CN109134784A - It is a kind of to promote solidifying high-early strength polyocarboxy acid superplasticiser and preparation method thereof - Google Patents
It is a kind of to promote solidifying high-early strength polyocarboxy acid superplasticiser and preparation method thereof Download PDFInfo
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- CN109134784A CN109134784A CN201810844151.3A CN201810844151A CN109134784A CN 109134784 A CN109134784 A CN 109134784A CN 201810844151 A CN201810844151 A CN 201810844151A CN 109134784 A CN109134784 A CN 109134784A
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- Prior art keywords
- parts
- feed liquid
- acid
- polyoxyethylene ether
- deionized water
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- 239000002253 acid Substances 0.000 title claims abstract description 93
- 239000008030 superplasticizer Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 158
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 72
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 72
- 239000000178 monomer Substances 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- 150000002148 esters Chemical class 0.000 claims abstract description 58
- 239000008367 deionised water Substances 0.000 claims abstract description 54
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 54
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 239000003999 initiator Substances 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 20
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 150000001408 amides Chemical class 0.000 claims abstract description 16
- 238000009413 insulation Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 32
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 25
- 239000011790 ferrous sulphate Substances 0.000 claims description 25
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 25
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 25
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 24
- -1 fumaric acid triethanolamine ester Chemical class 0.000 claims description 19
- 238000010792 warming Methods 0.000 claims description 15
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 13
- 229940043237 diethanolamine Drugs 0.000 claims description 11
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 10
- AFNWOEJOULWFIS-BTJKTKAUSA-N (z)-4-hydroxy-4-oxobut-2-enoate;tris(2-hydroxyethyl)azanium Chemical compound OC(=O)\C=C/C(O)=O.OCCN(CCO)CCO AFNWOEJOULWFIS-BTJKTKAUSA-N 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 8
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims description 6
- 150000007513 acids Chemical class 0.000 claims description 6
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 5
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 4
- 230000001737 promoting effect Effects 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- KMQVOGRHZHPXJT-UHFFFAOYSA-N C(C)O.C(C)O.C(C(=C)C)(=O)O Chemical compound C(C)O.C(C)O.C(C(=C)C)(=O)O KMQVOGRHZHPXJT-UHFFFAOYSA-N 0.000 claims description 3
- XIZXAROKMGJFNB-UHFFFAOYSA-N C(C=C)(=O)O.C(C)O.C(C)O Chemical compound C(C=C)(=O)O.C(C)O.C(C)O XIZXAROKMGJFNB-UHFFFAOYSA-N 0.000 claims description 3
- NDKPYWBMBAPIOV-UAIGNFCESA-N C(\C=C/C(=O)O)(=O)O.C(C)O.C(C)O Chemical compound C(\C=C/C(=O)O)(=O)O.C(C)O.C(C)O NDKPYWBMBAPIOV-UAIGNFCESA-N 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 3
- NDKPYWBMBAPIOV-SEPHDYHBSA-N C(C)O.C(\C=C\C(=O)O)(=O)O.C(C)O Chemical compound C(C)O.C(\C=C\C(=O)O)(=O)O.C(C)O NDKPYWBMBAPIOV-SEPHDYHBSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000001530 fumaric acid Substances 0.000 claims description 2
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 2
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims 2
- BKOOMYPCSUNDGP-UHFFFAOYSA-N 2-methylbut-2-ene Chemical group CC=C(C)C BKOOMYPCSUNDGP-UHFFFAOYSA-N 0.000 claims 1
- YICILWNDMQTUIY-UHFFFAOYSA-N 2-methylidenepentanamide Chemical compound CCCC(=C)C(N)=O YICILWNDMQTUIY-UHFFFAOYSA-N 0.000 claims 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Natural products OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 1
- 229930003268 Vitamin C Natural products 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 229940031098 ethanolamine Drugs 0.000 claims 1
- 229940087646 methanolamine Drugs 0.000 claims 1
- HZAXFHJVJLSVMW-UHFFFAOYSA-N monoethanolamine hydrochloride Natural products NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 235000019260 propionic acid Nutrition 0.000 claims 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims 1
- 125000003396 thiol group Chemical group [H]S* 0.000 claims 1
- 235000019154 vitamin C Nutrition 0.000 claims 1
- 239000011718 vitamin C Substances 0.000 claims 1
- 239000004567 concrete Substances 0.000 abstract description 36
- 230000001112 coagulating effect Effects 0.000 abstract description 4
- 239000004568 cement Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- 239000002270 dispersing agent Substances 0.000 description 12
- 238000013019 agitation Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229920005646 polycarboxylate Polymers 0.000 description 5
- PCHPORCSPXIHLZ-UHFFFAOYSA-N diphenhydramine hydrochloride Chemical class [Cl-].C=1C=CC=CC=1C(OCC[NH+](C)C)C1=CC=CC=C1 PCHPORCSPXIHLZ-UHFFFAOYSA-N 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 230000007306 turnover Effects 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 2
- SGZOTQPYJLDQRT-UHFFFAOYSA-N 2-ethenylbenzenesulfonic acid;sodium Chemical compound [Na].OS(=O)(=O)C1=CC=CC=C1C=C SGZOTQPYJLDQRT-UHFFFAOYSA-N 0.000 description 2
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920000151 polyglycol Polymers 0.000 description 2
- 239000010695 polyglycol Substances 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 1
- DPZFPPWWSNNMPI-UHFFFAOYSA-N [S]C=C Chemical compound [S]C=C DPZFPPWWSNNMPI-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- OVHHHVAVHBHXAK-UHFFFAOYSA-N n,n-diethylprop-2-enamide Chemical compound CCN(CC)C(=O)C=C OVHHHVAVHBHXAK-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012712 reversible addition−fragmentation chain-transfer polymerization Methods 0.000 description 1
- 239000011376 self-consolidating concrete Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
It is a kind of to promote solidifying high-early strength polyocarboxy acid superplasticiser and preparation method thereof, polycarboxylic acid super-plasticizer is made of the raw material of following mass fractions: 70~80 parts of polyoxyethylene ether polymeric monomer, 1~1.5 part of reducing agent, aqueous initiator, and 40~50 parts of deionized water, A feed liquid, B feed liquid；A feed liquid is mixed by 7~9 parts of acrylic acid, i.e. unsaturated 0.1~2 part of the alkanolamine ester of the solidifying early strong monomer of rush, 0.1~1 part of unsaturated amides, 15~25 parts of deionized water；B feed liquid is mixed by 0.08~0.15 part of reducing agent Y, 0.3~0.5 part of chain-transferring agent, 18~28 parts of deionized water.Preparation method: polyoxyethylene ether polymeric monomer, reducing agent and deionized water are put into reaction kettle, are heated up, stirring；Aqueous initiator is added in reaction kettle, A feed liquid and B feed liquid is added dropwise, after being added dropwise to complete, insulation reaction is down to room temperature, and liquid alkaline is added and adjusts pH value to 7.The present invention effectively increases early strength of concrete, shortens concrete coagulating time.
Description
Technical field
It is specifically a kind of to promote to coagulate the present invention relates to a kind of concrete admixture more particularly to a kind of polycarboxylic acid super-plasticizer
High-early strength polyocarboxy acid superplasticiser belongs to building material technical field.The invention further relates to a kind of systems of polycarboxylic acid super-plasticizer
Preparation Method, specifically a kind of preparation method for promoting solidifying high-early strength polyocarboxy acid superplasticiser.
Background technique
Prefabricated components are because its speed of application is fast, save manpower, improves construction site environment, good in economic efficiency characteristic gradually
It is widely applied commercially available.Quick template turnover is often required that in prefabricated components production, this often just needs coagulation
Soil has very high early strength.Usual way is: increasing cement consumption, mixes early strong inorganic salts, improve steam curing temperature.Increase water
Mud dosage bring is the increase of production cost, and it is very high and can bring under later strength to mix volume that inorganic salts usually require
Drop improves temperature and needs higher energy consumption.People begin to focus on the angle from dispersing agent to promote early strength of concrete.
The present invention is synthesized by using the long side chain of high component, can effectively facilitate cement early hydration, is generated more fine and close
With tiny hydrated product.Unsaturated hydramine is introduced in main chain, hydramine can be released because the alkaline environment of cement hydrolyzes,
It can further speed up aquation and play the role of condensing catalyst, while part carboxyl can also be protected to play holding slump-loss
Effect.Main chain is grafted partial amides group, because of the presence of N, it is strong to obtain early stage that early hydration can be promoted effect
Degree.Because what is do not introduced is all organo-functional group, it will not influence hydrated product mine and mutually change, under later strength is not in
The case where drop.
Inventor retrieves following Patents documents: CN101066853 discloses a kind of polyethers ultra early-strength coagulation
Native super plasticizer, is prepared using following steps: 1) water-based free radical copolyreaction: by 84~94% monomer a, 5%~15% is single
Free radicals copolymerization reaction occurs in an aqueous medium for body b and 1~3% monomer c；2) neutralization reaction: after copolyreaction, altogether
The alkoxy organic amine d as shown in general formula (5) or general formula (6) is added in polymers and carries out neutralization reaction, by the pH value tune of copolymer
Whole is 6.0~7.5.CN101085701 discloses a kind of super plasticizer for prefabricated components concrete pumping, by monomer a, list
The monomer d free radicals copolymerization reaction of body b, monomer c and modification are made, and the monomer d of the modification is by monomer d and Nano-meter SiO_22Reaction
It is made；The viscosity average molecular weigh of the super plasticizer is controlled 30000~80000.CN101357834 discloses a kind of early-strength
Polycarboxylic acid super-plasticizer, it be by four kinds of monomers in 60 DEG C~95 DEG C aqueous solutions, radical initiator and chain-transferring agent exist
Under conditions of be copolymerized and obtain.New polymerized monomer is introduced on polymer molecular chain, forms new polymer molecular structure, to mention
The water-reducing rate and early stage enhancing ability of higher polycarboxylic acid super plasticizer.CN107602773A discloses a kind of for the poly- of oil-well cement
Carboxylic dispersants and preparation method thereof, the polycarboxylate dispersant are with acrylic acid, n-vinyl pyrrolidone, itaconic acid, 2- third
Acrylamide base -2- methyl propane sulfonic acid, sodium vinyl sulfonate, vinylbenzenesulfonic acid sodium and allyl polyglycol are being total to for monomer
Polymers；The weight average molecular weight of allyl polyglycol is 300~2400；It is the matter of acrylic acid in terms of 100% by the gross mass of monomer
Measuring percentage is 0.5%~20%, and the mass percent of n-vinyl pyrrolidone is 0.5%~15%, the quality of itaconic acid
Percentage is that the mass percent of 0.5%~10%, 2- acrylamide-2-methylpro panesulfonic acid is 5%~60%, vinyl sulphur
The mass percent of sour sodium is 0.5%~30%, and the mass percent of vinylbenzenesulfonic acid sodium is 0.5%~30%, allyl
The mass percent of polyethylene glycol is 20%~70%；The weight average molecular weight of polycarboxylate dispersant is 5000~250000.
CN103406067A discloses a kind of polycarboxylate dispersant and the preparation method and application thereof.The polycarboxylate dispersant by 1.0~
3.0 parts by weight contain the unsaturated monomer of carboxyl, the sulfonic unsaturated monomer of 1.1~2.2 parts by weight and 0.6~1.2 weight
Part other free-radical polymerised unsaturated base monomers, 25~35 parts by weight water, 0.11~0.22 parts by weight initiator,
Free radical polymerization occurs under the conditions of 0.03~0.06 parts by weight chain-transferring agent and 1.5~4.0 parts by weight alkali compounds are existing
Reaction obtains.CN106519151A discloses amphipathic poly-carboxylic-acid cement dispersant and preparation method thereof.The amphipathic carboxylic
Sour water cement dispersant is a kind of dispersion liquid of polycarboxylic acids particle with vermiform micromorphology；It includes amphipathic carboxylic that it, which is formed,
Sour nanoparticle and water；The weight average molecular weight of the amphipathic carboxylic acid particle is 15000~40000, and it is poly- which employs RAFT
Conjunction method, but RAFT polymerization is with high costs, chain-transferring agent is more difficult to buy.It has difficulties in industrial practical application.
United States Patent 4792360 discloses the method by introducing styrene sulfonic acid to make amphipathic carboxylic acid
Dispersing agent.But the price of styrene sulfonic acid is very high, has equally existed and has been difficult to the problem of promoting.US Patent
5158996 disclose the method by using acetone as solvent synthesis amphoteric dispersant, but can be made to environment using solvent
It must also be removed by distillation at pollution, and in subsequent use, increased costs.
The above technology shortens coagulation for how to enable polycarboxylic acid super-plasticizer effectively improve early strength of concrete
Native setting time does not provide specific guidance program.
Summary of the invention
Promote solidifying high-early strength polyocarboxy acid superplasticiser, the polycarboxylic acids the technical problem to be solved by the invention is to provide a kind of
Super plasticizer can effectively improve early strength of concrete, shorten concrete coagulating time.
For this purpose, another technical problem to be solved by this invention is to provide, a kind of to promote solidifying early-strength polycarboxylic acids super plasticized
The preparation method of agent.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
It is a kind of to promote solidifying high-early strength polyocarboxy acid superplasticiser, its technical solution is that it is by the raw material system of following mass fractions
At: 70~80 parts of (unsaturation) polyoxyethylene ether polymeric monomer, 1~1.5 part of reducing agent X, aqueous initiator, deionized water 40~
50 parts, A feed liquid, B feed liquid.Above-mentioned A feed liquid is unsaturated alkanolamine ester 0.1~2 by 7~9 parts of acrylic acid, the solidifying early strong monomer of rush
Part, 0.1~1 part of unsaturated amides, 15~25 parts of deionized water mix；B feed liquid is by 0.08~0.15 part of reducing agent Y, chain
0.3~0.5 part of transfer agent, 18~28 parts of deionized water mix.
Wherein, above-mentioned polyoxyethylene ether polymeric monomer (molecular weight can be 4000-10000) improves steric hindrance.Polyoxy
Vinethene polymeric monomer be methyl allyl polyoxyethylene ether, allyl polyethenoxy ether, isoamyl alcohol polyoxyethylene ether (TPEG),
One of isobutene alcohol polyoxyethylene ether；Unsaturated alkanolamine ester be maleic acid triethanolamine dibasic acid esters, maleic acid diethanol amine ester,
Maleic acid alkanolamine ester, trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester, methacrylic acid diethanol amine ester, methacrylic acid list alkanolamine ester,
Acrylic acid diethanol amine ester, acrylic acid list alkanolamine ester, fumaric acid triethanolamine ester, fumaric acid diethanol amine ester, fumaric acid list second
(any quality proportioning group is pressed in either two kinds of combination or two or more combinations when combination at least one of alkanolamine ester
It closes)；Unsaturated amides are acrylamide, Methacrylamide, n-isopropyl acrylamide, methylene-bisacrylamide, N, N-
Dimethacrylamide, N, at least one in N- acrylamide (N, N- diethyl -2- acrylamide), 2- acrylamide
Kind of (either two kinds of combination or two or more combinations are combined by any quality proportioning when combination)；Aqueous initiator is double
One of oxygen water, persulfate, azo-bis-isobutyrate hydrochloride or any two kinds of combinations by any quality proportioning；Reduction
The mass ratio of agent Y and reducing agent X are 10~11:1.
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality
Proportion by 70~80 parts of polyoxyethylene ether polymeric monomer, reducing agent X and 40~50 parts of deionized waters investment reaction kettle (500ml's
Three-necked flask with magnetic agitation) in, 40~50 DEG C are warming up to, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2.
Aqueous initiator is added in reaction kettle, then using constant flow pump starts that A feed liquid and B feed liquid are added dropwise simultaneously, A feed liquid is small 2.5~3
When be added dropwise to complete, B feed liquid was added dropwise to complete at 3~3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5~2 hours,
Resulting product is finally down to room temperature, liquid alkaline is added and adjusts pH value to 7 to get the solidifying high-early strength polyocarboxy acid superplasticiser of rush.
In above-mentioned technical proposal, currently preferred technical solution be can be, and the reducing agent X is ferrous sulfate, also
Former agent Y is L-AA, and the mass ratio of reducing agent Y and reducing agent X are 10:1.Above-mentioned chain-transferring agent is mercaptopropionic acid.
In above-mentioned technical proposal, it is super that currently preferred technical solution is also possible that the rush coagulates early-strength polycarboxylic acids
Plasticiser is made of the raw material of following mass fractions: polyoxyethylene ether polymeric monomer i.e. 72 parts of isoamyl alcohol polyoxyethylene ether,
0.009 part of reducing agent ferrous sulfate, 1.2 parts of aqueous initiator, that is, hydrogen peroxide, 45 parts of deionized water, A feed liquid, B feed liquid；Above-mentioned
A feed liquid is by 8.6 parts of acrylic acid, unsaturated alkanolamine ester, that is, 0.4 part of trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester, unsaturated amides, that is, propylene
0.5 part of amide, 20 parts of deionized water mix；B feed liquid is by 0.09 part of reducing agent L-AA, chain-transferring agent, that is, sulfydryl third
0.3 part, 20 parts of deionized water of acid mixes.The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush includes as follows
Processing step: above-mentioned quality proportioning is 1. pressed by 0.009 part and 45 parts 72 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate deionizations
Water is put into reaction kettle, is warming up to 40 DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. being added in reaction kettle aqueous
1.2 parts of initiator, constant flow pump is then respectively adopted and starts that A feed liquid and B feed liquid are added dropwise simultaneously, A feed liquid was added dropwise to complete at 3 hours, B
Feed liquid was added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, was finally dropped resulting product
To room temperature, liquid alkaline is added and adjusts pH value to 7 to get the solidifying high-early strength polyocarboxy acid superplasticiser of rush.
In above-mentioned technical proposal, it is super that currently preferred technical solution is also possible that the rush coagulates early-strength polycarboxylic acids
Plasticiser is made of the raw material of following mass fractions: polyoxyethylene ether polymeric monomer i.e. 76 parts of isoamyl alcohol polyoxyethylene ether,
0.012 part of reducing agent ferrous sulfate, 1.5 parts of aqueous initiator, that is, hydrogen peroxide, 48 parts of deionized water, A feed liquid, B feed liquid；Above-mentioned
A feed liquid is by 9 parts of acrylic acid, 1 part of trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester, 0.2 part of Methacrylamide, 22 parts of deionized water mixing
It forms；B feed liquid is by 0.12 part of reducing agent L-AA, 0.32 part of chain-transferring agent, that is, mercaptopropionic acid, 25 parts of deionized water mixing
It forms.The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. matching by above-mentioned quality
Than being warming up to 42 in 0.012 part and 48 parts 76 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate deionized water investment reaction kettles
DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. 1.5 parts of aqueous initiator are added in reaction kettle, then adopt respectively
Being started that A feed liquid and B feed liquid are added dropwise simultaneously with constant flow pump, A feed liquid was added dropwise to complete at 3 hours, and B feed liquid was added dropwise to complete at 3.5 hours,
After all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, resulting product is finally down to room temperature, liquid alkaline is added and adjusts pH
Value promotees solidifying high-early strength polyocarboxy acid superplasticiser to 7.
Currently preferred technical solution is referring also to the following examples 3~5.
The present invention is synthesized by using the long side chain of high component, can effectively facilitate cement early hydration, is generated more fine and close
With tiny hydrated product.Unsaturated hydramine is introduced in main chain, hydramine can be released because the alkaline environment of cement hydrolyzes,
It can further speed up aquation and play the role of condensing catalyst, while part carboxyl can also be protected to play holding slump-loss
Effect.Main chain is grafted partial amides group, because of the presence of N, it is strong to obtain early stage that early hydration can be promoted effect
Degree.Because what is do not introduced is all organo-functional group, it will not influence hydrated product mine and mutually change, under later strength is not in
The case where drop.
Polycarboxylic acid super-plasticizer of the invention is related to polycarboxylate dispersant, by (methyl) acrylic acid, unsaturated alkanolamine ester,
Unsaturated amides, polyoxyethylene ether carry out free radical polymerization as monomer, and preparation promotees solidifying early strength water-reducing agent.It has high water reduction,
High holding capacity, and can effectively shorten concrete coagulating time, thus between reducing the prefabricated components quiet stopping time, such water-reducing agent energy
Accelerate template turnover, save the cost.Can effectively promote 1 day early strength of concrete does not reduce by 28 days intensity of concrete simultaneously,
Steam curing temperature can be reduced, stripping rate is accelerated, to save steam-cured energy consumption, while template turnover is improved, reduces building
Cost.
Detailed description of the invention
Fig. 1 is different sample concrete initial set time diagrams in test of the invention.
Specific embodiment
Embodiment 1: of the present invention to promote to coagulate high-early strength polyocarboxy acid superplasticiser to be by the raw material system of following mass fractions
At: polyoxyethylene ether polymeric monomer, that is, 72 parts of isoamyl alcohol polyoxyethylene ether (TPEG4000), reducing agent ferrous sulfate 0.009
Part, 1.2 parts of aqueous initiator, that is, hydrogen peroxide (30% mass percent concentration, hydrogen peroxide 30%), 45 parts of deionized water, A material
Liquid, B feed liquid.Above-mentioned A feed liquid by 8.6 parts of acrylic acid, unsaturated alkanolamine ester, that is, 0.4 part of trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester,
0.5 part of unsaturated amides, that is, acrylamide, 20 parts of deionized water mix；B feed liquid by 0.09 part of reducing agent L-AA,
0.3 part of chain-transferring agent, that is, mercaptopropionic acid, 20 parts of deionized water mix.
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality
Proportion by 72 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate 0.009 part and 45 parts deionized waters investment reaction kettles (500ml's
Three-necked flask with magnetic agitation) in, 40 DEG C are warming up to, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. reacting
1.2 parts of aqueous initiator are added in kettle, constant flow pump is then respectively adopted and starts that A feed liquid and B feed liquid are added dropwise simultaneously, A feed liquid is small 3
When be added dropwise to complete, B feed liquid was added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, finally will
Resulting product is down to room temperature, and liquid alkaline (can be the sodium hydrate aqueous solution that mass percent concentration is 30%) is added and adjusts pH
Value promotees solidifying high-early strength polyocarboxy acid superplasticiser to 7.
Embodiment 2: of the present invention to promote to coagulate high-early strength polyocarboxy acid superplasticiser to be by the raw material system of following mass fractions
At: polyoxyethylene ether polymeric monomer, that is, 76 parts of isoamyl alcohol polyoxyethylene ether (TPEG4000), reducing agent ferrous sulfate 0.012
Part, 1.5 parts of aqueous initiator, that is, hydrogen peroxide (hydrogen peroxide 30%), 48 parts of deionized water, A feed liquid, B feed liquid.Above-mentioned A feed liquid
It is mixed by 9 parts of acrylic acid, 1 part of trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester, 0.2 part of Methacrylamide, 22 parts of deionized water；
B feed liquid is mixed by 0.12 part of reducing agent L-AA, 0.32 part of chain-transferring agent, that is, mercaptopropionic acid, 25 parts of deionized water.
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality
Proportion by 76 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate 0.012 part and 48 parts deionized waters investment reaction kettles (500ml's
Three-necked flask with magnetic agitation) in, 42 DEG C are warming up to, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. reacting
1.5 parts of aqueous initiator are added in kettle, constant flow pump is then respectively adopted and starts that A feed liquid and B feed liquid are added dropwise simultaneously, A feed liquid is small 3
When be added dropwise to complete, B feed liquid was added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, finally will
Resulting product is down to room temperature, and liquid alkaline is added and adjusts pH value to 7 to get the solidifying high-early strength polyocarboxy acid superplasticiser of rush.
Embodiment 3: of the present invention to promote to coagulate high-early strength polyocarboxy acid superplasticiser to be by the raw material system of following mass fractions
At: polyoxyethylene ether polymeric monomer, that is, 72 parts of isoamyl alcohol polyoxyethylene ether (TPEG6000), reducing agent ferrous sulfate 0.015
Part, 1.5 parts of aqueous initiator, that is, hydrogen peroxide (hydrogen peroxide 30%), 46 parts of deionized water, A feed liquid, B feed liquid.Above-mentioned A feed liquid
It is mixed by 8 parts of acrylic acid, 1 part of maleic acid triethanolamine dibasic acid esters, 0.5 part of acrylamide, 21 parts of deionized water；B feed liquid by
0.15 part of reducing agent L-AA, 0.32 part of chain-transferring agent, that is, mercaptopropionic acid, 22 parts of deionized water mix.
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality
Proportion by 72 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate 0.015 part and 46 parts deionized waters investment reaction kettles (500ml's
Three-necked flask with magnetic agitation) in, 45 DEG C are warming up to, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. reacting
1.5 parts of aqueous initiator are added in kettle, constant flow pump is then respectively adopted and starts that A feed liquid and B feed liquid are added dropwise simultaneously, A feed liquid is small 3
When be added dropwise to complete, B feed liquid was added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, finally will
Resulting product is down to room temperature, and liquid alkaline is added and adjusts pH value to 7 to get the solidifying high-early strength polyocarboxy acid superplasticiser of rush.
Embodiment 4: of the present invention to promote to coagulate high-early strength polyocarboxy acid superplasticiser to be by the raw material system of following mass fractions
At: polyoxyethylene ether polymeric monomer, that is, 72 parts of methyl allyl polyoxyethylene ether, 0.015 part of reducing agent ferrous sulfate aqueous draw
It sends out 1.5 parts of agent, that is, hydrogen peroxide (hydrogen peroxide 30%), 44 parts of deionized water, A feed liquid, B feed liquid.Above-mentioned A feed liquid is by acrylic acid 9
Part, 2 parts of maleic acid triethanolamine dibasic acid esters, 1 part of acrylamide, 23 parts of deionized water mix；B feed liquid is anti-bad by reducing agent L-
0.15 part of hematic acid, 0.45 part of chain-transferring agent, that is, mercaptopropionic acid, 26 parts of deionized water mix.
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality
Proportion by 72 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate 0.015 part and 44 parts deionized waters investment reaction kettles (500ml's
Three-necked flask with magnetic agitation) in, 40 DEG C are warming up to, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. reacting
1.5 parts of aqueous initiator are added in kettle, constant flow pump is then respectively adopted and starts that A feed liquid and B feed liquid are added dropwise simultaneously, A feed liquid is small 3
When be added dropwise to complete, B feed liquid was added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, finally will
Resulting product is down to room temperature, and liquid alkaline is added and adjusts pH value to 7 to get the solidifying high-early strength polyocarboxy acid superplasticiser of rush.
Embodiment 5: of the present invention to promote to coagulate high-early strength polyocarboxy acid superplasticiser to be by the raw material system of following mass fractions
At: 75 parts of polyoxyethylene ether polymeric monomer, that is, isoamyl alcohol polyoxyethylene ether (TPEG, molecular weight 4000), reducing agent sulfuric acid are sub-
0.012 part of iron, 1 part of aqueous initiator, that is, azo-bis-isobutyrate hydrochloride, 42 parts of deionized water, A feed liquid, B feed liquid.Above-mentioned A
Feed liquid is by 8 parts of acrylic acid, unsaturated 0.6 part of alkanolamine ester, 0.8 part of unsaturated amides, that is, N,N-DMAA, deionization
20 parts of water mix；B feed liquid is by 0.12 part of reducing agent L-AA, 0.4 part of chain-transferring agent, that is, mercaptopropionic acid, deionized water
23 parts mix；Unsaturated alkanolamine ester is two kinds of maleic acid triethanolamine dibasic acid esters, trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester raw materials
Combination, the mass ratio of maleic acid triethanolamine dibasic acid esters and trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester is 2:1.
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality
Proportion by 75 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate 0.012 part and 42 parts deionized waters investment reaction kettles (500ml's
Three-necked flask with magnetic agitation) in, 40 DEG C are warming up to, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. reacting
1 part of aqueous initiator is added in kettle, constant flow pump is then respectively adopted and starts that A feed liquid and B feed liquid are added dropwise simultaneously, A feed liquid was at 3 hours
It being added dropwise to complete, B feed liquid was added dropwise to complete at 3.5 hours, after all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, finally by institute
The product obtained is down to room temperature, and liquid alkaline is added and adjusts pH value to 7 to get the solidifying high-early strength polyocarboxy acid superplasticiser of rush.
The following are test portions of the invention:
Test material:
Cement: high victory cement P.O 42.5, density=3.11g/cm3, specific surface area=362m2/ kg, compression strength 3d
=24.9Mpa, compression strength 28d=49.7Mpa.
1 cement component of table, is indicated with mass percent
Sand: machine-made sand, water absorption rate 1.2%, content of stone powder 16%, apparent density 2720kg/m3。
Stone: artificial rubble 5mm-20mm, water absorption rate 0.3%, elongated particles 6%, apparent density 2720kg/m3。
Performance evaluation: flowing degree of net paste of cement is tested according to " the concrete admixture homogeneity test side GB8077-2012
Method " regulation progress, select water-cement ratio 0.29.Admixture dosage is cement quality percentage, and specific test data is as follows:
The quiet slurry test data of table 2
Can be seen that commercially available PCE from net slurry test data has to the good dispersion of cement slurry and retention property, still
The dispersion of commercially available early-strength PCE and retention property are weaker than conventional PCE, especially extend and all lose very greatly, extend from initial 200mm
Degree loss only 140mm divergence to 1 hour, loss late is up to 30%.And the rush in the present invention coagulates early-strength PCE and routine PCE
With similar dispersibility and holding capacity, especially 5 product of example compared with conventional PCE for, have and preferably keep energy
Power, 1h loss late are only 2.3%.
Concrete test below, concrete mix is as shown in table 3, concrete slump and divergence test according to
GB/T50080-2002 " Standard for test methods of properties of ordinary concrete mixture standard (attached provision explanation) " regulation carries out, experimental temperature
20 degree, humidity 52%.
3 concrete mix of table
Under conditions of guaranteeing that water consumption is constant, adjusts PCE volume (with the mass percent of cement), gone out with reaching concrete
The machine slump having the same (the positive and negative 10mm of error).Concrete goes out the machine slump and gradual loss is as follows:
4 concrete slump experimental result of table
As can be seen from the above table, concrete test result and net slurry result are coincide.Commercially available morning strong PCE reaches the identical slump
Required volume highest, while half an hour loses to the slump and there was only 20mm, loss late is up to 76%.Rush in the present invention is solidifying early strong
Volume needed for type PCE and slump-loss situation are close with routine PCE, and 5 performance of example is also better than commercially available routine PCE.
Fig. 1 is different sample concrete initial set time diagrams in test of the invention.As seen from Figure 1, use is commercially available
The concrete initial set time of PCE, commercially available morning strong PCE and example 1 is close, in 250min or so.Using from example 2 to example 5
The concrete initial set time obviously shift to an earlier date, the especially 5 initial condensation time of example shortens 60% compared with commercially available PCE.
Concrete is die-filling, and at 20 DEG C, the laboratory of 52% appropriateness is quiet to stop 4 hours, is then placed in rapid curing case, into
40 DEG C of row 6 hours steam-cured, then takes out test specimen and is placed on 20 DEG C, 14 hours in 52% laboratory, then tests concrete one
Its intensity.Intensity data is as follows:
5 concrete strength data of table
As can be seen from the above table, commercially available early-strength PCE is obviously improved compared with 1 day intensity of conventional PCE, 28 days intensity
Slightly above routine PCE.Example in the present invention, 1 day and 28 days intensity are above strong PCE of commercially available morning.Especially example 5 is 1 day strong
Degree is higher than commercially available PCE 21%, is higher than strong PCE 11% of commercially available morning, has more obvious early strong effect.Intensity is higher than height within 28 days
In commercially available PCE7%, it is higher than strong PCE 6% of commercially available morning, also has promotion for late strength of concrete.
Above-mentioned 1~example of example 5 is 1~embodiment of embodiment 5.The present invention mainly improves early strength of concrete,
It is not adversely affected simultaneously for later strength.The present invention can be shortened the concrete initial set time simultaneously, to accelerate concrete
The turnover of clay model plate, improves economic benefit.And relevant document amphipathic carboxylic dispersants are then mainly by adjusting itself parent
Water oleophylic value, which reaches, improves concrete flowability, particularly self-compacting concrete handling capacity under the conditions of reinforcing bar concentration,
Concrete workability is promoted, it is wrapped.In contrast, proportion and component of the invention is different from, it is solved the technical issues of
It is different from.
In conclusion the present invention effectively increases early strength of concrete, concrete coagulating time is shortened.
Claims (10)
1. a kind of promote solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that it is made of the raw material of following mass fractions:
70~80 parts of polyoxyethylene ether polymeric monomer, 1~1.5 part of reducing agent X, aqueous initiator, 40~50 parts of deionized water, A feed liquid, B
Feed liquid；
Above-mentioned A feed liquid is unsaturated 0.1~2 part of alkanolamine ester, unsaturated amides by 7~9 parts of acrylic acid, the solidifying early strong monomer of rush
0.1~1 part, 15~25 parts of deionized water mixes；B feed liquid is by reducing agent Y0.08~0.15 part, chain-transferring agent 0.3~0.5
Part, 18~28 parts of deionized water mix；
Wherein, above-mentioned polyoxyethylene ether polymeric monomer is methyl allyl polyoxyethylene ether, allyl polyethenoxy ether, iso-amylene
One of alcohol polyoxyethylene ether (TPEG), isobutene alcohol polyoxyethylene ether；Unsaturated alkanolamine ester is that maleic acid triethanolamine is double
Ester, maleic acid diethanol amine ester, maleic acid alkanolamine ester, trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester, methacrylic acid diethanol amine ester,
Methacrylic acid list alkanolamine ester, acrylic acid diethanol amine ester, acrylic acid list alkanolamine ester, fumaric acid triethanolamine ester, fumaric acid two
At least one of ethanol amine ester, fumaric acid monoethanolamine ester；Unsaturated amides are acrylamide, Methacrylamide, N- different
Propylacrylamide, methylene-bisacrylamide, N,N-DMAA, N, N- acrylamide, 2- acryloyl
At least one of amine；Aqueous initiator is for one of hydrogen peroxide, persulfate, azo-bis-isobutyrate hydrochloride or arbitrarily
Two kinds of combinations by any quality proportioning；The mass ratio of reducing agent Y and reducing agent X are 10~11:1；
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality proportioning
In 70~80 parts of polyoxyethylene ether polymeric monomer, reducing agent X and 40~50 parts of deionized waters investment reaction kettles, 40 will be warming up to~
50 DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. aqueous initiator is added in reaction kettle, constant flow pump is then used
Starting while A feed liquid and B feed liquid is added dropwise, A feed liquid was added dropwise to complete at 2.5~3 hours, and B feed liquid was added dropwise to complete at 3~3.5 hours,
After all feed liquids are added dropwise to complete, insulation reaction 1.5~2 hours, resulting product is finally down to room temperature, liquid alkaline is added and adjusts
PH value promotees solidifying high-early strength polyocarboxy acid superplasticiser to 7.
2. according to claim 1 promote solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that above-mentioned reducing agent X is sulfuric acid
Ferrous iron, reducing agent Y are L-AA, and the mass ratio of reducing agent Y and reducing agent X are 10:1.
3. according to claim 1 promote solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that above-mentioned chain-transferring agent is mercapto
Base propionic acid.
4. according to claim 1 promote solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that it is by following mass parts
Made of several raw materials: polyoxyethylene ether polymeric monomer, that is, 72 parts of isoamyl alcohol polyoxyethylene ether, reducing agent ferrous sulfate 0.009
Part, 1.2 parts of aqueous initiator, that is, hydrogen peroxide, 45 parts of deionized water, A feed liquid, B feed liquid；Above-mentioned A feed liquid by 8.6 parts of acrylic acid,
Unsaturated alkanolamine ester, that is, 0.4 part of trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester, 0.5 part of unsaturated amides, that is, acrylamide, deionized water
20 parts mix；B feed liquid is by 0.09 part of reducing agent L-AA, 0.3 part of chain-transferring agent, that is, mercaptopropionic acid, deionized water 20
Part mixes；
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality proportioning
By in 0.009 part and 45 parts 72 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate deionized water investment reaction kettles, it is warming up to 40
DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. 1.2 parts of aqueous initiator are added in reaction kettle, then adopt respectively
Being started that A feed liquid and B feed liquid are added dropwise simultaneously with constant flow pump, A feed liquid was added dropwise to complete at 3 hours, and B feed liquid was added dropwise to complete at 3.5 hours,
After all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, resulting product is finally down to room temperature, liquid alkaline is added and adjusts pH
Value promotees solidifying high-early strength polyocarboxy acid superplasticiser to 7.
5. according to claim 1 promote solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that it is by following mass parts
Made of several raw materials: polyoxyethylene ether polymeric monomer, that is, 76 parts of isoamyl alcohol polyoxyethylene ether, reducing agent ferrous sulfate 0.012
Part, 1.5 parts of aqueous initiator, that is, hydrogen peroxide, 48 parts of deionized water, A feed liquid, B feed liquid；Above-mentioned A feed liquid is by 9 parts of acrylic acid, three
1 part of methacrylic acid triethanolamine ester, 0.2 part of Methacrylamide, 22 parts of deionized water mix；B feed liquid is by reducing agent
0.12 part of L-AA, 0.32 part of chain-transferring agent, that is, mercaptopropionic acid, 25 parts of deionized water mix；
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality proportioning
By in 0.012 part and 48 parts 76 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate deionized water investment reaction kettles, it is warming up to 42
DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. 1.5 parts of aqueous initiator are added in reaction kettle, then adopt respectively
Being started that A feed liquid and B feed liquid are added dropwise simultaneously with constant flow pump, A feed liquid was added dropwise to complete at 3 hours, and B feed liquid was added dropwise to complete at 3.5 hours,
After all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, resulting product is finally down to room temperature, liquid alkaline is added and adjusts pH
Value promotees solidifying high-early strength polyocarboxy acid superplasticiser to 7.
6. according to claim 1 promote solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that it is by following mass parts
Made of several raw materials: polyoxyethylene ether polymeric monomer, that is, 72 parts of isoamyl alcohol polyoxyethylene ether, reducing agent ferrous sulfate 0.015
Part, 1.5 parts of aqueous initiator, that is, hydrogen peroxide, 46 parts of deionized water, A feed liquid, B feed liquid；Above-mentioned A feed liquid is by 8 parts of acrylic acid, horse
Come 1 part of triethylenetetraminehexaacetic acid hydramine dibasic acid esters, 0.5 part of acrylamide, 21 parts of deionized water mix；B feed liquid is by reducing agent L- Vitamin C
Acid 0.15 part, 0.32 part of chain-transferring agent, that is, mercaptopropionic acid, 22 parts of deionized water mix；
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality proportioning
By in 0.015 part and 46 parts 72 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate deionized water investment reaction kettles, it is warming up to 45
DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. 1.5 parts of aqueous initiator are added in reaction kettle, then adopt respectively
Being started that A feed liquid and B feed liquid are added dropwise simultaneously with constant flow pump, A feed liquid was added dropwise to complete at 3 hours, and B feed liquid was added dropwise to complete at 3.5 hours,
After all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, resulting product is finally down to room temperature, liquid alkaline is added and adjusts pH
Value promotees solidifying high-early strength polyocarboxy acid superplasticiser to 7.
7. according to claim 1 promote solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that it is by following mass parts
Made of several raw materials: polyoxyethylene ether polymeric monomer, that is, 72 parts of methyl allyl polyoxyethylene ether, reducing agent ferrous sulfate 0.015
Part, 1.5 parts of aqueous initiator, that is, hydrogen peroxide, 44 parts of deionized water, A feed liquid, B feed liquid；Above-mentioned A feed liquid is by 9 parts of acrylic acid, horse
Come 2 parts of triethylenetetraminehexaacetic acid hydramine dibasic acid esters, 1 part of acrylamide, 23 parts of deionized water mix；B feed liquid is by reducing agent L-AA
0.15 part, 0.45 part of chain-transferring agent, that is, mercaptopropionic acid, 26 parts of deionized water mix；
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality proportioning
By in 0.015 part and 44 parts 72 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate deionized water investment reaction kettles, it is warming up to 40
DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. 1.5 parts of aqueous initiator are added in reaction kettle, then adopt respectively
Being started that A feed liquid and B feed liquid are added dropwise simultaneously with constant flow pump, A feed liquid was added dropwise to complete at 3 hours, and B feed liquid was added dropwise to complete at 3.5 hours,
After all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, resulting product is finally down to room temperature, liquid alkaline is added and adjusts pH
Value promotees solidifying high-early strength polyocarboxy acid superplasticiser to 7.
8. according to claim 1 promote solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that it is by following mass parts
Made of several raw materials: polyoxyethylene ether polymeric monomer, that is, 75 parts of isoamyl alcohol polyoxyethylene ether, reducing agent ferrous sulfate 0.012
Part, 1 part of aqueous initiator, that is, azo-bis-isobutyrate hydrochloride, 42 parts of deionized water, A feed liquid, B feed liquid；Above-mentioned A feed liquid is by third
8 parts of olefin(e) acid, unsaturated 0.6 part of alkanolamine ester, 0.8 part of unsaturated amides, that is, N,N-DMAA, 20 parts of deionized water it is mixed
It closes；B feed liquid is by 0.12 part of reducing agent L-AA, 0.4 part of chain-transferring agent, that is, mercaptopropionic acid, 23 parts of deionized water mixing
It forms；Unsaturated alkanolamine ester is the combination of maleic acid triethanolamine dibasic acid esters, trimethacrylate triethylenetetraminehexaacetic acid two kinds of raw materials of alkanolamine ester, horse
The mass ratio for coming triethylenetetraminehexaacetic acid hydramine dibasic acid esters and trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester is 2:1；
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality proportioning
By in 0.012 part and 42 parts 75 parts of polyoxyethylene ether polymeric monomer, ferrous sulfate deionized water investment reaction kettles, it is warming up to 40
DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. 1 part of aqueous initiator is added in reaction kettle, then it is respectively adopted
Constant flow pump starts that A feed liquid and B feed liquid are added dropwise simultaneously, and A feed liquid was added dropwise to complete at 3 hours, and B feed liquid was added dropwise to complete at 3.5 hours, when
After all feed liquids are added dropwise to complete, insulation reaction 1.5 hours, resulting product is finally down to room temperature, liquid alkaline is added and adjusts pH value
To 7 to get the solidifying high-early strength polyocarboxy acid superplasticiser of rush.
9. a kind of preparation method for promoting solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that the rush coagulates early-strength polycarboxylic acids
Super plasticizer is made of the raw material of following mass fractions: 70~80 parts of polyoxyethylene ether polymeric monomer, reducing agent X, aqueous being drawn
1~1.5 part of agent of hair, 40~50 parts of deionized water, A feed liquid, B feed liquid；Above-mentioned A feed liquid is solidifying early strong by 7~9 parts of acrylic acid, rush
Monomer be unsaturated 0.1~2 part of alkanolamine ester, 0.1~1 part of unsaturated amides, 15~25 parts of deionized water mix；B feed liquid
It is mixed by 0.08~0.15 part of reducing agent Y, 0.3~0.5 part of chain-transferring agent, 18~28 parts of deionized water；Wherein, above-mentioned
Polyoxyethylene ether polymeric monomer be methyl allyl polyoxyethylene ether, allyl polyethenoxy ether, isoamyl alcohol polyoxyethylene ether
One of TPEG, isobutene alcohol polyoxyethylene ether；Unsaturated alkanolamine ester is maleic acid triethanolamine dibasic acid esters, maleic acid diethanol
Amine ester, maleic acid alkanolamine ester, trimethacrylate triethylenetetraminehexaacetic acid alkanolamine ester, methacrylic acid diethanol amine ester, methacrylic acid single methanol
Amine ester, acrylic acid diethanol amine ester, acrylic acid list alkanolamine ester, fumaric acid triethanolamine ester, fumaric acid diethanol amine ester, rich horse
At least one of sour monoethanolamine ester；Unsaturated amides be acrylamide, Methacrylamide, n-isopropyl acrylamide,
Methylene-bisacrylamide, N,N-DMAA, N, at least one in N- acrylamide, 2- acrylamide
Kind；Aqueous initiator is that one of hydrogen peroxide, persulfate, azo-bis-isobutyrate hydrochloride or any two kinds press any matter
Measure the combination of proportion；The mass ratio of reducing agent Y and reducing agent X are 10~11:1；
The preparation method of the solidifying high-early strength polyocarboxy acid superplasticiser of the rush comprises the technical steps that: 1. by above-mentioned quality proportioning
In 70~80 parts of polyoxyethylene ether polymeric monomer, reducing agent X and 40~50 parts of deionized waters investment reaction kettles, 40 will be warming up to~
50 DEG C, stirring to polyoxyethylene ether polymeric monomer is completely dissolved；2. aqueous initiator is added in reaction kettle, constant flow pump is then used
Starting while A feed liquid and B feed liquid is added dropwise, A feed liquid was added dropwise to complete at 2.5~3 hours, and B feed liquid was added dropwise to complete at 3~3.5 hours,
After all feed liquids are added dropwise to complete, insulation reaction 1.5~2 hours, resulting product is finally down to room temperature, liquid alkaline is added and adjusts
PH value promotees solidifying high-early strength polyocarboxy acid superplasticiser to 7.
10. the preparation method according to claim 1 for promoting solidifying high-early strength polyocarboxy acid superplasticiser, it is characterised in that above-mentioned to go back
Former agent X is ferrous sulfate, and reducing agent Y is L-AA, and the mass ratio of reducing agent Y and reducing agent X are 10:1；Above-mentioned chain turns
Shifting agent is mercaptopropionic acid.
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