CN112708050A - Concrete water reducing agent and preparation method thereof - Google Patents
Concrete water reducing agent and preparation method thereof Download PDFInfo
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- CN112708050A CN112708050A CN202010859783.4A CN202010859783A CN112708050A CN 112708050 A CN112708050 A CN 112708050A CN 202010859783 A CN202010859783 A CN 202010859783A CN 112708050 A CN112708050 A CN 112708050A
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- concrete water
- acid
- water reducer
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- -1 benzil alcohol ketone Chemical class 0.000 claims abstract description 49
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 30
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 30
- 239000000178 monomer Substances 0.000 claims abstract description 29
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 27
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 16
- 238000005886 esterification reaction Methods 0.000 claims abstract description 11
- 230000032050 esterification Effects 0.000 claims abstract description 10
- 239000000543 intermediate Substances 0.000 claims abstract description 9
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 29
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 17
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 14
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 14
- 239000011976 maleic acid Substances 0.000 claims description 14
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 7
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 claims description 7
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 4
- 239000001530 fumaric acid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 150000008064 anhydrides Chemical class 0.000 claims description 2
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 claims description 2
- 229940018557 citraconic acid Drugs 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 239000003112 inhibitor Substances 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims 3
- 238000006243 chemical reaction Methods 0.000 abstract description 24
- 239000002245 particle Substances 0.000 abstract description 7
- 239000004568 cement Substances 0.000 abstract description 6
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 125000000542 sulfonic acid group Chemical group 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000003111 delayed effect Effects 0.000 abstract description 2
- 238000006703 hydration reaction Methods 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 78
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 50
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 28
- 229910052753 mercury Inorganic materials 0.000 description 28
- 229910052757 nitrogen Inorganic materials 0.000 description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 26
- 239000011259 mixed solution Substances 0.000 description 26
- 229910001873 dinitrogen Inorganic materials 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 20
- 239000000243 solution Substances 0.000 description 17
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 16
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 14
- 239000002994 raw material Substances 0.000 description 14
- 238000001816 cooling Methods 0.000 description 13
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 13
- 230000003472 neutralizing effect Effects 0.000 description 13
- 238000010992 reflux Methods 0.000 description 13
- 238000003756 stirring Methods 0.000 description 13
- 239000003513 alkali Substances 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 12
- 238000007599 discharging Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 8
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 7
- 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 description 6
- 239000004927 clay Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000010276 construction Methods 0.000 description 5
- NLGDWWCZQDIASO-UHFFFAOYSA-N 2-hydroxy-1-(7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-yl)-2-phenylethanone Chemical compound OC(C(=O)c1cccc2Oc12)c1ccccc1 NLGDWWCZQDIASO-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 229920005646 polycarboxylate Polymers 0.000 description 4
- 230000000379 polymerizing effect Effects 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- VQIDGTFLGAAJGI-UHFFFAOYSA-M sodium;prop-1-ene-1-sulfonate Chemical compound [Na+].CC=CS([O-])(=O)=O VQIDGTFLGAAJGI-UHFFFAOYSA-M 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 238000013016 damping Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 239000008030 superplasticizer Substances 0.000 description 3
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 3
- PMNLUUOXGOOLSP-UHFFFAOYSA-N 2-mercaptopropanoic acid Chemical compound CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000012986 chain transfer agent Substances 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 2
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 1
- 229940006193 2-mercaptoethanesulfonic acid Drugs 0.000 description 1
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical compound FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- ZNEWHQLOPFWXOF-UHFFFAOYSA-N coenzyme M Chemical compound OS(=O)(=O)CCS ZNEWHQLOPFWXOF-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 description 1
- GRWZHXKQBITJKP-UHFFFAOYSA-N dithionous acid Chemical compound OS(=O)S(O)=O GRWZHXKQBITJKP-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- PJUIMOJAAPLTRJ-UHFFFAOYSA-N monothioglycerol Chemical compound OCC(O)CS PJUIMOJAAPLTRJ-UHFFFAOYSA-N 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- DJEHXEMURTVAOE-UHFFFAOYSA-M potassium bisulfite Chemical compound [K+].OS([O-])=O DJEHXEMURTVAOE-UHFFFAOYSA-M 0.000 description 1
- 229940099427 potassium bisulfite Drugs 0.000 description 1
- HEZHYQDYRPUXNJ-UHFFFAOYSA-L potassium dithionite Chemical compound [K+].[K+].[O-]S(=O)S([O-])=O HEZHYQDYRPUXNJ-UHFFFAOYSA-L 0.000 description 1
- 235000010259 potassium hydrogen sulphite Nutrition 0.000 description 1
- 229910001380 potassium hypophosphite Inorganic materials 0.000 description 1
- RWPGFSMJFRPDDP-UHFFFAOYSA-L potassium metabisulfite Chemical compound [K+].[K+].[O-]S(=O)S([O-])(=O)=O RWPGFSMJFRPDDP-UHFFFAOYSA-L 0.000 description 1
- 229940043349 potassium metabisulfite Drugs 0.000 description 1
- 235000010263 potassium metabisulphite Nutrition 0.000 description 1
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 description 1
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 1
- 235000019252 potassium sulphite Nutrition 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229940047670 sodium acrylate Drugs 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 229940035024 thioglycerol Drugs 0.000 description 1
- NJRXVEJTAYWCQJ-UHFFFAOYSA-N thiomalic acid Chemical compound OC(=O)CC(S)C(O)=O NJRXVEJTAYWCQJ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- 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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Abstract
The invention relates to the technical field of building additives, in particular to a concrete water reducing agent and a preparation method thereof, wherein the concrete water reducing agent comprises the following components: a photopolymerizable monomer selected from alkoxy polyethylene glycol esterification intermediates; the photoinitiator is benzil alcohol ketone. The concrete water reducer provided by the invention adopts the alkoxy polyethylene glycol esterification intermediate, so that both slump retaining performance and water reducing performance can be considered, meanwhile, the reaction can be carried out at normal temperature or low temperature, monomer prepolymerization is directly initiated through light irradiation, the polymerization rate is greatly improved, the synthesis conversion rate is improved, the sensitivity is reduced, in addition, the addition of the sulfonic acid group can stably adsorb the surface of the cement particles, the hydration reaction can be effectively delayed, the dispersion slump retaining effect in the concrete with medium and low strength grades is enhanced, and the concrete water reducer has extremely wide market application prospect.
Description
Technical Field
The invention relates to the technical field of building additives, in particular to a concrete water reducing agent and a preparation method thereof.
Background
The polycarboxylate superplasticizer serving as a new-generation high-performance water reducing agent has the advantages of low mixing amount, high water reducing rate, good slump retaining property, environmental friendliness and the like, is more and more widely applied to engineering, and cannot be used for the construction of railways, highways, dams, bridges, tunnels and high-rise buildings. Particularly, the rapid development of high-speed rail projects in China in recent years further pulls the industrial development of the polycarboxylate superplasticizer, and the application of the polycarboxylate superplasticizer also extends to the civil building industry, including urban buildings, residential buildings and the like.
In order to improve the production efficiency, the application number of 201610225940.X discloses a photoinitiation type polycarboxylate water reducer and a preparation method thereof, the publication date is 2016, 8, 3 and changes the prior art that the polymerization crosslinking and the grafting reaction are initiated by heat or adding a reducing agent as an exciting agent to react and ultraviolet photons are emitted by an ultraviolet lamp, so that the production efficiency is improved.
Although the polycarboxylic acid water reducing agent has many advantages in performance and is more and more widely applied to the concrete industry, with the increasing use amount, some problems still exist in the production and use of the water reducing agent, and are to be solved and improved, in particular, the following are:
due to the rapid development of the building industry in recent years, the use amount of raw materials is more and more, high-quality sandstone is increasingly exhausted as a limited resource, and the mud content of poor-quality sandstone and machine-made sand is larger. Researches show that the montmorillonite has great influence on the performance of the polycarboxylic acid water reducing agent, and can greatly reduce the water reducing rate and slump retaining property of the polycarboxylic acid water reducing agent, so that the concrete has poor fluidity and extremely fast slump loss;
the polycarboxylic acid water reducing agent has strong sensitivity to temperature, and particularly has great slump loss of concrete under high-temperature environment in summer, thereby greatly influencing the construction performance of the concrete, not only influencing the transportation and construction, but also having great influence on the quality of the concrete. And the slump retention of concrete is far from each other in different seasons.
Therefore, the application number 201611256665.4 entitled "multicomponent phosphate-based admixture for low-and-medium-slump concrete and preparation method thereof" discloses a multicomponent phosphate-based admixture for low-and-medium-slump concrete and preparation method thereof, wherein the multicomponent phosphate-based admixture is 2016, 11, 10 days, and long-time slump retaining of low-and-medium-slump concrete is realized by introducing phosphoric acid or phosphorous acid functional compounds.
Therefore, the development of the concrete water reducing agent which can be used in the ready-mixed commercial concrete and has a good slump retaining effect has very important significance.
Disclosure of Invention
In order to solve the problem of poor slump retaining property of the existing concrete mentioned in the background technology, the invention provides a concrete water reducing agent, which comprises the following components in percentage by weight:
a photopolymerizable monomer selected from alkoxy polyethylene glycol esterification intermediates;
the photoinitiator is benzil alcohol ketone.
On the basis of the scheme, further, the photopolymerizable monomer also comprises a sulfonate monomer.
On the basis of the scheme, the sulfonate monomer is sodium propylene sulfonate.
On the basis of the scheme, the weight ratio of the sulfonate monomer to the photoinitiator is (5-9): (9-11).
On the basis of the scheme, further, the photopolymerizable monomer comprises vinyl monomers.
On the basis of the scheme, the vinyl monomer is at least one of acrylic acid, methacrylic acid, crotonic acid, maleic acid, itaconic acid, citraconic acid, fumaric acid and monovalent metal salt, divalent metal salt, ammonium salt or anhydride thereof.
On the basis of the scheme, the weight ratio of the vinyl monomer to the photoinitiator is (25-35): (9-11).
On the basis of the scheme, the alkoxy polyethylene glycol esterification intermediate is further prepared by carrying out esterification reaction on alkoxy polyethylene glycol and unsaturated carboxylic acid in the presence of a polymerization inhibitor.
On the basis of the scheme, the structural formula of the alkoxy polyethylene glycol is as follows:
wherein n is 18-22, and R is-CH3or-CH2CH3。
In addition to the above embodiments, the unsaturated carboxylic acid is at least one of acrylic acid and methacrylic acid.
On the basis of the scheme, the weight ratio of the alkoxy polyethylene glycol to the unsaturated carboxylic acid is (260-290): (40-50).
The invention provides a preparation method of a concrete water reducing agent, which is obtained by photopolymerization of a photopolymerizable monomer in the presence of a photoinitiator, wherein the photopolymerizable monomer is selected from an alkoxy polyethylene glycol esterification intermediate, a vinyl monomer and a mixture thereof.
On the basis of the scheme, further, the photopolymerization reaction is carried out under the irradiation of ultraviolet light.
On the basis of the scheme, the wavelength of the ultraviolet light is 350-250 nm.
The invention also provides a preferable scheme of the preparation method of the concrete water reducing agent, which comprises the following preparation steps:
(1) adding 260-290 parts by weight of methoxypolyethylene glycol having a molecular weight of 1004-1220, 40-50 parts by weight of methacrylic acid and 0.3-0.45 part by weight of hydroquinone into a reaction vessel including a thermometer, a stirrer, a nitrogen inlet tube and a reflux cooling tube (condenser), raising the temperature to 105-115 ℃, carrying out nitrogen substitution, and carrying out nitrogen substitution for 4 hours at a flow rate of 400 ml/min. Reducing the temperature to 60 ℃, and stopping introducing nitrogen to obtain a mixed solution A;
(2) sequentially adding 3-7 parts by weight of a chain transfer agent, 25-35 parts by weight of an alkene monomer, 5-9 parts by weight of sodium propylene sulfonate and 9-11 parts by weight of a photoinitiator into the mixed solution A obtained in the step (1), stirring for 10-20 min, then turning on an ultraviolet high-pressure mercury lamp, adjusting the wavelength to 350-250 nm, polymerizing for 60-80 min, then turning off the ultraviolet high-pressure mercury lamp, preserving heat for 1-2 h at the temperature below 45 ℃ (preferably normal temperature of 2-35 ℃) for aging reaction, and then neutralizing with an alkaline solution until the pH value is 6.8-7.2 to obtain the ultraviolet high-pressure mercury lamp;
on the basis of the above scheme, further, the chain transfer agent is isopropanol, phosphorous acid and hypophosphorous acid and salts thereof (sodium hypophosphite, potassium hypophosphite, etc.), sulfurous acid, bisulfite, dithionous acid and metabisulfite and salts thereof (sodium sulfite, sodium bisulfite, preferably sodium dithionite, sodium metabisulfite, potassium sulfite, potassium bisulfite, potassium dithionite, potassium metabisulfite, etc.), mercaptoethanol, thioglycerol, thioglycolic acid, mercaptopropionic acid, 2-mercaptopropionic acid, 3-mercaptopropionic acid, thiomalic acid, 2-mercaptoethanesulfonic acid and salts thereof.
Compared with the prior art, the concrete water reducing agent provided by the invention has the following technical principles and beneficial effects:
according to the invention, the alkoxy polyethylene glycol esterification intermediate is adopted, so that both slump retaining performance and water reducing performance can be taken into consideration, monomer polymerization is directly initiated under illumination, a large number of free radicals can be generated in the early stage of photoinitiator benzil ketone in the photopolymerization process, so that the polymerization reaction can be carried out at normal temperature or low temperature, the polymerization rate and the synthesis conversion rate are greatly improved, the reaction temperature in the later stage is increased, the decomposition product of benzil ketone is taken as a small-molecule damping agent, and is quickly and stably adsorbed on the surface of clay particles, and the slump retaining performance is improved while the sensitivity is reduced;
moreover, in order to further improve the slump retaining property of the cement paste, the absolute value of the Zeta potential on the clay surface is improved by introducing sulfonic acid groups, so that the dispersibility of the water reducing agent to a paste system is improved, and meanwhile, the adjustable ultraviolet high-pressure mercury lamp is used for irradiating to directly initiate monomer prepolymerization, so that the polymerization rate is greatly improved, the synthesis conversion rate is improved, the sulfonic acid groups can stably adsorb the surface of cement particles, the hydration reaction is delayed, and the dispersing slump retaining effect in concrete is enhanced.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the following description will clearly and completely describe the embodiments of the present invention, and obviously, the described embodiments are a part of the embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples and comparative examples, the alkoxy polyethylene glycol is methoxy polyethylene glycol, the average molecular weight of the methoxy polyethylene glycol is 1004-1220, and the structural formula is as follows:
The invention also provides the following examples and comparative examples:
example 1
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 260 parts by weight of methoxypolyethylene glycol, 0.35 part by weight of hydroquinone, 42 parts by weight of methacrylic acid, 350 parts by weight of water, 3.7 parts by weight of thioglycolic acid, 26 parts by weight of acrylic acid, 9.8 parts by weight of benzil ketone and 5.5 parts by weight of sodium propylene sulfonate.
The preparation method comprises the following steps:
(1) adding 260 parts by weight of methoxy polyethylene glycol, 42 parts by weight of methacrylic acid and 0.35 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 105 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 350 parts by weight of water, 3.7 parts by weight of thioglycollic acid, 26 parts by weight of acrylic acid, 5.5 parts by weight of sodium propylene sulfonate and 9.8 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 280nm to carry out polymerization for 60 min;
and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Example 2
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 270 parts by weight of methoxypolyethylene glycol, 0.39 part by weight of hydroquinone, 45 parts by weight of methacrylic acid, 380 parts by weight of water, 3.1 parts by weight of mercaptoethanol, 28 parts by weight of itaconic acid, 10.3 parts by weight of benzil ketone and 6.4 parts by weight of sodium propene sulfonate.
The preparation method comprises the following steps:
(1) adding 270 parts by weight of methoxy polyethylene glycol, 45 parts by weight of methacrylic acid and 0.39 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 110 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 380 parts by weight of water, 3.1 parts by weight of mercaptoethanol, 28 parts by weight of itaconic acid, 6.4 parts by weight of sodium propylene sulfonate and 10.3 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 290nm to polymerize for 60 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Example 3
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 265 parts by weight of methoxypolyethylene glycol, 0.36 part by weight of hydroquinone, 49 parts by weight of methacrylic acid, 385 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 25 parts by weight of crotonic acid, 10.5 parts by weight of benzil ketone and 7 parts by weight of sodium propylene sulfonate.
The preparation method comprises the following steps:
(1) adding 265 parts by weight of methoxy polyethylene glycol, 49 parts by weight of methacrylic acid and 0.36 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 112 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 385 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 25 parts by weight of crotonic acid, 7 parts by weight of sodium propylene sulfonate and 10.5 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, adjusting the wavelength to 310nm, and polymerizing for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Example 4
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 270 parts by weight of methoxypolyethylene glycol, 0.4 part by weight of hydroquinone, 50 parts by weight of methacrylic acid, 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 10.7 parts by weight of benzil ketone and 8 parts by weight of sodium propene sulfonate.
The preparation method comprises the following steps:
(1) adding 270 parts by weight of methoxy polyethylene glycol, 50 parts by weight of methacrylic acid and 0.4 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 108 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 8 parts by weight of sodium propylene sulfonate and 10.7 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 320nm for polymerization for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Example 5
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 265 parts by weight of methoxypolyethylene glycol, 0.35 part by weight of hydroquinone, 45 parts by weight of methacrylic acid, 380 parts by weight of water, 6 parts by weight of sodium hypophosphite, 26 parts by weight of acrylic acid, 9.7 parts by weight of benzil ketone and 7 parts by weight of sodium propylene sulfonate.
The preparation method comprises the following steps:
(1) adding 265 parts by weight of methoxy polyethylene glycol, 45 parts by weight of methacrylic acid and 0.35 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 110 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 380 parts by weight of water, 6 parts by weight of sodium hypophosphite, 26 parts by weight of acrylic acid, 7 parts by weight of sodium propylene sulfonate and 9.7 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, adjusting the wavelength to 310nm, and polymerizing for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Example 6
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 260 parts by weight of methoxypolyethylene glycol, 0.31 part by weight of hydroquinone, 40 parts by weight of methacrylic acid, 365 parts by weight of water, 6.5 parts by weight of sodium hypophosphite, 28 parts by weight of crotonic acid, 9.9 parts by weight of benzil ketone and 8.5 parts by weight of sodium propylene sulfonate.
The preparation method comprises the following steps:
(1) adding 260 parts by weight of methoxy polyethylene glycol, 40 parts by weight of methacrylic acid and 0.31 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 112 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 365 parts by weight of water, 6.5 parts by weight of sodium hypophosphite, 28 parts by weight of crotonic acid, 8.5 parts by weight of sodium propylene sulfonate and 9.9 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, opening an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 310nm for polymerization for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Example 7
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 280 parts by weight of methoxypolyethylene glycol, 0.43 part by weight of hydroquinone, 49 parts by weight of methacrylic acid, 395 parts by weight of water, 6.4 parts by weight of thioglycolic acid, 28 parts by weight of fumaric acid, 10.9 parts by weight of benzil ketone and 8.6 parts by weight of sodium propylene sulfonate.
The preparation method comprises the following steps:
(1) adding 260 parts by weight of methoxy polyethylene glycol, 40 parts by weight of methacrylic acid and 0.31 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 112 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 365 parts by weight of water, 6.5 parts by weight of sodium hypophosphite, 28 parts by weight of crotonic acid, 8.5 parts by weight of sodium propylene sulfonate and 9.9 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, opening an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 310nm for polymerization for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Comparative example 1
A commercially available polycarboxylic acid water reducing agent of BRS-501 type is adopted.
Comparative example 2
A commercially available polycarboxylic acid water reducing agent of HX-601B type is used.
Comparative example 3
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 270 parts by weight of methoxypolyethylene glycol, 0.4 part by weight of hydroquinone, 50 parts by weight of methacrylic acid, 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 10.7 parts by weight of azobisisobutyronitrile and 8 parts by weight of sodium acrylate sulfonate.
The preparation method comprises the following steps:
(1) adding 270 parts by weight of methoxy polyethylene glycol, 50 parts by weight of methacrylic acid and 0.4 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 108 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 8 parts by weight of sodium propylene sulfonate and 10.7 parts by weight of azobisisobutyronitrile into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 320nm for polymerization for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Comparative example 4
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 270 parts by weight of methoxypolyethylene glycol, 0.4 part by weight of hydroquinone, 50 parts by weight of methacrylic acid, 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 5 parts by weight of benzil ketone and 8 parts by weight of sodium propene sulfonate.
The preparation method comprises the following steps:
(1) adding 270 parts by weight of methoxy polyethylene glycol, 50 parts by weight of methacrylic acid and 0.4 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 108 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 8 parts by weight of sodium propylene sulfonate and 5 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 320nm for polymerization for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Comparative example 5
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 270 parts by weight of methoxypolyethylene glycol, 0.4 part by weight of hydroquinone, 50 parts by weight of methacrylic acid, 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 12 parts by weight of benzil ketone and 8 parts by weight of sodium propene sulfonate.
The preparation method comprises the following steps:
(1) adding 270 parts by weight of methoxy polyethylene glycol, 50 parts by weight of methacrylic acid and 0.4 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 108 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 8 parts by weight of sodium propylene sulfonate and 12 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, then turning on an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 320nm to polymerize for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Comparative example 6
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 270 parts by weight of methoxypolyethylene glycol, 0.4 part by weight of hydroquinone, 50 parts by weight of methacrylic acid, 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid and 10.7 parts by weight of benzil ketone.
The preparation method comprises the following steps:
(1) adding 270 parts by weight of methoxy polyethylene glycol, 50 parts by weight of methacrylic acid and 0.4 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 108 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid and 10.7 parts by weight of benzil ketone into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, adjusting the wavelength to 320nm, and polymerizing for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
Comparative example 7
The concrete water reducing agent is prepared from the following raw materials in parts by weight: 270 parts by weight of methoxypolyethylene glycol, 0.4 part by weight of hydroquinone, 50 parts by weight of methacrylic acid, 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 10.7 parts by weight of benzoin ether and 8 parts by weight of sodium allylsulfonate.
The preparation method comprises the following steps:
(1) adding 270 parts by weight of methoxy polyethylene glycol, 50 parts by weight of methacrylic acid and 0.4 part by weight of hydroquinone into a reaction vessel comprising a thermometer, a stirrer, a nitrogen inlet pipe and a reflux cooling pipe (condenser), heating the temperature to 108 ℃, carrying out nitrogen replacement, carrying out nitrogen gas at a flow rate of 400ml/min for 4 hours, reducing the temperature to 60 ℃, and stopping introducing the nitrogen gas to obtain a mixed solution A;
(2) adding 390 parts by weight of water, 6 parts by weight of mercaptopropionic acid, 28 parts by weight of maleic acid, 8 parts by weight of sodium propylene sulfonate and 10.7 parts by weight of benzoin ether into the mixed solution A obtained in the step (1) in sequence, stirring for 10min, turning on an ultraviolet high-pressure mercury lamp, and adjusting the wavelength to 320nm for polymerization for 70 min;
(3) and (3) closing the ultraviolet high-pressure mercury lamp, preserving the heat at 35 ℃ for 1.5h for polymerization reaction, then neutralizing with an alkali solution until the pH value is 7.0, and discharging to obtain the catalyst.
It should be noted that the specific parameters or some common reagents in the above embodiments are specific examples or preferred embodiments of the present invention, and are not limited thereto; those skilled in the art can adapt the same within the spirit and scope of the present invention.
The concrete water reducing agents synthesized in the examples 1 to 7 and the comparative examples 3 to 7 and the commercially available polycarboxylic acid water reducing agents are subjected to comparative experiments, small south China sea P. O42.5R cement is adopted, machine-made mountain sand with the mud content of 2.2% and the fineness modulus of 3.1, and continuous graded broken stones with the nominal particle size of 5-10mm and 10-20mm and the mud content of 0.6% are taken as materials, and the concrete loss over time is tested according to the detection method provided by GB8076-2008 concrete admixture for 3 hours according to the mixing amounts of 0.15%, 0.2% and 0.25% of the cement mass.
The concrete formulation for the test is shown in table 1:
TABLE 1 concrete Components Table
| Raw materials | Cement | River sand | Machine-made sand | Small stone | Big stone | Tap water |
| Single dosage/kg | 320 | 200 | 558 | 340 | 797 | 160 |
The loss of each slump retaining agent over time at 3h as measured by the test is shown in Table 2:
TABLE 2 test results of examples and comparative examples
From the test data in the table above, it can be seen that:
under the condition of the same mixing amount, compared with a comparative example 1 and a comparative example 2, after the water reducing agent prepared by the invention is added, the concrete expansion degree is stably maintained within 460-580 mm within 180min, the slump loss resistance is excellent, normal construction within 3h of transport distance is met, and the comparative example has the obvious phenomenon of insufficient slump loss resistance time, so that the long-time transportation and pumping construction are not facilitated.
Compared with the comparative example 3, the photoinitiator is replaced by the azobisisobutyronitrile, the comparative example has the initial 5 water-reducing rate and the loss with time is poor, the photoinitiator is replaced by the azobisisobutyronitrile, and the decomposition product of the benzil ketone can not be generated to be used as the micromolecule damping agent, so that the aim of preferentially adsorbing on the surface of the clay particle and improving the slump retaining performance of the clay particle can not be achieved, and therefore, the initial time is small and the loss is large;
compared with comparative examples 4 and 5, the photoinitiator is out of 9-11 parts by weight, so that the conditions of low initial water reduction and poor loss with time occur, the reaction efficiency is low due to too little photoinitiator, and the reaction is severe due to too much photoinitiator, so that the initial time is small and the loss is large;
compared with the comparative example 6, the condition of poor time loss can be caused without using sodium propylene sulfonate, sulfonic acid groups are not introduced, the absolute value of Zeta potential on the clay surface is low, and the dispersibility of the water reducing agent to a slurry system is weaker, so the time loss is larger;
compared with the comparative example 7, the replacement of the photoinitiator with the benzoin ether causes low initial water reduction and poor loss by 15 hours, and the replacement of the photoinitiator with the benzoin ether causes too high and unstable reaction activity, so that the initial time is small and the loss is large;
moreover, different mixing amount (%) comparisons show that after the water reducer prepared by the invention is added, the mixing amounts are 1.5%, 2.0% and 2.5%, the influence of the initial water reducing rate is small, the concrete expansion degree is stably kept within 460-580 mm within 180min, the slump retaining performance is still excellent, the sensitivity to the mixing amount is low, and the decomposition product of the benzil ketone is taken as a small molecular damping agent and is quickly and stably adsorbed on the surface of clay particles, so that the sensitivity is reduced, and the slump retaining performance is improved.
As described above, the concrete water-reducing agent of the present invention can be effectively used as a high slump-retaining polycarboxylic acid water-reducing agent.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (14)
1. A water reducing agent for concrete, characterized in that it comprises:
a photopolymerizable monomer comprising an alkoxy polyethylene glycol esterification intermediate;
the photoinitiator is benzil alcohol ketone.
2. The concrete water reducer of claim 1, characterized in that: the photopolymerizable monomer includes a sulfonate monomer.
3. The concrete water reducer of claim 2, characterized in that: the sulfonate monomer is sodium propylene sulfonate.
4. The concrete water reducer of claim 2, characterized in that: the weight ratio of the sulfonate monomer to the photoinitiator is (5-9): (9-11).
5. The concrete water reducer of claim 1, characterized in that: the photopolymerizable monomers include vinyl monomers.
6. The concrete water reducer of claim 5, characterized in that: the alkene monomer is at least one of acrylic acid, methacrylic acid, crotonic acid, maleic acid, itaconic acid, citraconic acid, fumaric acid and monovalent metal salt, divalent metal salt, ammonium salt or anhydride thereof.
7. The concrete water reducer of claim 5, characterized in that: the weight ratio of the vinyl monomer to the photoinitiator is (25-35): (9-11).
8. The concrete water reducer according to claim 1, wherein the alkoxy polyethylene glycol esterification intermediate is prepared by esterification of alkoxy polyethylene glycol and unsaturated carboxylic acid in the presence of a polymerization inhibitor.
9. The concrete water reducer of claim 8, characterized in that: the structural formula of the alkoxy polyethylene glycol is as follows:
wherein n is 18-22, and R is-CH3or-CH2CH3。
10. The concrete water reducer of claim 8, characterized in that: the unsaturated carboxylic acid is at least one of acrylic acid and methacrylic acid.
11. The concrete water reducer according to claim 8, wherein the weight ratio of the alkoxy polyethylene glycol to the unsaturated carboxylic acid is (260-290): (40-50).
12. A preparation method of a concrete water reducing agent is obtained by photopolymerization of a photopolymerizable monomer in the presence of a photoinitiator, and is characterized in that: the photopolymerizable monomer is selected from alkoxy polyethylene glycol esterification intermediates, olefinic monomers, and mixtures thereof.
13. The preparation method of the concrete water reducer according to claim 12, characterized in that: the photopolymerization is carried out under ultraviolet irradiation.
14. The preparation method of the concrete water reducer according to claim 13, characterized in that: the wavelength of the ultraviolet light is 350-250 nm.
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