CN108751785A - A kind of nanosized seeds early strength agent and preparation method thereof - Google Patents
A kind of nanosized seeds early strength agent and preparation method thereof Download PDFInfo
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- CN108751785A CN108751785A CN201810840594.5A CN201810840594A CN108751785A CN 108751785 A CN108751785 A CN 108751785A CN 201810840594 A CN201810840594 A CN 201810840594A CN 108751785 A CN108751785 A CN 108751785A
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- feed liquids
- feed
- early strength
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- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 256
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 118
- 239000002994 raw material Substances 0.000 claims abstract description 69
- 239000004815 dispersion polymer Substances 0.000 claims abstract description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000003999 initiator Substances 0.000 claims abstract description 35
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 28
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 16
- 229920000570 polyether Polymers 0.000 claims abstract description 16
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 15
- 229920000151 polyglycol Polymers 0.000 claims abstract description 15
- 239000010695 polyglycol Substances 0.000 claims abstract description 15
- 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 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 14
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 14
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 14
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical group CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims abstract description 13
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical group OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims abstract description 11
- ASUAYTHWZCLXAN-UHFFFAOYSA-N prenol Chemical compound CC(C)=CCO ASUAYTHWZCLXAN-UHFFFAOYSA-N 0.000 claims abstract description 10
- BYDRTKVGBRTTIT-UHFFFAOYSA-N 2-methylprop-2-en-1-ol Chemical compound CC(=C)CO BYDRTKVGBRTTIT-UHFFFAOYSA-N 0.000 claims abstract description 8
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 78
- 238000006243 chemical reaction Methods 0.000 claims description 57
- 239000003643 water by type Substances 0.000 claims description 54
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 claims description 19
- 239000002202 Polyethylene glycol Substances 0.000 claims description 18
- 229920001223 polyethylene glycol Polymers 0.000 claims description 18
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 15
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 13
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 12
- ZHJGWYRLJUCMRT-UHFFFAOYSA-N 5-[6-[(4-methylpiperazin-1-yl)methyl]benzimidazol-1-yl]-3-[1-[2-(trifluoromethyl)phenyl]ethoxy]thiophene-2-carboxamide Chemical compound C=1C=CC=C(C(F)(F)F)C=1C(C)OC(=C(S1)C(N)=O)C=C1N(C1=C2)C=NC1=CC=C2CN1CCN(C)CC1 ZHJGWYRLJUCMRT-UHFFFAOYSA-N 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 6
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 6
- -1 that is Substances 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical compound [Ca+2].[O-]C=O.[O-]C=O CBOCVOKPQGJKKJ-UHFFFAOYSA-L 0.000 claims description 3
- 239000004111 Potassium silicate Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 235000019255 calcium formate Nutrition 0.000 claims description 3
- 239000004281 calcium formate Substances 0.000 claims description 3
- 229940044172 calcium formate Drugs 0.000 claims description 3
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 239000002114 nanocomposite Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- 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 description 3
- HQAITFAUVZBHNB-UHFFFAOYSA-N sodium;pentahydrate Chemical compound O.O.O.O.O.[Na] HQAITFAUVZBHNB-UHFFFAOYSA-N 0.000 claims description 3
- 125000003396 thiol group Chemical class [H]S* 0.000 claims description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 4
- 235000001465 calcium Nutrition 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 230000000977 initiatory effect Effects 0.000 claims 1
- 239000004567 concrete Substances 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000007306 turnover Effects 0.000 abstract description 5
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 abstract description 4
- 239000001530 fumaric acid Substances 0.000 abstract description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 abstract description 2
- 150000001735 carboxylic acids Chemical class 0.000 abstract 2
- 239000004568 cement Substances 0.000 description 13
- 229920000642 polymer Polymers 0.000 description 9
- 239000002131 composite material Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000004570 mortar (masonry) Substances 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000010348 incorporation Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000011083 cement mortar Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- JPAOMENBKRZQDR-UHFFFAOYSA-N CC=CC.[Na] Chemical compound CC=CC.[Na] JPAOMENBKRZQDR-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical class OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 235000011148 calcium chloride Nutrition 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 235000012241 calcium silicate Nutrition 0.000 description 1
- JHLNERQLKQQLRZ-UHFFFAOYSA-N calcium silicate Chemical compound [Ca+2].[Ca+2].[O-][Si]([O-])([O-])[O-] JHLNERQLKQQLRZ-UHFFFAOYSA-N 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000012986 chain transfer agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 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
- 239000004035 construction material Substances 0.000 description 1
- 238000001816 cooling Methods 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
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- BCAARMUWIRURQS-UHFFFAOYSA-N dicalcium;oxocalcium;silicate Chemical compound [Ca+2].[Ca+2].[Ca]=O.[O-][Si]([O-])([O-])[O-] BCAARMUWIRURQS-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000344 molecularly imprinted polymer Polymers 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002627 poly(phosphazenes) Polymers 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920001444 polymaleic acid Polymers 0.000 description 1
- 230000008569 process Effects 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
- 230000001681 protective effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 235000019351 sodium silicates Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- 235000019976 tricalcium silicate Nutrition 0.000 description 1
- 229910021534 tricalcium silicate Inorganic materials 0.000 description 1
- 125000005591 trimellitate group Chemical group 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
A kind of nanosized seeds early strength agent and preparation method thereof, is first to prepare high molecular polymer dispersion liquid, then prepares nanosized seeds early strength agent again：High molecular polymer dispersion liquid is made of the raw material of following components and mass fraction：100 parts of polyether macromonomer, 2.5~4.5 parts of silane coupling agent, 7.5~12 parts of unsaturated carboxylic acid, 0.4~0.6 part of chain-transferring agent, 0.6~1.2 part of initiator, deionized water；Polyether macromonomer is one kind in prenol poly glycol monomethyl ether, methallyl alcohol poly glycol monomethyl ether；The silane coupling agent is vinyltriethoxysilane, and unsaturated carboxylic acid is one kind in acrylic acid, methacrylic acid, fumaric acid, and chain-transferring agent is mercaptopropionic acid, and initiator is at least one of ascorbic acid, hydrogen peroxide.The present invention also provides preparation methods.The present invention has apparent early strong effect to concrete, effectively shortens the concrete demoulding time, improves mold turnover and production efficiency.
Description
Technical field
The present invention relates to a kind of early strength agent, especially a kind of nanosized seeds early strength agent belongs to construction material chemical addition agent
Technical field.The invention further relates to the preparation method of the early strength agent, the preparation method of specifically a kind of nanosized seeds early strength agent.
Background technology
With the high speed development of China's modernization construction, building material field has welcome new opportunities and challenges.Currently, I
State greatly develops assembled architecture, subway and intercity track, and the application of Urban Underground pipe gallery etc., prefabricated components is more next
Wider, demand is growing day by day.Compared to ready-mixed concrete, prefabricated components can greatly improve production efficiency, save manpower, improve engineering
Quality reduces environmental pollution.But prefabricated components need in process of production improve early strength carried with shortening striking time
The turnover rate of high mold.Usual way has steam curing, increase cement consumption or incorporation early strength agent etc..Steam curing can not only
Consumption is big, and it is serious to go back environmental pollution；Increase cement consumption and be easy to cause the increase of engineering cracking risk；Common inorganic early strength agent is such as
There are many defects for villaumite, sulfate, can not only cause steel bar corrosion, have an effect on the later strength of cement-base composite material and resistance to
Long property；And some organic early strength agent such as triethanolamines, volume are not easy to control, easily cause cement-base composite material setting time mistake
It is long.In recent years, with the development of nanotechnology, in cement-base composite material, mix nano material, as nano silicon dioxide,
Nano-calcium carbonate, carbon nanotube etc. are to improve early strength, but nano particle is very easy to reunite, if cannot well divide
It dissipates, then can not effectively improve early strength；Nano material cost is higher simultaneously, and the popularization for seriously restricting it in building trade is answered
With.Therefore, research and development are environmentally protective, early strong effect is excellent, and the special early strength agent of the prefabricated components for not losing later strength is additional
The inexorable trend of agent industry development.
Inventor retrieves following Patents documents：CN102199016A discloses a kind of cement containing early strength agent,
Water is added to be configured to by hydrolyzed polymaleic acid, polyethylene glycol and sodium hydroxide by 0.03%~0.1% incorporation of cement weight to be ground
Solution, be added in cement to be ground, after grinding to obtain the final product.CN105198263A discloses a kind of preparation side of concrete early strength agent
Method first mixes allyl polyglycol, acrylic acid, methylpropene sodium sulfonate, maleic anhydride, peroxidized t-butyl perbenzoate,
Heating, heat preservation after being cooled to room temperature, are added octadecyl alcolol, p-methyl benzenesulfonic acid, ethyl acetate, heat up, and heat preservation is cooled to room temperature, institute
Mixture A successively through percent by volume be 1%~3% aqueous sulfuric acid, the NaOH of mass percent 1%~3% it is water-soluble
Liquid and water washing, dry, then with benzotriazole, 2,6- Butylated Hydroxytoluenes, hexa, trimellitate, table
Face activating agent, triisopropanolamine, sodium nitrite, sodium sulphate, calcium chloride, alum, ethyl alcohol mixing, stirring to get.
How the above technology accomplishes there is apparent early strong effect to concrete for the present invention, can effectively shorten mixed
Solidifying soil demoulding time, does not provide specific guidance program.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of nanosized seeds early strength agent, the nanosized seeds early strength agent
There is apparent early strong effect to concrete, can effectively shorten the concrete demoulding time, improve mold turnover and production efficiency.
For this purpose, the present invention also provides the preparation method of the nanosized seeds early strength agent.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
A kind of nanosized seeds early strength agent, its technical solution is that it is answered by high molecular polymer dispersion liquid and inorganic calcium silicon
The nanocomposite that object mixes is closed, wherein inorganic calcium silicon compound is nothing in the presence of high molecular polymer dispersion liquid
Machine calcareous raw material and inorganic siliceous raw material are finally obtained and are received by the tiny nanosized seeds of the size of in-situ precipitate reaction generation
Rice crystal seed early strength agent；I.e. it is first to prepare high molecular polymer dispersion liquid, then prepares nanosized seeds early strength agent again, specifically：
The high molecular polymer dispersion liquid is made of the raw material of following components and mass fraction：Polyether macromonomer
100 parts, 2.5~4.5 parts of silane coupling agent, 7.5~12 parts of unsaturated carboxylic acid, 0.4~0.6 part of chain-transferring agent, initiator 0.6~
1.2 parts, deionized water；The polyether macromonomer is prenol poly glycol monomethyl ether, methallyl alcohol polyethyleneglycol
The weight average molecular weight of one kind in methyl ether, polyether macromonomer can be 1200~4000；The silane coupling agent is vinyl
Triethoxysilane, unsaturated carboxylic acid are one kind in acrylic acid, methacrylic acid, fumaric acid, and the chain-transferring agent is mercapto
Base propionic acid, the initiator are at least one of ascorbic acid, hydrogen peroxide；
The preparation method of the high molecular polymer dispersion liquid comprises the technical steps that：Polyether macromonomer, silane is even
Join agent and 45~67 parts of deionized waters are added in reaction kettles (three-necked flask), starts blender, heat temperature raising, while by chain tra nsfer
Agent and part initiator, which are dissolved in 35~40 parts of deionized waters, is configured to A feed liquids；By unsaturated carboxylic acid addition 25~45 parts go from
B liquid is configured in sub- water；When reactor temperature rises to 45~50 DEG C, remaining initiator is added to bottom, while A is added dropwise
Feed liquid, B feed liquids, A feed liquid time for adding are 120~180 minutes, and B feed liquid time for adding is 90~150 minutes, A feed liquids, B feed liquids
Continue 45~50 DEG C of insulation reaction 0.5~1.0 hours again after dripping, reaction terminates, and deionized water is added and is diluted to theory
Solid content is 40% to get to high molecular polymer dispersion liquid；
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. taking and (having synthesized) above-mentioned macromolecule
10 parts, 150~155 parts deionized waters of polymer dispersion liquid are added in reaction kettle (three-necked flask of 500ml), start-up temperature control
Device and blender processed；2. weighing 11~12 parts of inorganic siliceous raw materials, 72~75 parts of deionized waters are added, are made into C feed liquids；Weigh 12
~18 parts of inorganic calcareous raw materials are added 40~48 parts of deionized waters and are configured to D feed liquids；3. when reactor temperature reaches 5~25
DEG C when, while C feed liquids and D feed liquids is added dropwise, C feed liquid time for adding is 110~120 minutes, and D feed liquid time for adding is 70~80 points
Clock makes solution ph in reaction kettle maintain 9.5~13.5, and after C feed liquids and D feed liquids are added dropwise, 2 parts of emulsifiers, which are added, is
Polyethylene glycol, then lasting stirring 24~72 hours are kept the temperature, after natural cooling, it is nanosized seeds morning to finally obtain milky white liquid
Strong agent.
The inorganic calcareous raw material is calcium nitrate, that is, calcium nitrate tetrahydrate [calcium nitrate (four water)], calcium formate, in calcium oxalate
One kind；Inorganic siliceous raw material is one in sodium metasilicate, potassium silicate, metasilicate pentahydrate sodium (five hydrated sodium silicates), potassium metasilicate
Kind.When synthesizing inorganic calcium silicon compound, one kind that mode is following methods is added dropwise：By inorganic calcareous raw material and inorganic siliceous
Raw material is added drop-wise in high molecular polymer dispersion liquid simultaneously, and inorganic calcareous raw material is added drop-wise to inorganic siliceous raw material and polyphosphazene polymer
In the mixed liquor for closing object dispersion liquid, or inorganic siliceous raw material is added drop-wise to inorganic calcareous raw material and high molecular polymer dispersion liquid
In mixed liquor.
In above-mentioned technical proposal, preferred technical solution can be, when being configured to A feed liquids, the dosage of initiator is preferably
The 8%~20% of its gross mass.Above-mentioned step 1. in the rotating speed of blender be preferably 200rpm~2000rpm.Carry out step
2. when, the NaOH solution that mass percent concentration is 30% is preferably first added dropwise, adjusts pH to 7.0.Step 3. in, preferably by drop
Add 1mol/l HNO3The NaOH solution that mass percent concentration is 30% is added dropwise in solution, and solution ph in reaction kettle is made to tie up
It holds 9.5~13.5.
In above-mentioned technical proposal, the preferred technical solution may also be that the nanosized seeds early strength agent is first to prepare height
Then Molecularly Imprinted Polymer dispersion liquid prepares nanosized seeds early strength agent again.The high molecular polymer dispersion liquid is by following components
And made of the raw material of mass fraction：Polyether macromonomer, that is, prenol poly glycol monomethyl ether that weight average molecular weight is 2400
100 parts, 4.4 parts of silane coupling agent, that is, vinyltriethoxysilane, 12 parts of unsaturated carboxylic acid, that is, acrylic acid, chain-transferring agent, that is, mercapto
0.55 part of base propionic acid, 0.6 part of initiator, deionized water, initiator are the combination of 0.1 part of ascorbic acid and 0.5 part of hydrogen peroxide.
The preparation method of the high molecular polymer dispersion liquid comprises the technical steps that：By prenol poly glycol monomethyl ether, second
Alkenyl triethoxysilane and 67 parts of deionized waters are added in reaction kettles, start blender, heat temperature raising, while by mercaptopropionic acid
It is dissolved in 40 parts of deionized waters with part initiator i.e. 0.1 part ascorbic acid and is configured to A feed liquids；By acrylic acid addition 45 parts go from
B liquid is configured in sub- water；When reactor temperature rises to 45 DEG C, the remaining i.e. 0.5 part of peroxidating of initiator is added to bottom
Hydrogen, while A feed liquids, B feed liquids is added dropwise, A feed liquid time for adding is 120 minutes, and B feed liquid time for adding is 90 minutes, A feed liquids, B material
Drop continues after adding 45 DEG C of insulation reaction 0.5 hours again, and reaction terminates, and deionized water is added is diluted to solid content and be
40% to get to high molecular polymer dispersion liquid.The preparation method of the nanosized seeds early strength agent comprises the technical steps that：①
10 parts, 150 parts deionized waters of above-mentioned high molecular polymer dispersion liquid are taken to be added in reaction kettle, start-up temperature controller and stirring
Device adjusts the rotating speed of blender to 400rpm, at the same be added dropwise mass percent concentration be 30% NaOH solution, adjust pH to
7.0；2. weighing 11 parts of inorganic siliceous raw materials i.e. five hydrated sodium metasilicates, 72 parts of deionized waters are added, are made into C feed liquids；Weigh 18
Inorganic calcareous raw material, that is, the calcium nitrate tetrahydrate of part is added 41 parts of deionized waters and is configured to D feed liquids；3. when reactor temperature reaches
At 20 DEG C, while C feed liquids and D feed liquids is added dropwise, C feed liquid time for adding is 110 minutes, and D feed liquid time for adding is 70 minutes, is passed through
1mol/l HNO are added dropwise3The NaOH solution that mass percent concentration is 30% is added dropwise in solution, makes solution ph in reaction kettle
11.5~12 are maintained, after C feed liquids and D feed liquids are added dropwise, 2 parts of polyethylene glycol is added, 24 are persistently stirred in 20 DEG C of heat preservations
Hour, it is nanosized seeds early strength agent to finally obtain milky white liquid.
In above-mentioned technical proposal, the preferred technical solution may also be the technical solutions that 2~embodiment of embodiment 7 is recorded.
In the use of the present invention, its volume is 0.5%~5% (mass percent) of gel material content in concrete,
It is used after being dissolved in mixing water.
The present invention nanosized seeds early strength agent be really high molecular polymer dispersion liquid and inorganic calcium silicon compound mixing and
At nanocomposite.Specifically the synthesis of high molecular polymer dispersion liquid is with polyether macromonomer, silane coupling agent, no
Saturated carboxylic acid is as comonomer, and initiator, chain-transferring agent are as molecular regulation agent, at a certain temperature, total by free radical
Poly- reaction synthesis.The synthesis of inorganic calcium silicon compound is to pass through inorganic calcareous raw material in the presence of high molecular polymer dispersion liquid
It is reacted with siliceous raw material and generates the tiny nano particle of size, the pH value of solution is controlled in reaction process.By high molecular polymer
Certain time is mixed to get to nanosized seeds early strength agent in dispersion liquid, inorganic calcium silicon compound, emulsifier.In synthesis high score
When sub- polymer dispersion liquid, silane coupling agent is added, generates the comb-shaped polymer with silanol (- Si-OH) group, is effect
Good dispersant.Inorganic water-soluble calcium salt reacts the inorganic calcium silicon compound grain generated with water-soluble silicate in preparation process
Son, itself can be condensed with silanol with the high molecular polymer dispersion liquid of synthesis, form chemical bond,
So that the inorganic calcium silicon compound particle generated, particle size are very tiny, belong to nanometer particle, can be dispersed in molten
In liquid, the stability of the early strength agent solution of synthesis is improved.The nanosized seeds early strength agent of the present invention is mixed into cement base composite wood
In material, the nucleus growth point of hydrated cementitious can be provided, reduces the nucleation barrier of hydrated cementitious, promotes early stage cement silicate mine
The aquation of object phase tricalcium silicate and dicalcium silicate, and then the early strength of cement-base composite material is improved, while not losing again
Later strength.
The nanosized seeds early strength agent of the present invention, has the following advantages：(1) simple production process, stability is good, facilitates storage
And transport；(2) there is certain water-reduction, i.e., under identical water consumption, mix nanosized seeds early strength agent, water can be improved
The workability of cement-based composite material；(3) compared with other inorganic early strength agent, nanosized seeds early strength agent of the invention not will produce
Side effect, while improving the early mechanics characteristics of cement-base composite material, later strength is unaffected, durability
Also it can improve；(4) when being used for prefabricated components production, easy to use, volume is relatively low, can effectively shorten demoulding time, improves life
Produce efficiency.
Specific implementation mode
Embodiment 1：Nanosized seeds early strength agent of the present invention is first to prepare high molecular polymer dispersion liquid, is then made again
Standby nanosized seeds early strength agent, specifically：
The high molecular polymer dispersion liquid is made of the raw material of following components and mass fraction：Weight average molecular weight is
2400 polyether macromonomer, that is, 100 parts of prenol poly glycol monomethyl ether, silane coupling agent, that is, vinyltriethoxysilane
4.4 parts, 12 parts of unsaturated carboxylic acid, that is, acrylic acid, 0.55 part of chain-transferring agent, that is, mercaptopropionic acid, 0.6 part of initiator, deionized water is drawn
Send out the combination that agent is 0.1 part of ascorbic acid and 0.5 part of hydrogen peroxide.The preparation method of the high molecular polymer dispersion liquid includes
Following processing step：Prenol poly glycol monomethyl ether, vinyltriethoxysilane and 67 parts of deionized waters are added anti-
It answers in kettle (three-necked flask of 500ml), starts blender, heat temperature raising, while by mercaptopropionic acid and part initiator i.e. 0.1 part
Ascorbic acid, which is dissolved in 40 parts of deionized waters, is configured to A feed liquids；Acrylic acid is added in 45 parts of deionized waters and is configured to B liquid；When
When reactor temperature rises to 45 DEG C, the remaining i.e. 0.5 part of hydrogen peroxide of initiator is added to bottom, while A feed liquids, B is added dropwise
Feed liquid, A feed liquid time for adding are 120 minutes, and B feed liquid time for adding is 90 minutes, and A feed liquids, B feed liquids continue after dripping 45
DEG C again insulation reaction 0.5 hour, reaction terminates, and it is 40% to get to macromolecule that deionized water, which is added, and is diluted to theoretical solid content
Polymer dispersion liquid.
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. above-mentioned high molecular polymer is taken to disperse
10 parts, 150 parts deionized waters of liquid are added in reaction kettle (three-necked flask of 500ml), start-up temperature controller and blender, are adjusted
The rotating speed of blender is saved to 400rpm, while the NaOH solution that mass percent concentration is 30% is added dropwise, adjusts pH to 7.0；②
11 parts of inorganic siliceous raw materials i.e. five hydrated sodium metasilicates are weighed, 72 parts of deionized waters are added, are made into C feed liquids；Weigh 18 parts it is inorganic
Calcareous raw material, that is, calcium nitrate tetrahydrate, (molar ratio 1.47: 1 is added 41 parts to the calcium silicon ratio of calcareous raw material and siliceous raw material used
Deionized water is configured to D feed liquids；3. when reactor temperature reaches 20 DEG C, while C feed liquids and D feed liquids is added dropwise, C feed liquids are added dropwise
Time is 110 minutes, and D feed liquid time for adding is 70 minutes, by the way that 1mol/l HNO are added dropwise3Mass percent is added dropwise in solution
A concentration of 30% NaOH solution makes solution ph in reaction kettle maintain 11.5~12, waits for that C feed liquids and D feed liquids are added dropwise
Afterwards, 2 parts of polyethylene glycol are added, heat preservation is persistently stirred 24 hours at 20 DEG C, and it is nanosized seeds morning to finally obtain milky white liquid
Strong agent.
Embodiment 2：Nanosized seeds early strength agent of the present invention is first to prepare high molecular polymer dispersion liquid, is then made again
Standby nanosized seeds early strength agent, specifically：
The component of the high molecular polymer dispersion liquid, mass fraction and the preparation method is the same as that of Example 1.
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. above-mentioned high molecular polymer is taken to disperse
10 parts, 150 parts deionized waters of liquid are added in reaction kettle (three-necked flask of 500ml), start-up temperature controller and blender, are adjusted
The rotating speed of blender is saved to 400rpm, while the NaOH solution that mass percent concentration is 30% is added dropwise, adjusts pH to 7.0；②
11 parts of inorganic siliceous raw materials i.e. five hydrated sodium metasilicates are weighed, 72 parts of deionized waters are added, are made into C feed liquids；Weigh 12 parts it is inorganic
The calcium silicon ratio (molar ratio) of calcareous raw material, that is, calcium nitrate tetrahydrate, calcareous raw material and siliceous raw material used is 0.98: 1, is added 47
Part deionized water is configured to D feed liquids；3. when reactor temperature reaches 20 DEG C, while C feed liquids and D feed liquids is added dropwise, C feed liquids drop
It is 110 minutes between added-time, D feed liquid time for adding is 70 minutes, by the way that 1mol/l HNO are added dropwise3Solution makes pH value of solution in reaction kettle
Value maintains 11.5, and after C feed liquids and D feed liquids are added dropwise, 2 parts of polyethylene glycol are added, and at 20 DEG C, persistently stirring 24 is small for heat preservation
When, it is nanosized seeds early strength agent to finally obtain milky white liquid.
Embodiment 3：Nanosized seeds early strength agent of the present invention is first to prepare high molecular polymer dispersion liquid, is then made again
Standby nanosized seeds early strength agent, specifically：
The component of the high molecular polymer dispersion liquid, mass fraction and the preparation method is the same as that of Example 1.
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. above-mentioned high molecular polymer is taken to disperse
10 parts, 150 parts deionized waters of liquid are added in reaction kettle (three-necked flask of 500ml), start-up temperature controller and blender, are adjusted
The rotating speed of blender is saved to 400rpm, while the NaOH solution that mass percent concentration is 30% is added dropwise, adjusts pH to 7.0；②
11 parts of inorganic siliceous raw materials i.e. five hydrated sodium metasilicates are weighed, 72 parts of deionized waters are added, are made into C feed liquids；Weigh 18 parts it is inorganic
The calcium silicon ratio (molar ratio) of calcareous raw material, that is, calcium nitrate tetrahydrate, calcareous raw material and siliceous raw material used is 1.47: 1, is added 41
Part deionized water is configured to D feed liquids；3. when reactor temperature reaches 20 DEG C, while C feed liquids and D feed liquids is added dropwise, C feed liquids drop
It is 110 minutes between added-time, D feed liquid time for adding is 70 minutes, the NaOH solution for being 30% by the way that mass percent concentration is added dropwise,
So that solution ph in reaction kettle is maintained 12.5~13, after C feed liquids and D feed liquids are added dropwise, 2 parts of polyethylene glycol are added,
20 DEG C of heat preservations are persistently stirred 24 hours, and it is nanosized seeds early strength agent to finally obtain milky white liquid.
Embodiment 4：Nanosized seeds early strength agent of the present invention is first to prepare high molecular polymer dispersion liquid, is then made again
Standby nanosized seeds early strength agent, specifically：
The high molecular polymer dispersion liquid is made of the raw material of following components and mass fraction：Weight average molecular weight is
100 parts of 3000 methallyl alcohol poly glycol monomethyl ether, 2.62 parts of vinyltriethoxysilane, unsaturated carboxylic acid, that is, propylene
7.62 parts of acid, 0.44 part of chain-transferring agent, that is, mercaptopropionic acid, 1.1 parts of initiator, deionized water, initiator are 0.1 part of ascorbic acid
With the combination of 1 part of hydrogen peroxide；
The preparation method of the high molecular polymer dispersion liquid comprises the technical steps that：By methallyl alcohol polyethylene glycol
Monomethyl ether, vinyltriethoxysilane and 46.41 parts of deionized waters are added in reaction kettle (three-necked flask of 500ml), start
Blender, heat temperature raising, while mercaptopropionic acid and part initiator i.e. 0.1 part ascorbic acid being dissolved in 35.7 parts of deionized waters
It is configured to A feed liquids；Acrylic acid is added in 25 parts of deionized waters and is configured to B liquid；When reactor temperature rises to 45 DEG C, to kettle
The remaining i.e. 1 part of hydrogen peroxide of initiator is added in bottom, while A feed liquids, B feed liquids is added dropwise, and A feed liquid time for adding is 180 minutes, B
Feed liquid time for adding is 150 minutes, and at 45 DEG C, insulation reaction 1.0 hours, reaction are tied again for continuation after A feed liquids, B feed liquids drip
Beam, it is 40% to get to high molecular polymer dispersion liquid that deionized water, which is added, and is diluted to theoretical solid content；
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. above-mentioned high molecular polymer is taken to disperse
10 parts, 150 parts deionized waters of liquid are added in reaction kettle (three-necked flask of 500ml), start-up temperature controller and blender, are adjusted
The rotating speed of blender is saved to 400rpm, while the NaOH solution that mass percent concentration is 30% is added dropwise, adjusts pH to 7.0；②
11 parts of inorganic siliceous raw materials i.e. five hydrated sodium metasilicates are weighed, 72 parts of deionized waters are added, are made into C feed liquids；Weigh 18 parts it is inorganic
The calcium silicon ratio (molar ratio) of calcareous raw material, that is, calcium nitrate tetrahydrate, calcareous raw material and siliceous raw material used is 1.47: 1, is added 41
Part deionized water is configured to D feed liquids；3. when reactor temperature reaches 20 DEG C, while C feed liquids and D feed liquids is added dropwise, C feed liquids drop
It is 110 minutes between added-time, D feed liquid time for adding is 70 minutes, by the way that 1mol/l HNO are added dropwise3Quality percentage is added dropwise in solution
The NaOH solution that specific concentration is 30%, makes solution ph in reaction kettle maintain 11.5~12, waits for that C feed liquids and D feed liquids drip
2 parts of polyethylene glycol are added in Bi Hou, and at 20 DEG C, heat preservation is persistently stirred 30 hours, and it is nanosized seeds to finally obtain milky white liquid
Early strength agent.
Embodiment 5：Nanosized seeds early strength agent of the present invention is first to prepare high molecular polymer dispersion liquid, is then made again
Standby nanosized seeds early strength agent, specifically：
Component, mass fraction and the preparation method of the high molecular polymer dispersion liquid are the same as embodiment 4.
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. above-mentioned high molecular polymer is taken to disperse
10 parts, 150 parts deionized waters of liquid are added in reaction kettle (three-necked flask of 500ml), start-up temperature controller and blender, are adjusted
The rotating speed of blender is saved to 400rpm, while the NaOH solution that mass percent concentration is 30% is added dropwise, adjusts pH to 7.0；②
11 parts of inorganic siliceous raw materials i.e. five hydrated sodium metasilicates are weighed, 72 parts of deionized waters are added, are made into C feed liquids；Weigh 12 parts it is inorganic
The calcium silicon ratio (molar ratio) of calcareous raw material, that is, calcium nitrate tetrahydrate, calcareous raw material and siliceous raw material used is 0.98: 1), it is added 47
Part deionized water is configured to D feed liquids；3. when reactor temperature reaches 20 DEG C, while C feed liquids and D feed liquids is added dropwise, C feed liquids drop
It is 110 minutes between added-time, D feed liquid time for adding is 70 minutes, by the way that 1mol/l HNO are added dropwise3Quality percentage is added dropwise in solution
The NaOH solution that specific concentration is 30%, makes solution ph in reaction kettle maintain 11.5~12, waits for that C feed liquids and D feed liquids drip
2 parts of polyethylene glycol are added in Bi Hou, and at 20 DEG C, heat preservation is persistently stirred 24 hours, and it is nanosized seeds to finally obtain milky white liquid
Early strength agent.
Embodiment 6：Nanosized seeds early strength agent of the present invention is first to prepare high molecular polymer dispersion liquid, is then made again
Standby nanosized seeds early strength agent, specifically：
Component, mass fraction and the preparation method of the high molecular polymer dispersion liquid are the same as embodiment 4.
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. above-mentioned high molecular polymer is taken to disperse
10 parts, 150 parts deionized waters of liquid are added in reaction kettle (three-necked flask of 500ml), start-up temperature controller and blender, are adjusted
The rotating speed of blender is saved to 400rpm, while the NaOH solution that mass percent concentration is 30% is added dropwise, adjusts pH to 7.0；②
11 parts of inorganic siliceous raw materials i.e. five hydrated sodium metasilicates are weighed, 72 parts of deionized waters are added, are made into C feed liquids；Weigh 18 parts it is inorganic
The calcium silicon ratio (molar ratio) of calcareous raw material, that is, calcium nitrate tetrahydrate, calcareous raw material and siliceous raw material used is 1.47: 1, is added 41
Part deionized water is configured to D feed liquids；3. when reactor temperature reaches 20 DEG C, while C feed liquids and D feed liquids is added dropwise, C feed liquids drop
It is 110 minutes between added-time, D feed liquid time for adding is 70 minutes, the NaOH solution for being 30% by the way that mass percent concentration is added dropwise,
So that solution ph in reaction kettle is maintained 12.5~13, after C feed liquids and D feed liquids are added dropwise, 2 parts of polyethylene glycol are added,
20 DEG C of heat preservations are persistently stirred 24 hours, and it is nanosized seeds early strength agent to finally obtain milky white liquid.
Embodiment 7：Nanosized seeds early strength agent of the present invention is first to prepare high molecular polymer dispersion liquid, is then made again
Standby nanosized seeds early strength agent, specifically：
Component, mass fraction and the preparation method of the high molecular polymer dispersion liquid are the same as embodiment 4.
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：Weigh 11 parts of inorganic siliceous raw materials i.e. five
Hydrated sodium metasilicate is added 72 parts of deionized waters, is made into C feed liquids；Weigh 18 parts of inorganic calcareous raw materials i.e. calcium nitrate tetrahydrate, institute
It is 1.47: 1 with the calcium silicon ratio (molar ratio) of calcareous raw material and siliceous raw material, 41 parts of deionized waters is added and are configured to D feed liquids；It takes
10 parts of high molecular polymer dispersion liquid, C feed liquids, 150 parts of deionized waters are stated to be added in reaction kettle (three-necked flask of 500ml),
Start-up temperature controller and blender adjust the rotating speed of blender to 400rpm；When reactor temperature reaches 20 DEG C, it is added dropwise
D feed liquids, D feed liquid time for adding are 70 minutes, while the NaOH solution for being 30% by the way that mass percent concentration is added dropwise, and make reaction
Solution ph maintains 12.5~13 in kettle, after D feed liquids are added dropwise, 2 parts of polyethylene glycol is added, keeps the temperature at 20 DEG C and persistently stirs
It mixes 24 hours, it is nanosized seeds early strength agent to finally obtain milky white liquid.
It is the experimental section of the present invention below：
Application example 1：Using P.O42.5 Lafarge cement, match ratio cement 450g, normal sand 1350g, the ratio of mud 0.5,
Early strength agent volume 2.0% (accounts for cement weight percentage), and mixing water need to deduct the water content in early strength agent, according to GB/T 2419-
2005《Mortar'S Flowability assay method》Test the mobility of cement mortar, GB 17671-1999《Strength of cement mortar detection side
Method》Carry out mortar strength experiment.Table 1 is that mortar performance tests table.
1 mortar performance of table tests table
The early strength agent that the present invention synthesizes it can be seen from 1 data of table has certain water-reducing effect, (not compared to blank group
Mix early strength agent), 1~embodiment of embodiment 7 all improves to Mortar'S Flowability, i.e., under identical water consumption, invention
Early strength agent can make mortar have better mobility.Compared to blank group, mixed with the mortar specimen of early strength agent, in standard curing item
Under part, compression strength all improves, and especially early anti pressured intension (12h~3d) is obviously improved, the resistance to compression of 28 days later stages
There is no reduce for intensity.Illustrate that the early strength agent of synthesis has good early strong effect, while later stage compression strength is not generated
Side effect.
Application example 2：According to GB/T 50080-2002《Standard for test methods of properties of ordinary concrete mixture standard》And GB/
T 50081—2002《Standard for test methods of mechanical properties of ordinary concrete》Testing concrete performance is carried out, it is main to investigate incorporation
After early-strength dose, concrete strength development.The conventional concrete match ratio of use is shown in Table 2, the fixed present invention's
Early strength agent volume be 2.0%, while using Chang'an cultivate people of ability company production GK-3000 polycarboxylate water-reducers, adjust each group coagulation
Native mobility (initial slump) is almost the same, and under the conditions of standard curing, the intensity test of each group concrete the results are shown in Table
3。
2 concrete mix of table
| Cement/kg | Flyash/kg | Sand/kg | Stone/kg | Water/kg |
| 335 | 90 | 770 | 1036 | 143 |
3 testing concrete performance table of table
It is supported in standard mixed with early-strength dose of concrete sample compared to blank group it can be seen from 3 data of table
Under the conditions of shield, compression strength all improves, and especially early anti pressured intension (12h~3d) is obviously improved, while the later stage
There is no retractions for 28 days compression strength.Thus illustrate that the early strength agent that the present invention synthesizes has apparent early strong effect to concrete,
It can effectively shorten the concrete demoulding time, improve mold turnover and production efficiency, through experiment, the present invention makes mold turnover carry
High by 25% or more, production efficiency improves 28% or more.
Early-strength dose is that the nanometer mixed by high molecular polymer dispersion liquid and inorganic calcium silicon compound is answered
Condensation material.Wherein inorganic calcium silicon compound is the inorganic calcareous raw material and inorganic siliceous in the presence of high molecular polymer dispersion liquid
Raw material passes through the tiny nanosized seeds of the size of in-situ precipitate reaction generation.The crystal seed early strength agent can improve cement base composite wood
The early strength of material shortens curing time, and does not lose later strength.
Above description is only the description to present pre-ferred embodiments, not to any restriction of the scope of the invention.Ability
Any change, the modification that field technique personnel are done according to the disclosure above content, belong to scope of the claims.
Claims (10)
1. a kind of nanosized seeds early strength agent, it is characterised in that it is mixed by high molecular polymer dispersion liquid and inorganic calcium silicon compound
Nanocomposite made of conjunction, wherein inorganic calcium silicon compound be in the presence of high molecular polymer dispersion liquid, it is inorganic calcareous
The nanosized seeds that raw material and inorganic siliceous raw material are generated by in-situ precipitate reaction, and finally obtain nanosized seeds early strength agent；I.e.
It is first to prepare high molecular polymer dispersion liquid, then prepares nanosized seeds early strength agent again：
The high molecular polymer dispersion liquid is made of the raw material of following components and mass fraction：100 parts of polyether macromonomer,
2.5~4.5 parts of silane coupling agent, 7.5~12 parts of unsaturated carboxylic acid, 0.4~0.6 part of chain-transferring agent, 0.6~1.2 part of initiator,
Deionized water；The polyether macromonomer is in prenol poly glycol monomethyl ether, methallyl alcohol poly glycol monomethyl ether
One kind；The silane coupling agent is vinyltriethoxysilane, and unsaturated carboxylic acid is acrylic acid, methacrylic acid, richness
One kind in horse acid, the chain-transferring agent are mercaptopropionic acid, the initiator is ascorbic acid, in hydrogen peroxide at least
It is a kind of；
The preparation method of the high molecular polymer dispersion liquid comprises the technical steps that：By polyether macromonomer, silane coupling agent
It is added in reaction kettles with 45~67 parts of deionized waters, starts blender, heat temperature raising, while by chain-transferring agent and part initiator
It is dissolved in 35~40 parts of deionized waters and is configured to A feed liquids；Unsaturated carboxylic acid is added in 25~45 parts of deionized waters and is configured to B
Liquid；When reactor temperature rises to 45~50 DEG C, remaining initiator is added to bottom, while A feed liquids, B feed liquids, A is added dropwise
Feed liquid time for adding is 120~180 minutes, and B feed liquid time for adding is 90~150 minutes, and A feed liquids, B feed liquids continue after dripping
45~50 DEG C of insulation reaction 0.5~1.0 hours again, reaction terminates, and it is 40% that deionized water, which is added, and is diluted to theoretical solid content,
Obtain high molecular polymer dispersion liquid；
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. taking above-mentioned high molecular polymer dispersion liquid 10
Part, 150~155 parts of deionized waters are added in reaction kettle (three-necked flask of 500ml), start-up temperature controller and blender；
2. weighing 11~12 parts of inorganic siliceous raw materials, 72~75 parts of deionized waters are added, are made into C feed liquids；Weigh 12~18 parts of inorganic calciums
Matter raw material is added 40~48 parts of deionized waters and is configured to D feed liquids；3. when reactor temperature reaches 5~25 DEG C, it is added dropwise simultaneously
C feed liquids and D feed liquids, C feed liquid time for adding are 110~120 minutes, and D feed liquid time for adding is 70~80 minutes, is made in reaction kettle
Solution ph maintains 9.5~13.5, after C feed liquids and D feed liquids are added dropwise, 2 parts of emulsifier, that is, polyethylene glycol is added, then protect
Temperature persistently stirs 24~72 hours, and it is nanosized seeds early strength agent to finally obtain milky white liquid；
The inorganic calcareous raw material is calcium nitrate, that is, calcium nitrate tetrahydrate, calcium formate, one kind in calcium oxalate；Inorganic siliceous raw material
For one kind in sodium metasilicate, potassium silicate, metasilicate pentahydrate sodium, potassium metasilicate.
2. nanosized seeds early strength agent according to claim 1, it is characterised in that when being configured to A feed liquids, the dosage of initiator
It is the 8%~20% of its gross mass.
3. nanosized seeds early strength agent according to claim 1, it is characterised in that above-mentioned step 1. in blender rotating speed
For 200rpm~2000rpm.
4. nanosized seeds early strength agent according to claim 1, it is characterised in that when carrying out step 2., quality percentage is first added dropwise
The NaOH solution that specific concentration is 30% adjusts pH to 7.0.
5. nanosized seeds early strength agent according to claim 1, it is characterised in that step 3. in, pass through be added dropwise 1mol/l HNO3
The NaOH solution that mass percent concentration is 30% is added dropwise in solution, and solution ph in reaction kettle is made to maintain 9.5~13.5.
6. nanosized seeds early strength agent according to claim 1, it is characterised in that it is first to prepare high molecular polymer dispersion
Then liquid prepares nanosized seeds early strength agent again：
The high molecular polymer dispersion liquid is made of the raw material of following components and mass fraction：Weight average molecular weight is 2400
Polyether macromonomer, that is, 100 parts of prenol poly glycol monomethyl ether, silane coupling agent, that is, vinyltriethoxysilane 4.4
Part, 12 parts of unsaturated carboxylic acid, that is, acrylic acid, 0.55 part of chain-transferring agent, that is, mercaptopropionic acid, 0.6 part of initiator, deionized water, initiation
Agent is the combination of 0.1 part of ascorbic acid and 0.5 part of hydrogen peroxide；
The preparation method of the high molecular polymer dispersion liquid comprises the technical steps that：By prenol polyethyleneglycol first
Ether, vinyltriethoxysilane and 67 parts of deionized waters are added in reaction kettles, start blender, heat temperature raising, while by mercapto
Base propionic acid and part initiator i.e. 0.1 part ascorbic acid, which are dissolved in 40 parts of deionized waters, is configured to A feed liquids；Acrylic acid is added 45
It is configured to B liquid in part deionized water；When reactor temperature rises to 45 DEG C, remaining i.e. 0.5 part of initiator is added to bottom
Hydrogen peroxide, while A feed liquids, B feed liquids is added dropwise, A feed liquid time for adding is 120 minutes, and B feed liquid time for adding is 90 minutes, A material
Liquid, B feed liquids continue after dripping 45 DEG C of insulation reaction 0.5 hours again, and reaction terminates, and deionized water is added and is diluted to solid content
For 40% to get to high molecular polymer dispersion liquid；
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. taking above-mentioned high molecular polymer dispersion liquid 10
Part, 150 parts of deionized waters be added in reaction kettle, start-up temperature controller and blender, adjust the rotating speed of blender to
400rpm, while the NaOH solution that mass percent concentration is 30% is added dropwise, adjust pH to 7.0；2. weigh 11 parts it is inorganic siliceous
Raw material i.e. five hydrated sodium metasilicates are added 72 parts of deionized waters, are made into C feed liquids；18 parts of inorganic calcareous raw materials i.e. four are weighed to be hydrated
Calcium nitrate is added 41 parts of deionized waters and is configured to D feed liquids；3. when reactor temperature reaches 20 DEG C, at the same be added dropwise C feed liquids and
D feed liquids, C feed liquid time for adding are 110 minutes, and D feed liquid time for adding is 70 minutes, by the way that 1mol/l HNO are added dropwise3Solution or
The NaOH solution that mass percent concentration is 30% is added dropwise in person, so that solution ph in reaction kettle is maintained 11.5~12, waits for C feed liquids
After being added dropwise with D feed liquids, 2 parts of polyethylene glycol are added, heat preservation is persistently stirred 24 hours at 20 DEG C, finally obtains milky white liquid
As nanosized seeds early strength agent.
7. nanosized seeds early strength agent according to claim 1, it is characterised in that it is first to prepare high molecular polymer dispersion
Then liquid prepares nanosized seeds early strength agent again：
The high molecular polymer dispersion liquid is made of the raw material of following components and mass fraction：Weight average molecular weight is 3000
100 parts of methallyl alcohol poly glycol monomethyl ether, 2.62 parts of vinyltriethoxysilane, unsaturated carboxylic acid, that is, acrylic acid
7.62 parts, 0.44 part of chain-transferring agent, that is, mercaptopropionic acid, 1.1 parts of initiator, deionized water, initiator is 0.1 part of ascorbic acid and 1
The combination of part hydrogen peroxide；
The preparation method of the high molecular polymer dispersion liquid comprises the technical steps that：By methallyl alcohol polyethyleneglycol first
Ether, vinyltriethoxysilane and 46.41 parts of deionized waters are added in reaction kettle, start blender, and heat temperature raising simultaneously will
Mercaptopropionic acid and part initiator i.e. 0.1 part ascorbic acid, which are dissolved in 35.7 parts of deionized waters, is configured to A feed liquids；By acrylic acid plus
Enter in 25 parts of deionized waters and is configured to B liquid；When reactor temperature rises to 45 DEG C, remaining initiator i.e. 1 is added to bottom
Part hydrogen peroxide, while A feed liquids, B feed liquids is added dropwise, A feed liquid time for adding is 180 minutes, and B feed liquid time for adding is 150 minutes,
A feed liquids, B feed liquids continue after dripping 45 DEG C of insulation reaction 1.0 hours again, and reaction terminates, be added deionized water be diluted to it is solid
Content is 40% to get to high molecular polymer dispersion liquid；
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. taking above-mentioned high molecular polymer dispersion liquid 10
Part, 150 parts of deionized waters be added in reaction kettle, start-up temperature controller and blender, adjust the rotating speed of blender to
400rpm, while the NaOH solution that mass percent concentration is 30% is added dropwise, adjust pH to 7.0；2. weigh 11 parts it is inorganic siliceous
Raw material i.e. five hydrated sodium metasilicates are added 72 parts of deionized waters, are made into C feed liquids；18 parts of inorganic calcareous raw materials i.e. four are weighed to be hydrated
Calcium nitrate is added 41 parts of deionized waters and is configured to D feed liquids；3. when reactor temperature reaches 20 DEG C, at the same be added dropwise C feed liquids and
D feed liquids, C feed liquid time for adding are 110 minutes, and D feed liquid time for adding is 70 minutes, by the way that 1mol/l HNO are added dropwise3Solution or
The NaOH solution that mass percent concentration is 30% is added dropwise in person, so that solution ph in reaction kettle is maintained 11.5~12, waits for C feed liquids
After being added dropwise with D feed liquids, 2 parts of polyethylene glycol are added, heat preservation is persistently stirred 30 hours at 20 DEG C, finally obtains milky white liquid
As nanosized seeds early strength agent.
8. a kind of preparation method of nanosized seeds early strength agent, it is characterised in that it is first to prepare high molecular polymer dispersion liquid, so
Prepare nanosized seeds early strength agent again afterwards：
The high molecular polymer dispersion liquid is made of the raw material of following components and mass fraction：100 parts of polyether macromonomer,
2.5~4.5 parts of silane coupling agent, 7.5~12 parts of unsaturated carboxylic acid, 0.4~0.6 part of chain-transferring agent, 0.6~1.2 part of initiator,
Deionized water；The polyether macromonomer is in prenol poly glycol monomethyl ether, methallyl alcohol poly glycol monomethyl ether
One kind；The silane coupling agent is vinyltriethoxysilane, and unsaturated carboxylic acid is acrylic acid, methacrylic acid, richness
One kind in horse acid, the chain-transferring agent are mercaptopropionic acid, the initiator is ascorbic acid, in hydrogen peroxide at least
It is a kind of；
The preparation method of the high molecular polymer dispersion liquid comprises the technical steps that：By polyether macromonomer, silane coupling agent
It is added in reaction kettles with 45~67 parts of deionized waters, starts blender, heat temperature raising, while by chain-transferring agent and part initiator
It is dissolved in 35~40 parts of deionized waters and is configured to A feed liquids；Unsaturated carboxylic acid is added in 25~45 parts of deionized waters and is configured to B
Liquid；When reactor temperature rises to 45~50 DEG C, remaining initiator is added to bottom, while A feed liquids, B feed liquids, A is added dropwise
Feed liquid time for adding is 120~180 minutes, and B feed liquid time for adding is 90~150 minutes, and A feed liquids, B feed liquids continue after dripping
45~50 DEG C of insulation reaction 0.5~1.0 hours again, reaction terminates, and it is 40% that deionized water, which is added, and is diluted to theoretical solid content,
Obtain high molecular polymer dispersion liquid；
The preparation method of the nanosized seeds early strength agent comprises the technical steps that：1. taking above-mentioned high molecular polymer dispersion liquid 10
Part, 150~155 parts of deionized waters are added in reaction kettle (three-necked flask of 500ml), start-up temperature controller and blender；
2. weighing 11~12 parts of inorganic siliceous raw materials, 72~75 parts of deionized waters are added, are made into C feed liquids；Weigh 12~18 parts of inorganic calciums
Matter raw material is added 40~48 parts of deionized waters and is configured to D feed liquids；3. when reactor temperature reaches 5~25 DEG C, it is added dropwise simultaneously
C feed liquids and D feed liquids, C feed liquid time for adding are 110~120 minutes, and D feed liquid time for adding is 70~80 minutes, is made in reaction kettle
Solution ph maintains 9.5~13.5, after C feed liquids and D feed liquids are added dropwise, 2 parts of emulsifier, that is, polyethylene glycol is added, then protect
Temperature persistently stirs 24~72 hours, and it is nanosized seeds early strength agent to finally obtain milky white liquid；
The inorganic calcareous raw material is calcium nitrate, that is, calcium nitrate tetrahydrate, calcium formate, one kind in calcium oxalate；Inorganic siliceous raw material
For one kind in sodium metasilicate, potassium silicate, metasilicate pentahydrate sodium, potassium metasilicate.
9. the preparation method of nanosized seeds early strength agent according to claim 8, it is characterised in that when being configured to A feed liquids, draw
Send out agent dosage be its gross mass 8%~20%, above-mentioned step 1. in blender rotating speed be 200rpm~2000rpm.
10. the preparation method of nanosized seeds early strength agent according to claim 8, it is characterised in that when carrying out step 2., first
The NaOH solution that mass percent concentration is 30% is added dropwise, adjusts pH to 7.0；Step 3. in, pass through be added dropwise 1mol/l HNO3It is molten
The NaOH solution that mass percent concentration is 30% is added dropwise in liquid, and solution ph in reaction kettle is made to maintain 9.5~13.5.
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