CN104479066A - Concrete viscosity adjusting agent and preparation method thereof - Google Patents
Concrete viscosity adjusting agent and preparation method thereof Download PDFInfo
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- CN104479066A CN104479066A CN201410717601.4A CN201410717601A CN104479066A CN 104479066 A CN104479066 A CN 104479066A CN 201410717601 A CN201410717601 A CN 201410717601A CN 104479066 A CN104479066 A CN 104479066A
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- concrete
- conditioning agent
- monomer
- concrete viscosity
- viscosity conditioning
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004034 viscosity adjusting agent Substances 0.000 title abstract description 10
- 239000000178 monomer Substances 0.000 claims abstract description 53
- 125000002091 cationic group Chemical group 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 56
- 230000003750 conditioning effect Effects 0.000 claims description 46
- -1 acrylyl Chemical group 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000003999 initiator Substances 0.000 claims description 13
- 239000004971 Cross linker Substances 0.000 claims description 11
- YXYZMHGSOKYZAF-UHFFFAOYSA-M [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C Chemical compound [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C YXYZMHGSOKYZAF-UHFFFAOYSA-M 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 9
- 230000002829 reductive effect Effects 0.000 claims description 9
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 9
- 239000004160 Ammonium persulphate Substances 0.000 claims description 8
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims description 7
- 239000007800 oxidant agent Substances 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 6
- 238000000354 decomposition reaction Methods 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 5
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 claims description 5
- 125000000129 anionic group Chemical group 0.000 claims description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 5
- 239000011976 maleic acid Substances 0.000 claims description 5
- TURITJIWSQEMDB-UHFFFAOYSA-N 2-methyl-n-[(2-methylprop-2-enoylamino)methyl]prop-2-enamide Chemical compound CC(=C)C(=O)NCNC(=O)C(C)=C TURITJIWSQEMDB-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 239000001530 fumaric acid Substances 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- NEBBLNDVSSWJLL-UHFFFAOYSA-N 2,3-bis(2-methylprop-2-enoyloxy)propyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(OC(=O)C(C)=C)COC(=O)C(C)=C NEBBLNDVSSWJLL-UHFFFAOYSA-N 0.000 claims description 2
- PUGOMSLRUSTQGV-UHFFFAOYSA-N 2,3-di(prop-2-enoyloxy)propyl prop-2-enoate Chemical compound C=CC(=O)OCC(OC(=O)C=C)COC(=O)C=C PUGOMSLRUSTQGV-UHFFFAOYSA-N 0.000 claims description 2
- TWIBMMJOYQLMPY-UHFFFAOYSA-M CCC[N+](CC)(CCC)C(CC)OC(C=C)=O.[Cl-] Chemical compound CCC[N+](CC)(CCC)C(CC)OC(C=C)=O.[Cl-] TWIBMMJOYQLMPY-UHFFFAOYSA-M 0.000 claims description 2
- OTNVZZJALIYNEO-UHFFFAOYSA-M [Br-].C(C=C)(=O)OC(C)[N+](CC)(CC)CC Chemical compound [Br-].C(C=C)(=O)OC(C)[N+](CC)(CC)CC OTNVZZJALIYNEO-UHFFFAOYSA-M 0.000 claims description 2
- 125000004386 diacrylate group Chemical group 0.000 claims description 2
- GRWZHXKQBITJKP-UHFFFAOYSA-N dithionous acid Chemical compound OS(=O)S(O)=O GRWZHXKQBITJKP-UHFFFAOYSA-N 0.000 claims description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Chemical compound CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 230000000977 initiatory effect Effects 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 2
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 claims description 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 2
- ZOJCYZJYLRWMCZ-UHFFFAOYSA-M triethyl(1-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)C(C)OC(=O)C=C ZOJCYZJYLRWMCZ-UHFFFAOYSA-M 0.000 claims description 2
- NRTLTGGGUQIRRT-UHFFFAOYSA-N triethylazanium;bromide Chemical compound [Br-].CC[NH+](CC)CC NRTLTGGGUQIRRT-UHFFFAOYSA-N 0.000 claims description 2
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 claims description 2
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 claims description 2
- BMXILUZRCXPKOI-UHFFFAOYSA-N tripropylazanium;chloride Chemical compound Cl.CCCN(CCC)CCC BMXILUZRCXPKOI-UHFFFAOYSA-N 0.000 claims description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims 1
- 239000004159 Potassium persulphate Substances 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 229910052783 alkali metal Inorganic materials 0.000 claims 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims 1
- 235000019394 potassium persulphate Nutrition 0.000 claims 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims 1
- 230000000740 bleeding effect Effects 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 7
- 229920000642 polymer Polymers 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 3
- 239000003431 cross linking reagent Substances 0.000 abstract 3
- 239000000654 additive Substances 0.000 abstract 1
- 150000003254 radicals Chemical class 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 27
- 239000000243 solution Substances 0.000 description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 16
- 238000003756 stirring Methods 0.000 description 16
- 239000007787 solid Substances 0.000 description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 8
- 238000006073 displacement reaction Methods 0.000 description 8
- 238000005227 gel permeation chromatography Methods 0.000 description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 8
- 239000003638 chemical reducing agent Substances 0.000 description 7
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 7
- 239000004568 cement Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 4
- 229920005646 polycarboxylate Polymers 0.000 description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 4
- 239000010881 fly ash Substances 0.000 description 3
- 239000012966 redox initiator Substances 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 230000008719 thickening Effects 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 229920002310 Welan gum Polymers 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a concrete viscosity adjusting agent and a preparation method thereof. The concrete viscosity adjusting agent is prepared by copolymerizing a cationic monomer, an anion carboxyl monomer and an inner cross-linking agent together with a free radical, wherein the mole ratio of the cationic monomer to the anion carboxyl monomer and the inner cross-linking agent is 1:(0.5-5):(0.01-0.1). As the cationic monomer and the anion carboxyl monomer are adopted to copolymerize to obtain an amphoteric polymer, the concrete viscosity adjusting agent has remarkable antipolyelectrolyte property and is relatively good in viscosity improvement property; due to adoption of the inner cross-linking agent, three-dimensional net-shaped structures are formed among the viscosity adjusting agent and binding material grains, the concrete disintegration bleeding problem is greatly solved, and the peaceability of concrete is improved. The prepared concrete viscosity adjusting agent is good in compatibility with other additives, the strength development of concrete is not affected, and particularly the concrete disintegration bleeding problem can be effectively solved under the condition of low binding materials.
Description
Technical field
The present invention relates to concrete admixture field, be specifically related to a kind of concrete viscosity conditioning agent and preparation method thereof.
Background technology
Along with the development of Architectural Structure Design and high-rise building, building operation it is also proposed higher requirement to concrete performance.The continuous increase of reinforcing bar density in the constantly complicated and building slab of concrete member, often require that concrete has large fluidised form, if but mixture is excessively rare, easily there is laminated segregation phenomenon in concrete, easily cause stifled pump, construction part to leak and water the accident such as not up to standard with cured body intensity, affect quality and the work-ing life of concrete works.Particularly along with the continuous deterioration of concrete raw material, this problem is more outstanding.
At present, the effective way solved the problem is admixture, and the suitable water conservation that has adjusts the thickening material of sticky effect to emanate the series of problems produced with the bleeding reducing polycarboxylate water-reducer susceptibility and bring.But the thickening material of the overwhelming majority, as: Mierocrystalline cellulose, welan gum, sodium alginate, polyvinyl alcohol, polyacrylamide, EVA rubber powder, sodium polyacrylate etc. all also exist inconsistent problem with polycarboxylate water-reducer, the air-entraining effect of above-mentioned thickening material, also can cause late strength of concrete on the low side simultaneously.
Summary of the invention
The object of this invention is to provide a kind of concrete viscosity conditioning agent and preparation method thereof, the concrete admixture consistencies such as described viscosity modifier and polycarboxylate water-reducer are good, and not bleed, significantly can improve concrete viscosity, effectively suppress concrete segregation bleeding.
For achieving the above object, the technical solution used in the present invention is: a kind of concrete viscosity conditioning agent, it is by cationic monomer, anionic carboxyl monomer and internal crosslinker by the free-radical polymerized amphiphilic polymers obtained, and the mol ratio of described cationic monomer, anionic monomer, internal crosslinker is 1:(0.5 ~ 5): (0.01 ~ 0.1).
According to such scheme, cationic monomer general structure is such as formula 1,
R in its Chinese style 1
1be selected from hydrogen, methyl, ethyl, propyl group; R
2be selected from methyl, ethyl, propyl group; R
3be selected from halogen.
According to such scheme, cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylyl oxy-ethyl triethyl ammonium chloride, acrylyl oxy-ethyl tripropyl ammonium chloride, methylacryoyloxyethyl triethyl ammonium chloride, methylacryoyloxyethyl tripropyl ammonium chloride, acrylyl oxy-ethyl-trimethyl brometo de amonio, acrylyl oxy-ethyl triethylammonium bromide, acrylyl oxy-ethyl tripropyl brometo de amonio, methylacryoyloxyethyl triethylammonium bromide, methylacryoyloxyethyl tripropyl brometo de amonio, with one or more in methylacryoyloxyethyl trimethylammonium bromide.
According to such scheme, described anionic carboxyl monomer is vinylformic acid, methacrylic acid, maleic acid, MALEIC ANHYDRIDE, FUMARIC ACID TECH GRADE and their monovalent base metal-salt, diatomic base metal-salt, one or more in ammonium salt mix in any proportion.
According to such scheme, for reducing polymeric reaction temperature, described anionic carboxyl monomer is preferably vinylformic acid and monovalent base metal-salt, ammonium salt; If be used alone maleic acid, MALEIC ANHYDRIDE or FUMARIC ACID TECH GRADE, or select the mixture of FUMARIC ACID TECH GRADE and maleic acid or MALEIC ANHYDRIDE, need suitable raising polymeric reaction temperature to reduce maleic acid, MALEIC ANHYDRIDE, fumaric monomer residue.
According to such scheme, described internal crosslinker is the linking agent containing two and two or more unsaturated double-bond, as: N, one or more in N'-methylene-bisacrylamide, N, N'-methylenebismethacrylamide, diallyldimethylammonium chloride, diallyl diethyl malonate, polyethyleneglycol diacrylate, polyethylene glycol dimethacrylate, glycerol tri-acrylate, glycerol trimethacrylate are by any proportioning mixing.Internal crosslinker is preferably the N containing two unsaturated double-bonds, N'-methylene-bisacrylamide, N, N'-methylenebismethacrylamide, diallyldimethylammonium chloride.
According to such scheme, described concrete viscosity conditioning agent amphiphilic polymers weight average molecular weight range is 600,000 ~ 5,000,000.Preferable weight-average molecular weight scope is the polymkeric substance of 800,000 ~ 2,000,000.
The preparation method of above-mentioned a kind of concrete viscosity conditioning agent, comprise the following steps: be 1:(0.5 ~ 5 in molar ratio by cationic monomer, anionic carboxyl monomer and internal crosslinker): (0.01 ~ 0.1) is dissolved in deionized water, under the condition of excluding air, add initiator initiated polymerization, temperature of reaction is 20 ~ 80 DEG C, reaction times is 2 ~ 5h, reaction terminates aqueous sodium hydroxide solution adjustment pH to 5 ~ 8 that rear concentration is 30wt%, obtains described solidifying native viscosity modifier.
According to such scheme, redox type initiator is made up of oxidant constituents and reductive agent component, oxidant constituents is described thermal decomposition initiating, reductive agent component is the mol ratio >1:1 of one or more in hydrosulphite, sulphite, xitix, thiosulfate, pyrosulfite and ferrous salt, oxidant constituents and reductive agent component.
When adopting described redox type initiator to carry out radical polymerization, free radical polymerization can be produced at a lower temperature, and discharge a large amount of heats along with the carrying out reacted and elevate the temperature, when temperature arrives the decomposition temperature of heat decomposition type initiator, the decomposition of second segment heat decomposition type initiator can be caused, make whole polyreaction more complete.
According to such scheme, the consumption of described initiator is 0.01 ~ 10wt% (accounting for the mass percent of cationic monomer and anionic monomer total mass), and preferable amount is 0.1 ~ 2wt%.
According to such scheme, described cationic monomer and anionic monomer are polymerized under aqueous conditions, and the concentration of cations in aqueous solution monomer and negatively charged ion is 5 ~ 50wt%, are preferably 10 ~ 30wt%.
According to such scheme, the solid content of obtained concrete viscosity conditioning agent is 10% ~ 30%.
Compared with prior art, the invention has the beneficial effects as follows:
(1) the present invention adopts cationic monomer, anionic carboxyl monomer and internal crosslinker by the free-radical polymerized amphiphilic polymers obtained, and this amphiphilic polymers has significantly anti-poly-electric matter character, shows good Efficient Adhesive Promotion; What add that internal crosslinker makes to obtain forms tridimensional network between viscosity modifier and cement granules simultaneously, significantly reduces concrete disintegration bleeding, improves concrete workability.
(2) the concrete admixture consistencies such as obtained concrete viscosity conditioning agent and polycarboxylate water-reducer are good, and not bleed, can significantly improve concrete workability.
(3) preparation method of the present invention is simple, and cost is low, and the raw material sources related to are wide, environmental friendliness.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
A kind of concrete viscosity conditioning agent, the monomer ratio related to is acrylyl oxy-ethyl-trimethyl salmiac, the mol ratio of vinylformic acid, N, N'-methylene-bisacrylamide is 1:0.5:0.01, and its preparation method comprises the following steps:
In the four-hole bottle being furnished with Dropping feeder, agitator, prolong, thermometer, nitrogen gatherer, add the deionized water of 300g, the acrylyl oxy-ethyl-trimethyl salmiac of 38.6g, the vinylformic acid of 7.2g, the N of 0.31g, N'-methylene-bisacrylamide, and stir until monomer all dissolves at 70 DEG C.Nitrogen is incorporated into the air in flask displacement flask.Then the ammonium persulphate of 0.46g is joined in flask, continuously stirring and keep flask interior temperature be 70 DEG C start polymerization.Isothermal reaction 4 hours, is cooled to 40 DEG C, is then aqueous sodium hydroxide solution regulator solution about the pH to 6 of 30wt% by concentration, obtains solid containing the concrete viscosity conditioning agent being about 13%.
The present embodiment products obtained therefrom concrete viscosity conditioning agent is that standard specimen adopts gel permeation chromatography to measure with polyoxyethylene glycol, and its weight-average molecular weight is 875700.
Embodiment 2
A kind of concrete viscosity conditioning agent, the mol ratio of the monomer propylene acyloxyethyl trimethyl ammonium chloride related to, vinylformic acid, N, N'-methylene-bisacrylamide is 1:1:0.02, and its preparation method comprises the following steps:
Acrylyl oxy-ethyl-trimethyl salmiac, vinylformic acid, N, N'-methylene-bisacrylamide is in the four-hole bottle being furnished with Dropping feeder, agitator, prolong, thermometer, nitrogen gatherer, add the deionized water of 300g, the acrylyl oxy-ethyl-trimethyl salmiac of 38.6g, the vinylformic acid of 14.4g, the N of 0.62g, N'-methylene-bisacrylamide, and stir until monomer all dissolves at 65 DEG C.Nitrogen is incorporated into the air in flask displacement flask.Then the ammonium persulphate of 0.84g is joined in flask, continuously stirring and keep flask interior temperature be 65 DEG C start polymerization.Isothermal reaction 4 hours, is cooled to 40 DEG C, is then aqueous sodium hydroxide solution regulator solution about the pH to 7 of 30wt% by concentration, obtains solid containing the concrete viscosity conditioning agent being about 15%.
The present embodiment products obtained therefrom concrete viscosity conditioning agent is that standard specimen adopts gel permeation chromatography to measure with polyoxyethylene glycol, and its weight-average molecular weight is 1257400.
Embodiment 3
A kind of concrete viscosity conditioning agent, the mol ratio of the monomer propylene acyloxyethyl trimethyl ammonium chloride related to, vinylformic acid, N, N'-methylene-bisacrylamide is 1:1:0.1, and its preparation method comprises the following steps:
In the four-hole bottle being furnished with Dropping feeder, agitator, prolong, thermometer, nitrogen gatherer, add the deionized water of 500g, the acrylyl oxy-ethyl-trimethyl salmiac of 38.6g, the vinylformic acid of 14.4g, the N of 3.1g, N'-methylene-bisacrylamide, and stir until monomer all dissolves at 60 DEG C.Nitrogen is incorporated into the air in flask displacement flask.Then the ammonium persulphate of 0.51g is joined in flask, continuously stirring and keep flask interior temperature be 60 DEG C start polymerization.Isothermal reaction 5 hours, is cooled to 40 DEG C, is then aqueous sodium hydroxide solution regulator solution about the pH to 7 of 30wt% by concentration, obtains solid containing the concrete viscosity conditioning agent being about 10%.
The present embodiment products obtained therefrom concrete viscosity conditioning agent is that standard specimen adopts gel permeation chromatography to measure with polyoxyethylene glycol, and its weight-average molecular weight is 4828300.
Embodiment 4
A kind of concrete viscosity conditioning agent, the mol ratio of the monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride related to, methacrylic acid, N, N'-methylene-bisacrylamide is 1:2:0.02, and its preparation method comprises the following steps:
In the four-hole bottle being furnished with Dropping feeder, agitator, prolong, thermometer, nitrogen gatherer, add the deionized water of 400g, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 41.6g, the methacrylic acid of 17.2g, the N of 0.62g, N'-methylene-bisacrylamide, and stir until monomer all dissolves at 62 DEG C.Nitrogen is incorporated into the air in flask displacement flask.Then the ammonium persulphate of 1.2g is joined in flask, continuously stirring and keep flask interior temperature be 62 DEG C start polymerization.Isothermal reaction 5 hours, is cooled to 40 DEG C, is then aqueous sodium hydroxide solution regulator solution about the pH to 8 of 30wt% by concentration, obtains solid containing the concrete viscosity conditioning agent being about 13%.
The present embodiment products obtained therefrom concrete viscosity conditioning agent is that standard specimen adopts gel permeation chromatography to measure with polyoxyethylene glycol, and its weight-average molecular weight is 1357200.
Embodiment 5
A kind of concrete viscosity conditioning agent, the mol ratio of the monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride related to, vinylformic acid, N, N'-methylene-bisacrylamide is 1:2:0.03, and its preparation method comprises the following steps:
In the four-hole bottle being furnished with Dropping feeder, agitator, prolong, thermometer, nitrogen gatherer, add the deionized water of 300g, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 20.8g, the vinylformic acid of 14.4g, the N of 0.46g, N'-methylene-bisacrylamide, and stir until monomer all dissolves at 62 DEG C.Nitrogen is incorporated into the air in flask displacement flask.Then the ammonium persulphate of 1.0g is joined in flask, in flask, monomer mixture that 28.9g is pre-formed is added (by by the vinylformic acid of 20.8g MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, 14.4g, the N of 0.46g by Dropping feeder, N'-methylene-bisacrylamide is mixed to form), above-mentioned monomer mixture was added dropwise to complete in 2 hours.After being added dropwise to complete, 62 DEG C of constant temperature stir 2 hours, are cooled to 40 DEG C, are then aqueous sodium hydroxide solution regulator solution about the pH to 7 of 30wt% by concentration, obtain solid containing the concrete viscosity conditioning agent being about 16%.
The present embodiment products obtained therefrom concrete viscosity conditioning agent is that standard specimen adopts gel permeation chromatography to measure with polyoxyethylene glycol, and its weight-average molecular weight is 2375400.
Embodiment 6
A kind of concrete viscosity conditioning agent, the mol ratio of the monomer MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride related to, vinylformic acid, N, N'-methylene-bisacrylamide is 1:5:0.02, and its preparation method comprises the following steps:
In the four-hole bottle being furnished with Dropping feeder, agitator, prolong, thermometer, nitrogen gatherer, add the deionized water of 300g, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 20.8g, the vinylformic acid of 36.0g, the N of 0.31g, N'-methylene-bisacrylamide, and stir until monomer all dissolves at 40 DEG C.Nitrogen is incorporated into the air in flask displacement flask.Then the oxygenant ammonium persulphate of 1.0g is joined in flask, in flask, add 20g reductant solution (being formed by being dissolved in 19.5g deionized water by 0.5g sodium bisulfite) with Dropping feeder and form redox initiation system.Above-mentioned reductive agent was added dropwise to complete in 3 hours.After being added dropwise to complete, continuing constant temperature at 40 DEG C and stir 2 hours, is then aqueous sodium hydroxide solution regulator solution about the pH to 7 of 30wt% by concentration, obtains solid containing the concrete viscosity conditioning agent being about 15%.
The present embodiment products obtained therefrom concrete viscosity conditioning agent is that standard specimen adopts gel permeation chromatography to measure with polyoxyethylene glycol, and its weight-average molecular weight is 3742800.
Embodiment 7
A kind of concrete viscosity conditioning agent, the mol ratio of the monomer propylene acyloxyethyl trimethyl ammonium chloride related to, MALEIC ANHYDRIDE, N, N'-methylenebismethacrylamide is 1:0.5:0.06, and its preparation method comprises the following steps:
In the four-hole bottle being furnished with Dropping feeder, agitator, prolong, thermometer, nitrogen gatherer, add the deionized water of 200g, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 20.8g, the MALEIC ANHYDRIDE of 4.9g, the N of 0.92g, N'-methylenebismethacrylamide, and stir until monomer all dissolves at 30 DEG C.Nitrogen is incorporated into the air in flask displacement flask.Then the oxygenant ammonium persulphate of 0.8g is joined in flask, cross Dropping feeder in flask, add 20g reductant solution (by 0.2g dissolution of ascorbic acid being formed in 19.8g deionized water) formation redox initiation system.Above-mentioned reductive agent was added dropwise to complete in 3 hours.After being added dropwise to complete, continuing 30 DEG C of constant temperature and stir 2 hours, is then aqueous sodium hydroxide solution regulator solution about the pH to 7 of 30wt% by concentration, obtains solid containing the concrete viscosity conditioning agent being about 10%.
The present embodiment products obtained therefrom concrete viscosity conditioning agent is that standard specimen adopts gel permeation chromatography to measure with polyoxyethylene glycol, and its weight-average molecular weight is 2267900.
Embodiment 8
A kind of concrete viscosity conditioning agent, the mol ratio of the monomer propylene acyloxyethyl trimethyl ammonium chloride related to, MALEIC ANHYDRIDE, diallyldimethylammonium chloride is 1:1:0.05, and its preparation method comprises the following steps:
In the four-hole bottle being furnished with Dropping feeder, agitator, prolong, thermometer, nitrogen gatherer, add the deionized water of 300g, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride of 41.6g, the MALEIC ANHYDRIDE of 19.6g, the diallyldimethylammonium chloride of 1.6g, and stir until monomer all dissolves at 45 DEG C.Nitrogen is incorporated into the air in flask displacement flask.Then the oxidant hydrogen peroxide of 1.2g is joined in flask, in flask, add 20g reductant solution (by 0.2g dissolution of ascorbic acid being formed in 19.8g deionized water) with Dropping feeder and form redox initiation system.Above-mentioned reductive agent was added dropwise to complete in 3 hours.After being added dropwise to complete, continuing 45 DEG C of constant temperature and stir 2 hours, is then aqueous sodium hydroxide solution regulator solution about the pH to 7 of 30wt% by concentration, obtains solid containing the concrete viscosity conditioning agent being about 17%.
The present embodiment products obtained therefrom concrete viscosity conditioning agent is that standard specimen adopts gel permeation chromatography to measure with polyoxyethylene glycol, and its weight-average molecular weight is 1964700.
Concrete viscosity conditioning agent obtained for the embodiment of the present invention 1 ~ 8 is applied to concrete, carry out mechanical property and pressured bleeding test, testing method is with reference to GB/T50080-2002 " normal concrete mix method for testing performance standard " and GB/T50081-2002 " standard for test methods of mechanical properties of ordinary concrete ", and test result is in table 1.
Described concrete is made up of gelling material, Yueyang river sand, coarse aggregate and water, and wherein gelling material content is 380kg/m
3(comprise cement and flyash, wherein cement consumption cement is 310kg/m
3, flyash 70kg/m
3, cement is the new PO 42.5R of China, and flyash is I level ash), Yueyang river sand content is 760kg/m
3(fineness modulus is 2.6), coarse aggregate content is 1110kg/m
3(being 5 ~ 30 continuous grading basalt), water-cement ratio is 0.41.
Table 1 concrete viscosity conditioning agent implementation result
Test result shows, the normal concrete pressured bleeding of adding Concrete viscosity modifier is not 72%, and the phenomenon of segregation bleeding has appearred in concrete after placing 20 minutes.And after mixing concrete viscosity conditioning agent, concrete pressure bleeding rate is 5 ~ 16%, show good Efficient Adhesive Promotion, workability is good, can ensure concrete smooth construction, does not affect concrete strength development simultaneously.
The each raw material that the present invention relates to and bound value thereof, interval value can realize the present invention, and lower limit value and the interval value of processing parameter of the present invention (as temperature, time etc.) can realize the present invention, do not enumerate embodiment at this.The above is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some improvement and conversion, these all belong to protection scope of the present invention.
Claims (10)
1. a concrete viscosity conditioning agent, it is with cationic monomer, anionic carboxyl monomer and internal crosslinker for polymerizable raw material forms, and the mol ratio of described cationic monomer, anionic monomer, internal crosslinker is 1:(0.5 ~ 5): (0.01 ~ 0.1).
2. concrete viscosity conditioning agent according to claim 1, is characterized in that described cationic monomer general structure is such as formula 1, R in its Chinese style 1
1be selected from hydrogen, methyl, ethyl, propyl group; R
2be selected from methyl, ethyl, propyl group; R
3be selected from halogen.
3. according to claim 1 or 2, cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylyl oxy-ethyl triethyl ammonium chloride, acrylyl oxy-ethyl tripropyl ammonium chloride, methylacryoyloxyethyl triethyl ammonium chloride, methylacryoyloxyethyl tripropyl ammonium chloride, acrylyl oxy-ethyl-trimethyl brometo de amonio, acrylyl oxy-ethyl triethylammonium bromide, acrylyl oxy-ethyl tripropyl brometo de amonio, methylacryoyloxyethyl triethylammonium bromide, one or more in methylacryoyloxyethyl tripropyl brometo de amonio and methylacryoyloxyethyl trimethylammonium bromide.
4. concrete viscosity conditioning agent according to claim 1, it is characterized in that, described anionic carboxyl monomer is one or more in vinylformic acid, methacrylic acid, maleic acid, MALEIC ANHYDRIDE, FUMARIC ACID TECH GRADE and their an alkali metal salt, ammonium salt.
5. concrete viscosity conditioning agent according to claim 1, it is characterized in that, described internal crosslinker contains two and two or more unsaturated double-bond, for N, one or more in N'-methylene-bisacrylamide, N, N'-methylenebismethacrylamide, diallyldimethylammonium chloride, diallyl diethyl malonate, polyethyleneglycol diacrylate, polyethylene glycol dimethacrylate, glycerol tri-acrylate and glycerol trimethacrylate.
6. a kind of concrete viscosity conditioning agent according to any one of Claims 1 to 5, is characterized in that, the weight-average molecular weight of described concrete viscosity conditioning agent is 600,000 ~ 5,000,000.
7. the preparation method of the concrete viscosity conditioning agent according to any one of Claims 1 to 5, it is characterized in that, comprise the following steps: be 1:(0.5 ~ 5 in molar ratio by cationic monomer, anionic carboxyl monomer and internal crosslinker): (0.01 ~ 0.1) is dissolved in deionized water, under the condition of excluding air, add initiator initiated polymerization, polymeric reaction temperature is 20 ~ 80 DEG C, time is 2 ~ 5h, finally add alkali lye and regulate pH to 5 ~ 8, obtain described concrete viscosity conditioning agent.
8. the preparation method of a kind of concrete viscosity conditioning agent according to claim 7, is characterized in that, described initiator is heat decomposition type initiator or redox type initiator.
9. the preparation method of a kind of concrete viscosity conditioning agent according to claim 8, is characterized in that, described heat decomposition type initiator is one or more in ammonium persulphate, Potassium Persulphate, Sodium Persulfate and hydrogen peroxide; Redox type initiator is made up of oxidant constituents and reductive agent component, oxidant constituents is described thermal decomposition initiating, reductive agent component is the mol ratio >1:1 of one or more in hydrosulphite, sulphite, xitix, thiosulfate, pyrosulfite and ferrous salt, oxidant constituents and reductive agent component.
10. want the preparation method of a kind of concrete viscosity conditioning agent described in 7 according to right, it is characterized in that, described initiators for polymerization consumption is 0.1 ~ 5% of cationic monomer and anionic monomer quality summation.
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| CN105601787A (en) * | 2015-12-24 | 2016-05-25 | 江苏苏博特新材料股份有限公司 | Method for preparing cement dispersant with both high water reduction effect and viscosity reduction effect |
| CN105837740A (en) * | 2016-04-01 | 2016-08-10 | 贵州铁建恒发新材料科技股份有限公司 | Concrete viscosity regulating agent and preparation method thereof |
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