CN104231152A - Preparation method of concrete thickener - Google Patents
Preparation method of concrete thickener Download PDFInfo
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- CN104231152A CN104231152A CN201410529763.5A CN201410529763A CN104231152A CN 104231152 A CN104231152 A CN 104231152A CN 201410529763 A CN201410529763 A CN 201410529763A CN 104231152 A CN104231152 A CN 104231152A
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- Prior art keywords
- sodium
- concrete
- preparation
- minor comonomer
- unsaturated
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- 239000004567 concrete Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002562 thickening agent Substances 0.000 title abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000008346 aqueous phase Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 32
- 230000008719 thickening Effects 0.000 claims description 32
- -1 unsaturated acyl amine Chemical class 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 28
- 238000007334 copolymerization reaction Methods 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 8
- 150000003460 sulfonic acids Chemical class 0.000 claims description 8
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 7
- 239000004159 Potassium persulphate Substances 0.000 claims description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 7
- 235000019394 potassium persulphate Nutrition 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- 230000002829 reductive effect Effects 0.000 claims description 6
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 6
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 6
- 229960005055 sodium ascorbate Drugs 0.000 claims description 6
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 6
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 5
- XEEYSDHEOQHCDA-UHFFFAOYSA-N 2-methylprop-2-ene-1-sulfonic acid Chemical compound CC(=C)CS(O)(=O)=O XEEYSDHEOQHCDA-UHFFFAOYSA-N 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical group FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 claims description 4
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims description 4
- 239000004160 Ammonium persulphate Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 125000005336 allyloxy group Chemical group 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 claims description 4
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 claims description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 3
- 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 description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- SYGAXBISYRORDR-UHFFFAOYSA-N ethyl 2-(hydroxymethyl)prop-2-enoate Chemical class CCOC(=O)C(=C)CO SYGAXBISYRORDR-UHFFFAOYSA-N 0.000 claims description 3
- RFUCOAQWQVDBEU-UHFFFAOYSA-N methyl 2-(hydroxymethyl)prop-2-enoate Chemical class COC(=O)C(=C)CO RFUCOAQWQVDBEU-UHFFFAOYSA-N 0.000 claims description 3
- VLCAYQIMSMPEBW-UHFFFAOYSA-N methyl 3-hydroxy-2-methylidenebutanoate Chemical compound COC(=O)C(=C)C(C)O VLCAYQIMSMPEBW-UHFFFAOYSA-N 0.000 claims description 3
- RQAKESSLMFZVMC-UHFFFAOYSA-N n-ethenylacetamide Chemical compound CC(=O)NC=C RQAKESSLMFZVMC-UHFFFAOYSA-N 0.000 claims description 3
- ZQXSMRAEXCEDJD-UHFFFAOYSA-N n-ethenylformamide Chemical compound C=CNC=O ZQXSMRAEXCEDJD-UHFFFAOYSA-N 0.000 claims description 3
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 3
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 3
- KPGNTWPHBLZNCH-UHFFFAOYSA-N sodium;prop-2-en-1-olate Chemical compound [Na+].[O-]CC=C KPGNTWPHBLZNCH-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 claims description 2
- INWATCUTVADDFP-UHFFFAOYSA-N [K].OS(=O)(=O)C=CC1=CC=CC=C1 Chemical compound [K].OS(=O)(=O)C=CC1=CC=CC=C1 INWATCUTVADDFP-UHFFFAOYSA-N 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 125000003545 alkoxy group Chemical group 0.000 claims description 2
- 125000001118 alkylidene group Chemical group 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- NTXJYWXCKBIGFH-UHFFFAOYSA-N ethenesulfonic acid;potassium Chemical compound [K].OS(=O)(=O)C=C NTXJYWXCKBIGFH-UHFFFAOYSA-N 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 2
- 230000033116 oxidation-reduction process Effects 0.000 claims description 2
- 150000004968 peroxymonosulfuric acids Chemical group 0.000 claims description 2
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 229950000244 sulfanilic acid Drugs 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 abstract description 6
- 238000005204 segregation Methods 0.000 abstract description 5
- 238000010526 radical polymerization reaction Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000000178 monomer Substances 0.000 abstract 3
- 150000001408 amides Chemical class 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 18
- 239000007864 aqueous solution Substances 0.000 description 11
- 238000003756 stirring Methods 0.000 description 10
- 239000001913 cellulose Substances 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 6
- 230000000740 bleeding effect Effects 0.000 description 5
- 238000010276 construction Methods 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 229920002401 polyacrylamide Polymers 0.000 description 4
- 229920005646 polycarboxylate Polymers 0.000 description 3
- 239000004034 viscosity adjusting agent Substances 0.000 description 3
- CIWBSHSKHKDKBQ-DUZGATOHSA-N D-isoascorbic acid Chemical compound OC[C@@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-DUZGATOHSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- JPAOMENBKRZQDR-UHFFFAOYSA-N CC=CC.[Na] Chemical compound CC=CC.[Na] JPAOMENBKRZQDR-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229920002148 Gellan gum Polymers 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229920002310 Welan gum Polymers 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000000216 gellan gum Substances 0.000 description 1
- 235000010492 gellan gum Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- DOKHEARVIDLSFF-UHFFFAOYSA-N prop-1-en-1-ol Chemical group CC=CO DOKHEARVIDLSFF-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
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a preparation method of a concrete thickener. The preparation method of the concrete thickener comprises subjecting small unsaturated amide monomers, small unsaturated hydroxyl-ester monomers and small unsaturated sulfoacid monomers to aqueous phase radical polymerization under the combined action of a redox system composed of initiating agent and reducing agent to obtain polymerized products; adjusting the PH of the polymerized products to be 6-7; adding water into the polymerized water to obtain the concrete thickener at a concentration of 3-10wt%. According to the preparation method of the concrete thickener, the product performance can be adjusted by controlling the molecular weight of the polymerized products, so that high reaction velocity can be obtained, organic solvent can be omitted, and being non-toxic and pollution-free and simple in operation can be achieved. The concrete thickener prepared through the method can avoid segregation under the premise of achieving high water retention, thereby guaranteeing the slump resisting performance of concrete and achieving stable product performance.
Description
Technical field
The present invention relates to a kind of preparation method of concrete thickening material, be related specifically to a kind of concrete synthetic method adopting radical polymerization to prepare concrete thickening material.
Background technology
The reinforcement of concrete thickening material was succeeded in developing by West Germany at first in 1974, within 1977, was formally applied in engineering.Japan continues research equipment Imported From German EMH Company patent in 1978, and existing more than ten companies have developed more than ten and plant thickener products at present, and quantities reaches millions of square metres.1984, China's oil research institute successfully developed Propylene Series anti-dispersant, and name UWB type water-holding agent, is proposed again SCR Mierocrystalline cellulose series thickening material, finds application, obtain good social benefit and economic gain in multinomial heavy construction.
Thickening material chemically composition sees mainly polymeric admixture, is divided into several large classes such as polyacrylamide, cellulose family, polyacrylic and xanthan gum.High molecular thickening material needs less amount just can reach required viscosity, and most water-soluble high-molecular compound is not only used for thickening material, and is used for suspension agent, dispersion agent etc.Polyacrylamide mainly includes polyacrylamide, the multipolymer of acrylamide and the hydrolysate etc. of polyacrylamide.Mierocrystalline cellulose series is more, as methylcellulose gum, ethyl cellulose, Walocel MT 20.000PV, Natvosol, hydroxy propylene Mierocrystalline cellulose etc.They are all water-soluble powdery substances, and can be used to the viscosity improving aqueous phase, can alleviate segregation and the bleeding of concrete mix to a certain extent, reach the object of thickening, general consumption is no more than 0.5% of gelling material.
Viscosity modifier majority used at present both at home and abroad be can soluble high molecular polymer, and Mierocrystalline cellulose series, up-to-date achievement in research comprises Welland resin, namely welan gum, in addition gellan gum, determines excellent glue etc.Most viscosity modifier effectively can reduce bleeding on the one hand, concrete slump divergence is made again to reduce but then, water requirement increases, need to add more water reducer to maintain the required slump, and it is many and polycarboxylate water-reducer compatibleness is bad, difficulty of construction is increased, and its application receives obvious restriction.The viscosity modifier dissolution raties such as existing ether of cellulose are slow, expensive, and dissolution rate is slow, and while minimizing bleeding, cause the slump to reduce, difficulty of construction is increased, market receptance is low.
Summary of the invention
The object of the invention is the preparation method providing a kind of concrete thickening material in order to improve the deficiencies in the prior art, its segregation reducing agent again under the prerequisite of high water conservation, ensure that concrete slump retaining.
Technical scheme of the present invention is: a kind of preparation method of concrete thickening material, and its concrete steps are as follows:
1) by the oxidation-reduction system acting in conjunction that unsaturated acyl amine minor comonomer, unsaturated hydroxy ester class minor comonomer, unsaturated sulfonic acid class minor comonomer form at initiator and reductive agent, carry out 3 ~ 5 hours aqueous phase Raolical polymerizables under remaining on the temperature of 35 ~ 80 DEG C and obtain copolymerization product; The mass ratio of wherein said unsaturated acyl amine minor comonomer, unsaturated hydroxy ester class minor comonomer, unsaturated sulfonic acid class minor comonomer, initiator and reductive agent is 1:(0.1 ~ 2): (0.1 ~ 1): (0.03 ~ 0.2): (0.01 ~ 0.1);
2) with alkali lye by step 1) pH value that is obtained by reacting copolymerization product is adjusted to 6 ~ 7, add water and obtain the concrete thickening material that mass concentration is 3 ~ 10%.
Above-mentioned unsaturated acyl amine minor comonomer general formula R
1cONR
2r
3represent, wherein R
1be alkyl or the alkoxyl group of 2 ~ 6 carbon atoms, R
2, R
3be alkyl or the H of 1 ~ 4 carbon atom; Described unsaturated hydroxy ester class minor comonomer general formula R
4cOOR
5oH represents, wherein R
4, R
5be the ethylenic unsaturation alkyl of 1 ~ 4 carbon atom, alkylidene group or alkyl; Described unsaturated sulfonic acid class minor comonomer general formula R
6sO
3m represents, wherein R
6be the unsaturated olefin substrate of 3 ~ 8 carbon atoms, M is H, metal ion, ammonium or organic amino group.
Preferably above-mentioned unsaturated acyl amine minor comonomer is N-caprolactam, N, the one or more combination of N-DMAA, N, N-acrylamide, N-isopropylacrylamide, NVP, N-vinyl acetamide, N-vinyl formamide, N-methyl-Nvinylacetamide, N-alkyl acrylate or N-alkylmethacrylate, described unsaturated hydroxy ester class minor comonomer is the one or more combination of acrylate, Hydroxyethyl acrylate, the positive butyl ester of vinylformic acid hydroxyl, hydroxymethylacrylate methyl esters, hydroxymethylacrylate ethyl ester, hydroxyethyl methyl esters, hydroxyethyl methylacrylate, hydroxyethyl methacrylate n-propyl, described unsaturated sulfonic acid class minor comonomer is sodium allyl sulfonate, 2-acrylamide-2-methylpro panesulfonic acid (AMPS), Sodium styrene sulfonate, sodium vinyl sulfonate, methallylsulfonic acid sodium, methyl allyloxy sodium sulfonate, allyl sulphonic acid amine, styrene sulfonic acid amine, vinyl sulfonic acid amine, methallylsulfonic acid amine, methyl allyloxy sulfanilic acid, allyl sulphonic acid potassium, styrene sulfonic acid potassium, vinyl sulfonic acid potassium, the one or more combination of methallylsulfonic acid potassium or methyl allyloxy potassium sulfonate.
Preferably described initiator is persulfuric acid thing or superoxide.Preferably described initiator is one or more combinations of hydrogen peroxide, ammonium persulphate, Sodium Persulfate or Potassium Persulphate.Preferably described reductive agent is one or more combinations of sodium bisulfite, S-WAT, rongalite, sodium ascorbate, SODIUM ISOVITAMIN C or sodium hypophosphite.Preferably described alkali lye is one or more combinations of potassium hydroxide, sodium hydroxide or calcium hydroxide.
The present invention is in conjunction with concrete practical situation, synthesized agent for polyacrylic acid thickening, cellulose ethers thickening effectiveness can be reached, and can carry out composite with polycarboxylate water-reducer, when not affecting concrete slump, improve concrete bleeding, segregation phenomenon, greatly reduce difficulty of construction, and be conducive to preparing high slump concrete.
The inventive method adopts radical polymerization synthesis concrete thickening material, and technique is simple, and imparts the new function of thickening material, improves concrete education resistance, in turn ensure that concrete slump retaining.
Beneficial effect:
1. the abundant raw material source that utilizes of the inventive method.
2. the concrete thickener products prepared of the inventive method, can carry out composite with polycarboxylate water-reducer.
3. the concrete thickener products prepared of the inventive method, improves concrete bleeding, segregation phenomenon, in turn ensure that concrete slump retaining.
4. the concrete thickener products that prepared by the inventive method is made into stable performance after the aqueous solution, not stratified during storage, do not precipitate, and is convenient to transport.
5. the concrete thickener products prepared of the inventive method, reduces difficulty of construction greatly, and is conducive to preparing high slump concrete.
6. the inventive method is safe and reliable in the whole preparation process of concrete thickener products of preparation, operation steps is simple and convenient, not with an organic solvent, and nontoxic pollution-free, the advantage such as environmentally safe.
Embodiment
Below by embodiment, technical solution of the present invention is described in further detail.
Embodiment 1
N-caprolactam 10g, acrylate 20g and sodium allyl sulfonate 10g are added in reactor and stirs, then the aqueous solution containing 2g hydrogen peroxide and 0.3g sodium ascorbate is dripped respectively, keep temperature 35 DEG C, react after 3 hours, obtain copolymerization product; Regulate pH to 6 with sodium hydroxide solution, add water and obtain the concrete thickening material of 3wt% concentration.
Embodiment 2
N,N-DMAA 10g, Hydroxyethyl acrylate 1g and Sodium styrene sulfonate 1g are added in reactor, stirs, then the aqueous solution of liquid containing ammonium sulfate 0.3g and 0.1g S-WAT was dripped respectively, keep temperature 45 C, react after 4 hours, obtain copolymerization product; Regulate pH to 6 with potassium hydroxide solution, add water and obtain the concrete thickening material of 4wt% concentration.
Embodiment 3:
N, N-acrylamide 10g, hy-droxybutyl 10g and sodium vinyl sulfonate 5g are added in reactor, stirs, then the aqueous solution containing Potassium Persulphate 1g and 0.6g sodium bisulfite is dripped respectively, keep temperature 50 C, react after 4.5 hours, obtain copolymerization product; Regulate pH to 7 with sodium hydroxide solution, add water and obtain the concrete thickening material of 5wt% concentration.
Embodiment 4:
N-isopropylacrylamide 10g, hydroxymethylacrylate methyl esters 15g, Hydroxyethyl acrylate 5g and methylpropene sodium sulfonate 10g are added in reactor, stir, then the aqueous solution containing ammonium persulphate 0.85g and 0.5g sodium ascorbate is dripped respectively, keep temperature 55 DEG C, react after 5 hours, obtain copolymerization product; Regulate pH to 6 with sodium hydroxide and aqua calcis, add water and obtain the concrete thickening material of 6wt% concentration.
Embodiment 5:
NVP 10g, hydroxymethylacrylate ethyl ester 5g, the positive butyl ester 5g of vinylformic acid hydroxyl and 2-acrylamide-2-methylpro panesulfonic acid 5g are added in reactor, stir, then the aqueous solution containing Sodium Persulfate 0.11g, Potassium Persulphate 1.2g and 0.9g sodium ascorbate is dripped respectively, keep temperature 60 C, react after 3 hours, obtain copolymerization product; Regulate pH to 7 with sodium hydroxide and potassium hydroxide solution, add water and obtain the concrete thickening material of 7wt% concentration.
Embodiment 6:
N-vinyl acetamide 10g, hydroxyethyl methyl esters 10g and 2-acrylamide-2-methylpro panesulfonic acid 10g are added in reactor, stir, then drip the aqueous solution containing hydrogen peroxide 1.8g and 0.8g rongalite respectively, keep temperature 65 DEG C, react after 3.5 hours, obtain copolymerization product; Regulate pH to 7 with potassium hydroxide solution, add water and obtain the concrete thickening material of 8wt% concentration.
Embodiment 7:
N-vinyl formamide 10g, hydroxyethyl methylacrylate 16g and 2-acrylamide-2-methylpro panesulfonic acid 7g are added in reactor, stir, then the aqueous solution containing Potassium Persulphate 1.6g and 0.6g saccharosonic acid is dripped respectively, keep temperature 70 C, react after 4 hours, obtain copolymerization product; Regulate pH to 6 with sodium hydroxide solution, add water and obtain the concrete thickening material of 9wt% concentration.
Embodiment 8:
N-methyl-Nvinylacetamide 10g, hydroxyethyl methacrylate n-propyl 14g, methyl allyloxy sodium sulfonate 2g and 2-acrylamide-2-methylpro panesulfonic acid 8g are added in reactor, stir, then respectively containing the aqueous solution dripping ammonium persulphate 0.8g and 0.4g sodium hypophosphite, keep temperature 75 DEG C, react after 4.5 hours, obtain copolymerization product; Regulate pH to 6 with aqua calcis, add water and obtain the concrete thickening material of 10wt% concentration.
Embodiment 9:
N-alkyl acrylate 10g, Hydroxyethyl acrylate 10g, the positive butyl ester 5g of vinylformic acid hydroxyl, sodium vinyl sulfonate 5g, methallylsulfonic acid sodium 4g are added in reactor, stir, then the aqueous solution containing Potassium Persulphate 0.5g and 0.1g saccharosonic acid is dripped respectively, keep temperature 80 DEG C, react after 5 hours, obtain copolymerization product; Regulate pH to 7 with potassium hydroxide solution, add water and obtain the concrete thickening material of 5wt% concentration.
Embodiment 10:
N-alkylmethacrylate 10g, the positive butyl ester 8g of vinylformic acid hydroxyl, sodium allyl sulfonate 5g and Sodium styrene sulfonate 5g are added in reactor, stir, then the aqueous solution containing Potassium Persulphate 1.4g and 0.6g sodium ascorbate is dripped respectively, keep temperature 80 DEG C, react after 5 hours, obtain copolymerization product; Regulate pH to 6 with sodium hydroxide solution, add water and obtain the concrete thickening material of 6wt% concentration.
By FANN rotational viscosimeter (r
rotor=1.8415, r
stator=1.8415, h
stator=1.8415, d
circular clearance=1.8415, r
rotor=1.8415, instrument(al)constant K=300.0 (spring F1)) thickening effectiveness that embodiment 1 carries out cement paste to embodiment 10 gained sample is detected, select commercially available a kind of concrete thickening material methylcellulose gum to do reference.
The cement paste viscosity of the different sample of table 3
Testing concrete performance: to embodiment 10 gained sample, concrete strength inspection is carried out to embodiment 1 with reference to GB8076-2008 " concrete admixture ".The solid volume of admixture folding is 0.05g, as can be seen from following table, compare with blank the embodiment 1 that with the addition of admixture and arrive embodiment 10 gained sample 3 days, 7 days, within 28 days, ultimate compression strength is all greater than blank sample, illustrates that the thickening of this concrete thickening material does not affect concrete strength simultaneously.
The mechanical performance of concrete of the different sample of table 2
Claims (7)
1. a preparation method for concrete thickening material, its concrete steps are as follows:
1) by the oxidation-reduction system acting in conjunction that unsaturated acyl amine minor comonomer, unsaturated hydroxy ester class minor comonomer, unsaturated sulfonic acid class minor comonomer form at initiator and reductive agent, carry out 3 ~ 5 hours aqueous phase Raolical polymerizables under remaining on the temperature of 35 ~ 80 DEG C and obtain copolymerization product; The mass ratio of wherein said unsaturated acyl amine minor comonomer, unsaturated hydroxy ester class minor comonomer, unsaturated sulfonic acid class minor comonomer, initiator and reductive agent is 1:(0.1 ~ 2): (0.1 ~ 1): (0.03 ~ 0.2): (0.01 ~ 0.1);
2) with alkali lye by step 1) pH value that is obtained by reacting copolymerization product is adjusted to 6 ~ 7, add water and obtain the concrete thickening material that mass concentration is 3 ~ 10%.
2. preparation method according to claim 1, is characterized in that described unsaturated acyl amine minor comonomer general formula R
1cONR
2r
3represent, wherein R
1be alkyl or the alkoxyl group of 2 ~ 6 carbon atoms, R
2, R
3be alkyl or the H of 1 ~ 4 carbon atom; Described unsaturated hydroxy ester class minor comonomer general formula R
4cOOR
5oH represents, wherein R
4, R
5be the ethylenic unsaturation alkyl of 1 ~ 4 carbon atom, alkylidene group or alkyl; Described unsaturated sulfonic acid class minor comonomer general formula R
6sO
3m represents, wherein R
6be the unsaturated olefin substrate of 3 ~ 8 carbon atoms, M is H, metal ion, ammonium or organic amino group.
3. preparation method according to claim 1, it is characterized in that described unsaturated acyl amine minor comonomer is N-caprolactam, N, the one or more combination of N-DMAA, N, N-acrylamide, N-isopropylacrylamide, NVP, N-vinyl acetamide, N-vinyl formamide, N-methyl-Nvinylacetamide, N-alkyl acrylate or N-alkylmethacrylate, described unsaturated hydroxy ester class minor comonomer is the one or more combination of acrylate, Hydroxyethyl acrylate, the positive butyl ester of vinylformic acid hydroxyl, hydroxymethylacrylate methyl esters, hydroxymethylacrylate ethyl ester, hydroxyethyl methyl esters, hydroxyethyl methylacrylate, hydroxyethyl methacrylate n-propyl, described unsaturated sulfonic acid class minor comonomer is sodium allyl sulfonate, 2-acrylamide-2-methylpro panesulfonic acid, Sodium styrene sulfonate, sodium vinyl sulfonate, methallylsulfonic acid sodium, methyl allyloxy sodium sulfonate, allyl sulphonic acid amine, styrene sulfonic acid amine, vinyl sulfonic acid amine, methallylsulfonic acid amine, methyl allyloxy sulfanilic acid, allyl sulphonic acid potassium, styrene sulfonic acid potassium, vinyl sulfonic acid potassium, the one or more combination of methallylsulfonic acid potassium or methyl allyloxy potassium sulfonate.
4. preparation method according to claim 1, is characterized in that described initiator is persulfuric acid thing or superoxide.
5. preparation method according to claim 1, is characterized in that described initiator is one or more combinations of hydrogen peroxide, ammonium persulphate, Sodium Persulfate or Potassium Persulphate.
6. preparation method according to claim 1, is characterized in that described reductive agent is one or more combinations of sodium bisulfite, S-WAT, rongalite, sodium ascorbate, SODIUM ISOVITAMIN C or sodium hypophosphite.
7. preparation method according to claim 1, is characterized in that described alkali lye is one or more combinations of potassium hydroxide, sodium hydroxide or calcium hydroxide.
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