CN104891835B - A kind of graft-modification method of fire-retardant flyash - Google Patents
A kind of graft-modification method of fire-retardant flyash Download PDFInfo
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- CN104891835B CN104891835B CN201510253924.7A CN201510253924A CN104891835B CN 104891835 B CN104891835 B CN 104891835B CN 201510253924 A CN201510253924 A CN 201510253924A CN 104891835 B CN104891835 B CN 104891835B
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- flyash
- weight
- retardant
- hours
- graft
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- 239000010881 fly ash Substances 0.000 title claims abstract description 100
- 239000003063 flame retardant Substances 0.000 title claims abstract description 41
- 238000002715 modification method Methods 0.000 title claims abstract description 23
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000839 emulsion Substances 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
- 239000010703 silicon Substances 0.000 claims abstract description 12
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052796 boron Inorganic materials 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 7
- WHHGLZMJPXIBIX-UHFFFAOYSA-N decabromodiphenyl ether Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1OC1=C(Br)C(Br)=C(Br)C(Br)=C1Br WHHGLZMJPXIBIX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 21
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 16
- 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 15
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 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 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000012190 activator Substances 0.000 claims description 10
- 230000029936 alkylation Effects 0.000 claims description 10
- 238000005804 alkylation reaction Methods 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 6
- MPPQGYCZBNURDG-UHFFFAOYSA-N 2-propionyl-6-dimethylaminonaphthalene Chemical compound C1=C(N(C)C)C=CC2=CC(C(=O)CC)=CC=C21 MPPQGYCZBNURDG-UHFFFAOYSA-N 0.000 claims description 5
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 5
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 5
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 239000004359 castor oil Substances 0.000 claims description 5
- 235000019438 castor oil Nutrition 0.000 claims description 5
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229960003540 oxyquinoline Drugs 0.000 claims description 5
- 229940068041 phytic acid Drugs 0.000 claims description 5
- 235000002949 phytic acid Nutrition 0.000 claims description 5
- 239000000467 phytic acid Substances 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- UMKARVFXJJITLN-UHFFFAOYSA-N lead;phosphorous acid Chemical compound [Pb].OP(O)O UMKARVFXJJITLN-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 12
- 238000006884 silylation reaction Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 2
- -1 flame-retardant compound Chemical class 0.000 abstract description 2
- 239000004567 concrete Substances 0.000 description 13
- 239000004568 cement Substances 0.000 description 12
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 11
- 239000010883 coal ash Substances 0.000 description 9
- 239000003245 coal Substances 0.000 description 8
- 239000011449 brick Substances 0.000 description 7
- 239000000292 calcium oxide Substances 0.000 description 6
- 235000012255 calcium oxide Nutrition 0.000 description 6
- 239000002689 soil Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000010440 gypsum Substances 0.000 description 5
- 229910052602 gypsum Inorganic materials 0.000 description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000002956 ash Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003818 cinder Substances 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003337 fertilizer Substances 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000002817 coal dust Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000004035 construction material Substances 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000003516 soil conditioner Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 1
- 241000876852 Scorias Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- HHZLLMMKYBCNMW-UHFFFAOYSA-N [P].[Mg].[Ca].[Si].C(CC(O)(C(=O)O)CC(=O)O)(=O)O Chemical compound [P].[Mg].[Ca].[Si].C(CC(O)(C(=O)O)CC(=O)O)(=O)O HHZLLMMKYBCNMW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- ZCILODAAHLISPY-UHFFFAOYSA-N biphenyl ether Natural products C1=C(CC=C)C(O)=CC(OC=2C(=CC(CC=C)=CC=2)O)=C1 ZCILODAAHLISPY-UHFFFAOYSA-N 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 125000001246 bromo group Chemical class Br* 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000010457 zeolite Substances 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
Landscapes
- Fireproofing Substances (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of graft-modification method of fire-retardant flyash, the present invention utilizes 3 aminopropyltriethoxywerene werenes, make the mix surface silylation obtained by flyash, then butyl methacrylate is grafted on to the silylation surface of compound, improve the stability of system, water-resistance and cohesive, flyash is mixed with silicon emulsion by the present invention with the siliceous filtrate after soaking with sodium hydroxide and tetraethyl orthosilicate, with high boron line borate, decabromodiphenyl oxide etc. is mixed to form highly effective flame-retardant compound, not only there is good mechanical performance, also improve anti-flammability and security.
Description
Technical field
The present invention relates to a kind of method that flyash recycles, more particularly to a kind of graft modification side of fire-retardant flyash
Method.
Background technology
Flyash, is the fine ash that catching is got off from the flue gas after coal combustion, and flyash is the main of coal-burning power plant's discharge
Solid waste.The main oxides of power plants flyash form:SiO2、Al2O3、FeO、Fe2O3、CaO、TiO2Deng.Powder
Coal ash is one of larger industrial residue of the current discharge capacity in China, and with the development of power industry, the flyash of coal-burning power plant discharges
Amount increases year by year.Substantial amounts of flyash is untreated, will produce airborne dust, pollutes air;River can be caused to become silted up if being discharged into water system
Plug, and toxic chemical substance therein can also damage to human body and biology.Other flyash can be as the blending of concrete
Material.
China is a big coal country, using coal as power generation substantially fuel.The energy industry stable development in China, generate electricity
Ability annual growth is 7.3%, and power industry develops rapidly, brings sharply increasing for flyash discharge capacity, Hazards in Power Plant
The flyash total amount discharged every year increases year by year, and nineteen ninety-five flyash discharge capacity is up to 1.25 hundred million tons, 2000 about 1.5 hundred million
Ton, was up to 300,000,000 tons, the development of the national economy and ecological environment to China cause huge pressure by 2010.On the other hand,
China is the limited country of a per capita resource reserve again, the comprehensive utilization of flyash, turns waste into wealth, turns bane into boon,
It is to solve China's power generation environmental pollution, resource shortage as an important techno-economic policy in economic construction of China
Between contradiction important means, and power generation faces one of task of solution.By exploitation, flyash is being built work, built
The all departments such as material, water conservancy are widely used.
In the 1970s, exhaustion of worldwide energy crisis, environmental pollution and mineral resources etc. consumingly excites
The research and development of utilization of fly ash, international flyash meeting is repeatedly held, research work is increasingly deep, and application aspect also has
Significant progress.Flyash turns into noticeable aboundresources, cheap, the new construction brought good to and remove all evil on international market
The raw material of material raw material and chemical products, is favored by people.Research work to flyash is mostly turned to by theoretical research should
With research, important Resource analysis and utilization are particularly.The product produced using flyash is being continuously increased, and technology exists
Constantly update.Domestic and international total utilization of PCA work, there occurs great change, is mainly shown as compared with the past:Powder
The guiding theory that coal ash is administered is the comprehensive regulation, recycling from past simple environment angle change;Flyash integrates
The approach utilized is outside the application of past roadbed, embankment, concrete admixture, soil remediation etc., to develop into water
Mud raw material, cement mixture, Large Hydro-Junction engineering, pump concrete, mass concrete product, advanced filler etc. are advanced
Change utilization ways.
Flyash be coal dust formed after high-temp combustion one kind like pozzolana mixed material.It is the generating of burning coal
Factory wears into coal less than 100 microns of coal dust, and spray into burner hearth with preheated air is burnt into suspended state, and generation is contaminated with largely not
The high-temperature flue gas of combustion things, flyash is just obtained through dust collect plant trapping.The chemical composition of flyash is similar to clayey, mainly
Composition is silica, alundum (Al2O3), di-iron trioxide, calcium oxide and uncompleted burned carbon.Flyash is mainly used to produce fine coal
Ash concrete, flyash brick, fly ash silicate building block, powder ash air-entrained concrete and other construction materials, also act as agricultural
Fertilizer and soil conditioner, reclaim the raw material of industry and make environmentally conscious materialses.Flyash answering in cement industry and concrete works
With:Flyash replaces raw clay production cement, made of Portland clinker and flyash addition proper amount of gypsum are levigate
Hydraulic binder materials, cement industry can utilize unburnt carbon therein using flyash dispensing;Flyash makees cement mixture;Powder
Coal ash produces low-temperature synthesizing water mud, and production principle is that the steam curing of batch elder generation is generated into hyrate, then through dehydration and low temperature
Solid phase reaction forms cement minerals;Flyash makes clinker-free cement, including lime fly ash cement and pure fly ash cement, stone
Grey pulverized fuel ash cement is the quick lime or calcium hydroxide and a small amount of gypsum combined grinding that dry flyash is mixed to 10%-30%, or
Remixed after levigate respectively uniformly made of hydraulic cementing materials;Flyash makees the admixture of mortar or concrete, in coagulation
Adding coal ash replaces part of cement or fine aggregate in soil, can not only reduce cost, and can improve the workability of concrete, carry
High waterproof, gas, Sulphate-resistant property and chemistry-resistant characteristic, the resistance to elevated temperatures for reducing the heat of hydration, improving concrete,
Mitigate particle separation and bleed phenomenon, the contraction of reduction concrete and cracking and suppress stray electrical current to reinforcement in concrete
Corrosion.Application of the flyash in building product:Flyash brick is steamed, with fly ash in electric power plant and quick lime or other alkaline excitations
Agent is primary raw material, can also mix appropriate gypsum, and adds the aggregates such as a certain amount of cinder or water-granulated slag, by processing,
A kind of materials for wall formed after stirring, digestion, rolling, compressing, normal pressure or autoclave curing;Sintered coal ash
Brick, using flyash, clay and other industrial wastes as raw material, brick is made through Raw material processing, stirring, shaping, drying, roast;Steam
Pressure production foam powder coal ash insulating brick, using flyash as primary raw material, add a certain amount of lime and foaming agent, by dispensing,
A kind of novel insulating brick that stirring, burning injection forming and steam pressure form;Fly ash silicate building block, using flyash, lime, gypsum as
Binder materials, cinder, blast-furnace cinder etc. is aggregate, the materials for wall for adding water stirring, vibration moulding, steam curing to form;Fine coal
Ash aerated concrete, using flyash as raw material, quick lime, cement, gypsum and aluminium powder are added in right amount, add water stirring in slurry, injection
A kind of steam-cured porous light construction material formed of mould;Lytag, using flyash as primary raw material, mix a small amount of bond
Agent and solid fuel, blended, balling-up, high temperature roast and a kind of artificial lightweight aggregate made;Coal ash light heat insulation brick,
It is to be carried out dispensing with flyash, scoria, soft soil and wood chip and formed, has insulating efficiency high, refractoriness is done, and thermal conductivity is small, energy
Mitigate furnace wall thickness, shorten firing time, reduce fuel consumption, improve the thermal efficiency, reduce cost.Flyash make agricultural fertilizer and
Soil conditioner:Flyash has good physicochemical properties, can be widely used in transform rich clay, the raw-soil, acid soil and
Saline-alkali soil, the defects of its thin plate of acid is viscous is made up, contains battalion necessary to the crops such as a large amount of solubility in citric acid silicon-calcium-magnesium phosphorus in flyash
Element is supported, therefore agricultural fertilizer can be used as.Reclaim the raw material of industry:Reclaiming coal resource, using floatation in the flyash containing coal
Floating agent is added in grey pulp-water, then using air flotation technology, coal grain is adhered to bubble floating and is separated with lime-ash;Reclaim metal
Contain Fe in material flyash2O3、Al2O3And a large amount of rare metals;Cenosphere is sorted, cenosphere has quality small, high
Intensity, high temperature resistant and good insulating, it can be used for the ideal filler of plastics, for lightweight refracrory and thermal insulation material,
For petro chemical industry, for military industry field, tank brake.Make environment-friendly materials:Molecular sieve, flocculation can be manufactured using flyash
The environment-friendly materials such as agent and sorbing material;Flyash can also be used to handle fluoride waste, electroplating wastewater and the waste water of example containing heavy metal
And oily waste water, the Al contained in flyash2O3, CaO isoreactivity components, can with fluorine produce complex or production have flocculation to fluorine
The colloid ion of effect, also containing zeolite, mullite, carbon granule and silica gel etc., there is inorganic ions commutativity and adsorption bleaching
Effect.
The content of the invention
The object of the invention just there is provided a kind of graft-modification method of fire-retardant flyash.
The present invention is achieved by the following technical solutions：
A kind of graft-modification method of fire-retardant flyash, it is characterised in that comprise the following steps：
（1）Flyash is crushed, 200-300 mesh sieves is crossed, is mixed with the aqueous solution of its weight 3-5% activator, in 70-
Insulated and stirred 2-3 hours at 80 DEG C, drying are removed water, and 1-2 hours are calcined at 800-900 DEG C, normal temperature is cooled to, is added to concentration
In 10-16% sodium hydrate aqueous solution, the heat-insulation soaking 3-5 hours at 50-60 DEG C, filtering, filter residue and filtrate are obtained, by filter residue
Washing, drying, obtains flyash dry powder；
（2）The PH for adjusting above-mentioned filtrate is 6-7, adds its weight 7-10% tetraethyl orthosilicate, and rise temperature is 70-76
DEG C, batch mixing weight 0.1-0.2% castor oil polyoxyethylene ether is added, insulated and stirred 10-20 minutes, obtains silicon emulsion；
（3）It is 10-12 to take weight ratio:0.1-0.2:3-5：0.01-0.02 high boron line borate, 8-hydroxyquinoline, ten bromines
Biphenyl Ether, dibasic lead phosphite mixing, ball milling, obtain flame retardant；
（4）Above-mentioned flyash dry powder, flame retardant, silicon emulsion are mixed, 500-600 revs/min of stirring 10-20 minute, often
The lower ageing of temperature stands 2-3 hours, press filtration, vacuum drying, ball milling, adds ball milling material weight 50-60% 3- aminopropyls three
Ethoxysilane, insulated and stirred 10-20 hours at 20-30 DEG C, obtain alkylation batch mixing；
（5）Polyvinyl alcohol is taken, is added in 20-30 times of water of its weight, stirs, adds abovementioned alkyl batch mixing, is adjusted
It is 60-70 DEG C to save temperature, under the protection of nitrogen, sequentially adds butyl methacrylate, divinylbenzene, azodiisobutyronitrile,
Stirring reaction 6-7 hours, reaction are washed successively after terminating with ethanol, deionized water, press filtration, vacuum drying, are produced.
A kind of graft-modification method of fire-retardant flyash, step（4）Described in flyash dry powder, the weight of flame retardant
Than for 100: 6-10.
A kind of graft-modification method of fire-retardant flyash, step（5）Described in polyvinyl alcohol, butyl methacrylate,
Divinylbenzene, the weight ratio of azodiisobutyronitrile and alkylation batch mixing are 3-4：17-20：1-2：0.1-0.14：16-30.
A kind of graft-modification method of fire-retardant flyash, step（1）Described in the aqueous solution of activator be by following heavy
Measure the raw material mixing composition of part：Prodan 7-10 parts by weight, sodium chloride 2-3 parts by weight, phytic acid 0.2-0.4 weight
Part, the parts by weight of deionized water 100.
It is an advantage of the invention that：
The present invention utilizes APTES, makes the mix surface silylation obtained by flyash,
Then butyl methacrylate is grafted on to the silylation surface of compound, improve the stability of system, water-resistance and viscous
Conjunction property, flyash is mixed with silicon emulsion by the present invention with the siliceous filtrate after soaking with sodium hydroxide and tetraethyl orthosilicate, with height
Boron line borate, decabromodiphenyl oxide etc. are mixed to form highly effective flame-retardant compound, not only with good mechanical performance, also improve resistance
Combustion property and security.
Embodiment
The present invention is described in further detail with reference to embodiment：
Embodiment 1：
A kind of graft-modification method of fire-retardant flyash, it is characterised in that comprise the following steps：
（1）Flyash is crushed, 200 mesh sieves is crossed, mixes with the aqueous solution of the activator of its weight 4%, be incubated at 70 DEG C
Stirring 2 hours, drying remove water, and are calcined 2 hours at 900 DEG C, are cooled to normal temperature, are added to the sodium hydrate aqueous solution of concentration 16%
In, heat-insulation soaking 3 hours at 60 DEG C, filtering, filter residue and filtrate are obtained, filter residue is washed, dried, obtain flyash dry powder；
（2）The PH for adjusting above-mentioned filtrate is 7, adds its weight 7-10% tetraethyl orthosilicate, rise temperature is 76 DEG C, is added
Enter the castor oil polyoxyethylene ether of batch mixing weight 0.2%, insulated and stirred 20 minutes, obtain silicon emulsion；
（3）It is 12 to take weight ratio:0.2:3：0.02 high boron line borate, 8-hydroxyquinoline, decabromodiphenyl oxide, dibasic are sub-
Lead phosphate mixes, and ball milling, obtains flame retardant；
（4）Above-mentioned flyash dry powder, flame retardant, silicon emulsion are mixed, 500 revs/min are stirred 17 minutes, are aged under normal temperature
2 hours are stood, press filtration, vacuum drying, ball milling, the APTES of addition ball milling material weight 50%, 20
Insulated and stirred 18 hours at DEG C, obtain alkylation batch mixing；
（5）Polyvinyl alcohol is taken, is added in 26 times of water of its weight, stirs, adds abovementioned alkyl batch mixing, regulation temperature
Spend for 70 DEG C, under the protection of nitrogen, sequentially add butyl methacrylate, divinylbenzene, azodiisobutyronitrile, stirring reaction
6 hours, reaction was washed successively after terminating with ethanol, deionized water, press filtration, vacuum drying, was produced.
A kind of graft-modification method of fire-retardant flyash, step（4）Described in flyash dry powder, the weight of flame retardant
Than for 100: 7.
A kind of graft-modification method of fire-retardant flyash, step（4）Described in polyvinyl alcohol, butyl methacrylate,
The weight ratio of divinylbenzene, azodiisobutyronitrile and alkylation batch mixing is 3：20：1：0.14：30.
A kind of graft-modification method of fire-retardant flyash, step（1）Described in the aqueous solution of activator be by following heavy
Measure the raw material mixing composition of part：The parts by weight of prodan 9, the parts by weight of sodium chloride 2, the parts by weight of phytic acid 0.26, go from
The sub- parts by weight of water 100.
Embodiment 2
A kind of graft-modification method of fire-retardant flyash, it is characterised in that comprise the following steps：
（1）Flyash is crushed, 300 mesh sieves is crossed, mixes with the aqueous solution of the activator of its weight 4%, be incubated at 80 DEG C
Stirring 2 hours, drying remove water, and are calcined 1 hour at 900 DEG C, are cooled to normal temperature, are added to the sodium hydrate aqueous solution of concentration 10%
In, heat-insulation soaking 3 hours at 60 DEG C, filtering, filter residue and filtrate are obtained, filter residue is washed, dried, obtain flyash dry powder；
（2）The PH for adjusting above-mentioned filtrate is 6, adds the tetraethyl orthosilicate of its weight 10%, and rise temperature is 70 DEG C, is added
The castor oil polyoxyethylene ether of batch mixing weight 0.17%, insulated and stirred 18 minutes, obtains silicon emulsion；
（3）Weight is taken than 12:0.2:3：0.01 high boron line borate, 8-hydroxyquinoline, decabromodiphenyl oxide, dibasic phosphorous
Lead plumbate mixes, and ball milling, obtains flame retardant；
（4）Above-mentioned flyash dry powder, flame retardant, silicon emulsion are mixed, 600 revs/min are stirred 20 minutes, are aged under normal temperature
2 hours are stood, press filtration, vacuum drying, ball milling, the APTES of addition ball milling material weight 60%, 27
Insulated and stirred 10 hours at DEG C, obtain alkylation batch mixing；
（5）Polyvinyl alcohol is taken, is added in 28 times of water of its weight, stirs, adds abovementioned alkyl batch mixing, regulation temperature
Spend for 70 DEG C, under the protection of nitrogen, sequentially add butyl methacrylate, divinylbenzene, azodiisobutyronitrile, stirring reaction
6 hours, reaction was washed successively after terminating with ethanol, deionized water, press filtration, vacuum drying, was produced.
A kind of graft-modification method of fire-retardant flyash, step（4）Described in flyash dry powder, the weight of flame retardant
Than for 10: 1.
A kind of graft-modification method of fire-retardant flyash, step（5）Described in polyvinyl alcohol, butyl methacrylate,
The weight ratio of divinylbenzene, azodiisobutyronitrile and alkylation batch mixing is 3：19：1：0.12：21.
A kind of graft-modification method of fire-retardant flyash, step（1）Described in the aqueous solution of activator be by following heavy
Measure the raw material mixing composition of part：The parts by weight of prodan 9, the parts by weight of sodium chloride 3, the parts by weight of phytic acid 0.4, deionization
The parts by weight of water 100.
Embodiment 3
A kind of graft-modification method of fire-retardant flyash, comprises the following steps：
（1）Flyash is crushed, 300 mesh sieves is crossed, mixes with the aqueous solution of the activator of its weight 3%, be incubated at 80 DEG C
Stirring 2 hours, drying remove water, and are calcined 1 hour at 900 DEG C, are cooled to normal temperature, are added to the sodium hydrate aqueous solution of concentration 16%
In, heat-insulation soaking 3 hours at 60 DEG C, filtering, filter residue and filtrate are obtained, filter residue is washed, dried, obtain flyash dry powder；
（2）The PH for adjusting above-mentioned filtrate is 6, adds its weight 7-10% tetraethyl orthosilicate, rise temperature is 76 DEG C, is added
Enter the castor oil polyoxyethylene ether of batch mixing weight 0.17%, insulated and stirred 20 minutes, obtain silicon emulsion；
（3）It is 10 to take weight ratio:0.17:3：0.01 high boron line borate, 8-hydroxyquinoline, decabromodiphenyl oxide, dibasic
Lead phosphite mixes, and ball milling, obtains flame retardant；
（4）Above-mentioned flyash dry powder, flame retardant, silicon emulsion are mixed, 560 revs/min are stirred 13 minutes, are aged under normal temperature
2 hours are stood, press filtration, vacuum drying, ball milling, the APTES of addition ball milling material weight 51%, 28
Insulated and stirred 18 hours at DEG C, obtain alkylation batch mixing；
（5）Polyvinyl alcohol is taken, is added in 24 times of water of its weight, stirs, adds abovementioned alkyl batch mixing, regulation temperature
Spend for 68 DEG C, under the protection of nitrogen, sequentially add butyl methacrylate, divinylbenzene, azodiisobutyronitrile, stirring reaction
6 hours, reaction was washed successively after terminating with ethanol, deionized water, press filtration, vacuum drying, was produced.
A kind of graft-modification method of fire-retardant flyash, step（4）Described in flyash dry powder, the weight of flame retardant
Than for 100: 9.
A kind of graft-modification method of fire-retardant flyash, step（5）Described in polyvinyl alcohol, butyl methacrylate,
The weight ratio of divinylbenzene, azodiisobutyronitrile and alkylation batch mixing is 3：20：1：0.1：17.
A kind of graft-modification method of fire-retardant flyash, step（1）Described in the aqueous solution of activator be by following heavy
Measure the raw material mixing composition of part：The parts by weight of prodan 9, the parts by weight of sodium chloride 2, the parts by weight of phytic acid 0.2, deionization
The parts by weight of water 100.
Claims (3)
1. a kind of graft-modification method of fire-retardant flyash, it is characterised in that comprise the following steps：
(1) flyash is crushed, crosses 200-300 mesh sieves, mixed with the aqueous solution of its weight 3-5% activator, at 70-80 DEG C
Lower insulated and stirred 2-3 hours, drying are removed water, and 1-2 hours are calcined at 800-900 DEG C, normal temperature is cooled to, is added to concentration 10-
In 16% sodium hydrate aqueous solution, the heat-insulation soaking 3-5 hours at 50-60 DEG C, filtering, filter residue and filtrate are obtained, by filter residue water
Wash, dry, obtain flyash dry powder；
(2) pH for adjusting above-mentioned filtrate is 6-7, adds its weight 7-10% tetraethyl orthosilicate, and rise temperature is 70-76 DEG C,
Batch mixing weight 0.1-0.2% castor oil polyoxyethylene ether is added, insulated and stirred 10-20 minutes, obtains silicon emulsion；
(3) it is 10-12 to take weight ratio:0.1-0.2:3-5：0.01-0.02 high boron line borate, 8-hydroxyquinoline, decabromodiphenyl
Ether, dibasic lead phosphite mixing, ball milling, obtain flame retardant；
(4) above-mentioned flyash dry powder, flame retardant, silicon emulsion are mixed, 500-600 revs/min of stirring 10-20 minute, under normal temperature
Ageing stands 2-3 hours, press filtration, vacuum drying, ball milling, adds the ball milling material weight 50-60% second of 3- aminopropyls three
TMOS, insulated and stirred 10-20 hours at 20-30 DEG C, obtain alkylation batch mixing；
(5) polyvinyl alcohol is taken, is added in 20-30 times of water of its weight, stirs, adds abovementioned alkyl batch mixing, regulation temperature
Spend for 60-70 DEG C, under the protection of nitrogen, sequentially add butyl methacrylate, divinylbenzene, azodiisobutyronitrile, stir
React 6-7 hours, reaction is washed successively after terminating with ethanol, deionized water, press filtration, vacuum drying, is produced；
The aqueous solution of activator described in step (1) is made up of the raw material mixing of following weight parts：Prodan 7-10
Parts by weight, sodium chloride 2-3 parts by weight, phytic acid 0.2-0.4 parts by weight, the parts by weight of deionized water 100.
2. the graft-modification method of a kind of fire-retardant flyash according to claim 1, it is characterised in that described in step (4)
Flyash dry powder, flame retardant weight ratio be 100:6-10.
3. the graft-modification method of a kind of fire-retardant flyash according to claim 1, it is characterised in that described in step (5)
Polyvinyl alcohol, butyl methacrylate, divinylbenzene, azodiisobutyronitrile with alkylation batch mixing weight ratio be 3-4：17-
20：1-2：0.1-0.14：16-30.
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Inventor after: Li Yanheng Inventor after: Sun Yuzhuang Inventor after: Zhang Haidao Inventor after: Wang Jinxi Inventor after: Zhao Bin Inventor after: Lin Mingyue Inventor after: Jin Kankun Inventor after: Meng Zhiqiang Inventor before: Sun Yuzhuang Inventor before: Zhang Haidao Inventor before: Wang Jinxi Inventor before: Zhao Bin Inventor before: Lin Mingyue Inventor before: Jin Kankun Inventor before: Meng Zhiqiang |
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