL of thionyl chloride is slowly added dropwise, magnetic stirring is carried out, nitrogen is introduced to protect acrylic acid and a product from self-polymerization, and the solution is subjected to ice bath reaction for 2 hours and then is subjected to room temperature overnight. Filtering to remove a small amount of black insoluble substances after the reaction is finished, washing the filtrate with water to obtain a brown product, depositing the brown product at the bottom, standing, pouring out supernatant, repeatedly washing with water, centrifuging at high speed for 3 times at 10000 revolutions per minute, removing small molecular byproducts and a small amount of self-polymerized acrylic acid which are wrapped in the product, and freeze-drying at-40 ℃ to obtain a brown intermediate product;
s2, conjugated diene stable-curing graphene oxide: into a 50mL round bottom flask was charged 2g of the intermediate prepared in S1, 2g of butadiene and 25mL of anhydrous xylene, a reflux condenser was connected, and heated to reflux at 140℃for 25min. And (5) oscillating the crystals precipitated on the edge of the liquid level, continuing to heat for 5min, and stopping heating. Filtering the hot and intentionally preheated Buchner funnel when the liquid is not refluxed, cooling the filtrate, filtering to separate out a solid product, and drying in a vacuum dryer to obtain the modified graphene oxide
Preparation example 3
The preparation example discloses modified graphene oxide, which is prepared by the following steps:
s1, unsaturated fatty acid functionalized graphene oxide: 0.5g of graphene oxide is taken and dissolved in 150mL of dehydrated DMF solvent, the solution is transferred into a 250mL four-neck flask equipped with a dry tail pipe and a tail gas removing device after being uniformly dispersed, 20mL of acrylic acid, 1mg of hydroquinone polymerization inhibitor and 30mg of triethylamine are added, 30mL of thionyl chloride is slowly added dropwise, magnetic stirring is carried out, nitrogen is introduced to protect acrylic acid and products from self-polymerization, and the solution is subjected to ice bath reaction for 2 hours and then is subjected to room temperature overnight. Filtering to remove a small amount of black insoluble substances after the reaction is finished, washing the filtrate with water to obtain a brown product, depositing the brown product at the bottom, standing, pouring out supernatant, repeatedly washing with water, centrifuging at high speed for 3 times at 10000 revolutions per minute, removing small molecular byproducts and a small amount of self-polymerized acrylic acid which are wrapped in the product, and freeze-drying at-40 ℃ to obtain a brown intermediate product;
s2, conjugated diene stable-curing graphene oxide: into a 50mL round bottom flask was charged 2g of the intermediate obtained in S1, 2g of 1, 4-pentadiene and 25mL of anhydrous xylene, a reflux condenser was connected, and the mixture was heated at 140℃for 25min under reflux. And (5) oscillating the crystals precipitated on the edge of the liquid level, continuing to heat for 5min, and stopping heating. Filtering the hot and intentionally preheated Buchner funnel when the liquid is not refluxed, cooling the filtrate, filtering to separate out a solid product, and drying in a vacuum dryer to obtain the modified graphene oxide
Preparation example 4
The preparation example discloses reinforced modified composite powder, which is prepared by the following steps:
s1, mixing 2mL of polyethylene glycol monomethyl ether and 8mL of oleic acid, and then mixing with 4g of calcium metaborate, and ball milling for 10 hours;
s2, adding 1g of the modified graphene oxide prepared in the preparation example 1, and continuously ball milling for 10 hours to prepare the reinforced modified composite powder.
Preparation example 5
The preparation example discloses reinforced modified composite powder, which is prepared by the following steps:
s1, mixing 2mL of polyethylene glycol monomethyl ether and 8mL of oleic acid, and then mixing with 4g of calcium metaborate, and ball milling for 10 hours;
s2, adding 1g of the modified graphene oxide prepared in the preparation example 2, and continuously ball milling for 10 hours to prepare the reinforced modified composite powder.
Preparation example 6
The preparation example discloses reinforced modified composite powder, which is prepared by the following steps:
s1, mixing 2mL of polyethylene glycol monomethyl ether and 8mL of oleic acid, and then mixing with 4g of calcium metaborate, and ball milling for 10 hours;
s2, adding 1g of the modified graphene oxide prepared in the preparation example 3, and continuously ball milling for 10 hours to prepare the reinforced modified composite powder.
Preparation example 7
The preparation example discloses reinforced modified composite powder, which is prepared by the following steps:
s1, mixing and ball-milling 10mL of oleic acid and 4g of calcium metaborate for 10 hours;
s2, adding 1g of the modified graphene oxide prepared in the preparation example 3, and continuously ball milling for 10 hours to prepare the reinforced modified composite powder.
Examples
Example 1
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.06kg of dispersant A,0.0014kg of reagent A,0.001kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.25kg of initiator A,0.03kg of initiator B,0.2kg of initiator C,0.6kg of flame retardant, 0.2kg of plasticizer, 0.005kg of stabilizer and 0.1kg of nucleating agent;
s3, heating to 88 ℃, and reacting for 5 hours;
s4, adding 0.2kg of dispersant B, and then adding 0.5kg of foaming agent;
s5, heating to 118 ℃ and reacting for 2.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; the reagent A is polyvinyl alcohol; the reagent B is potassium metabisulfite; the initiator A is azodiisobutyronitrile; the initiator B is bis (4-tert-butylcyclohexyl) peroxydicarbonate; the initiator C is tert-butyl peroxybenzoate; the flame retardant is methyl octabromoether; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is isopentane.
Example 2
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.07kg of dispersant A,0.0016kg of reagent A,0.0011kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.4kg of initiator A,0.055kg of initiator B,0.35kg of initiator C,0.75kg of flame retardant, 0.4kg of plasticizer, 0.0065kg of stabilizer and 0.15kg of nucleating agent;
s3, heating to 89 ℃, and reacting for 5.5 hours;
s4, adding 0.25kg of dispersant B, and then adding 0.75kg of foaming agent;
s5, heating to 124 ℃, and reacting for 3.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxymethyl cellulose; the reagent B is potassium persulfate; the initiator A is benzoyl peroxide; the initiator B is dicumyl peroxide; the initiator C is tert-butyl peroxy-2-ethylhexyl carbonate; the flame retardant is brominated styrene butadiene copolymer; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is n-pentane.
Example 3
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.08kg of dispersant A,0.0018kg of reagent A and 0.0012kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.55kg of initiator A,0.08kg of initiator B,0.5kg of initiator C,0.9kg of flame retardant, 0.6kg of plasticizer, 0.008kg of stabilizer and 0.2kg of nucleating agent;
s3, heating to 90 ℃ and reacting for 6 hours;
s4, adding 0.3kg of dispersant B, and then adding 1.2kg of foaming agent;
s5, heating to 130 ℃, and reacting for 5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxyethyl cellulose; the reagent B is potassium persulfate; the initiator A is tert-butyl peroxy-2-ethyl hexyl carbonate; initiator B is hexadecyl ester; the initiator C is tert-butyl peroxyneodecanoate; the flame retardant is a mixture of brominated styrene butadiene copolymer and methyl octabromoether in a weight ratio of 1:1; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is neopentane.
Example 4
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.07kg of dispersant A,0.0016kg of reagent A,0.0011kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.4kg of initiator A,0.055kg of initiator B,0.35kg of initiator C,0.75kg of flame retardant, 0.4kg of plasticizer, 0.0065kg of stabilizer, 0.15kg of nucleating agent and 0.5kg of reinforced modified composite powder prepared in preparation example 4;
s3, heating to 89 ℃, and reacting for 5.5 hours;
s4, adding 0.25kg of dispersant B, and then adding 0.75kg of foaming agent;
s5, heating to 124 ℃, and reacting for 3.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxymethyl cellulose; the reagent B is potassium persulfate; the initiator A is benzoyl peroxide; the initiator B is dicumyl peroxide; the initiator C is tert-butyl peroxy-2-ethylhexyl carbonate; the flame retardant is brominated styrene butadiene copolymer; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is n-pentane.
Example 5
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.07kg of dispersant A,0.0016kg of reagent A,0.0011kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.4kg of initiator A,0.055kg of initiator B,0.35kg of initiator C,0.75kg of flame retardant, 0.4kg of plasticizer, 0.0065kg of stabilizer, 0.15kg of nucleating agent and 1kg of reinforced modified composite powder prepared in preparation example 4;
s3, heating to 89 ℃, and reacting for 5.5 hours;
s4, adding 0.25kg of dispersant B, and then adding 0.75kg of foaming agent;
s5, heating to 124 ℃, and reacting for 3.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxymethyl cellulose; the reagent B is potassium persulfate; the initiator A is benzoyl peroxide; the initiator B is dicumyl peroxide; the initiator C is tert-butyl peroxy-2-ethylhexyl carbonate; the flame retardant is brominated styrene butadiene copolymer; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is n-pentane.
Example 6
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.07kg of dispersant A,0.0016kg of reagent A,0.0011kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.4kg of initiator A,0.055kg of initiator B,0.35kg of initiator C,0.75kg of flame retardant, 0.4kg of plasticizer, 0.0065kg of stabilizer, 0.15kg of nucleating agent and 1.5kg of reinforced modified composite powder prepared in preparation example 4;
s3, heating to 89 ℃, and reacting for 5.5 hours;
s4, adding 0.25kg of dispersant B, and then adding 0.75kg of foaming agent;
s5, heating to 124 ℃, and reacting for 3.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxymethyl cellulose; the reagent B is potassium persulfate; the initiator A is benzoyl peroxide; the initiator B is dicumyl peroxide; the initiator C is tert-butyl peroxy-2-ethylhexyl carbonate; the flame retardant is brominated styrene butadiene copolymer; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is n-pentane.
Example 7
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.07kg of dispersant A,0.0016kg of reagent A,0.0011kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.4kg of initiator A,0.055kg of initiator B,0.35kg of initiator C,0.75kg of flame retardant, 0.4kg of plasticizer, 0.0065kg of stabilizer, 0.15kg of nucleating agent and 1kg of reinforced modified composite powder prepared in preparation example 5;
s3, heating to 89 ℃, and reacting for 5.5 hours;
s4, adding 0.25kg of dispersant B, and then adding 0.75kg of foaming agent;
s5, heating to 124 ℃, and reacting for 3.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxymethyl cellulose; the reagent B is potassium persulfate; the initiator A is benzoyl peroxide; the initiator B is dicumyl peroxide; the initiator C is tert-butyl peroxy-2-ethylhexyl carbonate; the flame retardant is brominated styrene butadiene copolymer; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is n-pentane.
Example 8
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.07kg of dispersant A,0.0016kg of reagent A,0.0011kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.4kg of initiator A,0.055kg of initiator B,0.35kg of initiator C,0.75kg of flame retardant, 0.4kg of plasticizer, 0.0065kg of stabilizer, 0.15kg of nucleating agent and 1kg of reinforced modified composite powder prepared in preparation example 6;
s3, heating to 89 ℃, and reacting for 5.5 hours;
s4, adding 0.25kg of dispersant B, and then adding 0.75kg of foaming agent;
s5, heating to 124 ℃, and reacting for 3.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxymethyl cellulose; the reagent B is potassium persulfate; the initiator A is benzoyl peroxide; the initiator B is dicumyl peroxide; the initiator C is tert-butyl peroxy-2-ethylhexyl carbonate; the flame retardant is brominated styrene butadiene copolymer; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is n-pentane.
Example 9
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.07kg of dispersant A,0.0016kg of reagent A,0.0011kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.4kg of initiator A,0.055kg of initiator B,0.35kg of initiator C,0.75kg of flame retardant, 0.4kg of plasticizer, 0.0065kg of stabilizer, 0.15kg of nucleating agent and 1kg of reinforced modified composite powder prepared in preparation example 7;
s3, heating to 89 ℃, and reacting for 5.5 hours;
s4, adding 0.25kg of dispersant B, and then adding 0.75kg of foaming agent;
s5, heating to 124 ℃, and reacting for 3.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxymethyl cellulose; the reagent B is potassium persulfate; the initiator A is benzoyl peroxide; the initiator B is dicumyl peroxide; the initiator C is tert-butyl peroxy-2-ethylhexyl carbonate; the flame retardant is brominated styrene butadiene copolymer; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is n-pentane.
Example 10
The embodiment discloses a method for preparing environment-friendly flame-retardant expandable polystyrene, which comprises the following steps:
s1, adding 110kg of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.07kg of dispersant A,0.0016kg of reagent A,0.0011kg of reagent B;
s2, adding 100kg of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.4kg of initiator A,0.055kg of initiator B,0.35kg of initiator C,0.75kg of flame retardant, 0.4kg of plasticizer, 0.0065kg of stabilizer, 0.15kg of nucleating agent and 1kg of modified graphene oxide prepared in preparation example 1;
s3, heating to 89 ℃, and reacting for 5.5 hours;
s4, adding 0.25kg of dispersant B, and then adding 0.75kg of foaming agent;
s5, heating to 124 ℃, and reacting for 3.5 hours;
s6, cooling and discharging to obtain the environment-friendly flame-retardant expandable polystyrene.
In this example dispersant a is active calcium phosphate; reagent A is carboxymethyl cellulose; the reagent B is potassium persulfate; the initiator A is benzoyl peroxide; the initiator B is dicumyl peroxide; the initiator C is tert-butyl peroxy-2-ethylhexyl carbonate; the flame retardant is brominated styrene butadiene copolymer; the plasticizer is epoxy resin; the stabilizer is a mixture of magnesium phosphate and zinc phosphate in a weight ratio of 1:1; the nucleating agent is polyethylene wax; dispersant B is a mixture of calcium phosphate and calcium carbonate in a weight ratio of 1:1; the foaming agent is n-pentane.
Application example
Application example 1
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 1, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, and the plate forming machineThe internal pressure is 0.06MPa, the steam pressure for forming the plate is 0.7MPa, and the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 2
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 2, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the steam pressure of the plate forming machine is 0.7MPa, so that the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 3
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 3, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the steam pressure of the plate forming machine is 0.7MPa, so that the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 4
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 4, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the plate forming vapor pressure is equal to that of the plate forming machineThe force is 0.7MPa, and the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 5
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 5, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the steam pressure of the plate forming machine is 0.7MPa, so that the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 6
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 6, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the steam pressure of the plate forming machine is 0.7MPa, so that the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 7
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 7, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the steam pressure of the plate forming machine is 0.7MPa, so that the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 8
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 8, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the steam pressure of the plate forming machine is 0.7MPa, so that the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 9
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 9, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the steam pressure of the plate forming machine is 0.7MPa, so that the apparent density is 22kg/m 3 Is a plate material of the (c).
Application example 10
The application example discloses a preparation method of an environment-friendly flame-retardant expandable polystyrene board, which comprises the following steps:
s1, pre-expanding the environment-friendly flame-retardant expandable polystyrene prepared in the embodiment 10, wherein the pre-expanding steam temperature is 100 ℃, and the steam pressure is 0.1MPa;
s2, curing the pre-developed raw materials for 24 hours;
s3, finally, placing the cured raw materials into a plate forming machine for forming, wherein the internal pressure of the plate forming machine is 0.06MPa, and the steam pressure of the plate forming machine is 0.7MPa, so that the apparent density is 22kg/m 3 Is a plate material of the (c).
Performance test
Thermal conductivity (thermal conductivity GB/T10294), flame retardant properties (flame retardant grades GB 8624-2012), tensile properties (JG 149-2003), compression properties (GB/T8813), dimensional stability (GB/T6342 dimensional deviation), breaking flexural load capacity (GB/T8812)
The panels prepared in application examples 1-10 were subjected to performance testing, and the test items and reference standards were as follows:
1. thermal conductivity coefficient, GB/T10294-2008 method for measuring steady-state thermal resistance and related characteristics of heat-insulating materials;
2. flame retardant rating, GB8624-2012 classification of combustion properties of building materials and articles;
3. tensile strength, JG149-2003, expanded polystyrene board thin plastering external wall external insulation System;
4. compression strength, GB/T8813-2020 determination of compression Property of rigid foam;
5. dimensional deviation, GB/T6342-1996 determination of Linear size of foam and rubber;
6. flexural load at break, GB/T8812-1988 method for flexural test of rigid foam.
Table 1 application examples 1-12 performance test data table
It can be seen from the combination of application examples 2 and 5 and the combination of table 1 that the performance of the board can be effectively improved by adding the reinforcing modified composite powder, and the addition of the flame retardant makes the prepared polystyrene have reduced performance due to poor compatibility based on the scheme of application example 2, while the reinforcing modified composite powder compensates for the reduced performance of the polystyrene caused by the addition of the flame retardant.
It can be seen from the combination of application examples 4, 5 and 6 and the combination of table 1 that the properties of the finally prepared polystyrene are changed by adjusting the addition amount of the reinforced modified composite powder, and the properties of the polystyrene can be effectively enhanced by selecting the most suitable proportion.
It can be seen from the combination of application examples 4, 7 and 8 and the combination of table 1 that the graphene oxide, the unsaturated fatty acid and the conjugated diene are selected, so that the graphene oxide and the unsaturated fatty acid are combined to perform an acyl chlorination reaction, the compatibility of the modified graphene oxide in the oily auxiliary material is improved, the modified graphene oxide is more conveniently dispersed in the oily auxiliary material, and then the unsaturated fatty acid and the conjugated diene on the graphene oxide form the graphene oxide containing the cyclic unsaturated fatty acid, so that the dispersion performance of the graphene oxide is improved, and the overall stability of the modified graphene oxide is improved, so that the dispersion of the graphene oxide is more facilitated.
As can be seen from the combination of application example 4, application example 9 and application example 10 and the combination of table 1, the double modification is performed on the graphene oxide, so that the double modified graphene oxide is uniformly dispersed, and the improvement of the performance of the plate is facilitated.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. A method for preparing environment-friendly flame-retardant expandable polystyrene, which is characterized by comprising the following steps: s1, adding 110 parts by weight of pure water into a reaction kettle; adding the following water-based auxiliary materials and uniformly stirring: 0.06 to 0.08 weight part of dispersant A,0.0014 to 0.0018 weight part of reagent A and 0.001 to 0.0012 weight part of reagent B;
s2, adding 100 parts by weight of styrene; adding the following oily auxiliary materials and uniformly stirring: 0.25 to 0.55 weight part of initiator A,0.03 to 0.08 weight part of initiator B,0.2 to 0.5 weight part of initiator C,0.6 to 0.9 weight part of flame retardant, 0.2 to 0.6 weight part of plasticizer, 0.005 to 0.008 weight part of stabilizer and 0.1 to 0.2 weight part of nucleating agent;
s3, heating to 88-90 ℃ and reacting for 5-6 hours;
s4, adding 0.2 to 0.3 weight part of dispersant B, and then adding 0.5 to 1.2 weight parts of foaming agent;
s5, heating to 118-130 ℃ and reacting for 2.5-5 hours;
s6, cooling and discharging.
2. The method for preparing environment-friendly flame-retardant expandable polystyrene according to claim 1, wherein the initiator a is one or more of azobisisobutyronitrile, benzoyl peroxide and tert-butyl peroxy-2-ethyl hexyl carbonate.
3. The method for preparing environment-friendly flame-retardant expandable polystyrene according to claim 1, wherein the initiator B is one or more of dicumyl peroxide, bis (4-tert-butylcyclohexyl) peroxydicarbonate and hexadecyl ester.
4. The method for preparing environment-friendly flame-retardant expandable polystyrene according to claim 1, wherein the initiator C is one or more of tert-butyl peroxybenzoate, tert-butyl peroxyneodecanoate and tert-butyl peroxycarbonate-2-ethylhexyl.
5. The method for preparing environment-friendly flame-retardant expandable polystyrene according to claim 1, wherein the foaming agent is one or more of n-pentane, isopentane and neopentane.
6. The method for preparing environment-friendly flame-retardant expandable polystyrene according to claim 1, wherein the oily auxiliary material further comprises 0.5-1.5 parts by weight of reinforced modified composite powder, and the reinforced modified composite powder comprises modified graphene oxide, calcium metaborate and polyethylene glycol monomethyl ether.
7. The method for preparing environment-friendly flame-retardant expandable polystyrene according to claim 6, wherein said reinforced modified composite powder is prepared by the steps of: mixing and ball milling calcium metaborate and oleic acid mixed with polyethylene glycol monomethyl ether, then adding modified graphene oxide, and continuing mixing and ball milling, thereby enhancing the modified composite powder.
8. The method for preparing environment-friendly flame-retardant expandable polystyrene according to claim 7, wherein the modified graphene oxide is prepared from graphene oxide, unsaturated fatty acid and conjugated diene.
9. The method for preparing environment-friendly flame-retardant expandable polystyrene according to claim 8, wherein said modified graphene oxide is prepared by the steps of: s1, carrying out acyl chlorination reaction on graphene oxide and unsaturated fatty acid to obtain an intermediate product; s2, reacting the intermediate product with conjugated diene to generate final modified graphene oxide.
10. The method for preparing environment-friendly flame-retardant expandable polystyrene according to any one of claims 1 to 9, wherein said expandable polystyrene is used for preparing foam boards, which comprises the following preparation steps: the environment-friendly flame-retardant expandable polystyrene is subjected to pre-expansion, curing and forming processes to prepare the foam board.
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