CN114292296A - Preparation method of anti-mud factor and anti-mud polycarboxylate superplasticizer - Google Patents
Preparation method of anti-mud factor and anti-mud polycarboxylate superplasticizer Download PDFInfo
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- CN114292296A CN114292296A CN202111571478.6A CN202111571478A CN114292296A CN 114292296 A CN114292296 A CN 114292296A CN 202111571478 A CN202111571478 A CN 202111571478A CN 114292296 A CN114292296 A CN 114292296A
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- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000008030 superplasticizer Substances 0.000 title claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 40
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 21
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 21
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- ULTHEAFYOOPTTB-UHFFFAOYSA-N 1,4-dibromobutane Chemical compound BrCCCCBr ULTHEAFYOOPTTB-UHFFFAOYSA-N 0.000 claims abstract description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 5
- -1 acrylic ester Chemical class 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 16
- 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 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- 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 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 9
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 9
- 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
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 7
- SLAONPBUWDUSSO-UHFFFAOYSA-N 2-[2-[2-[2-(4-methylphenyl)sulfonyloxyethoxy]ethoxy]ethoxy]ethyl 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)OCCOCCOCCOCCOS(=O)(=O)C1=CC=C(C)C=C1 SLAONPBUWDUSSO-UHFFFAOYSA-N 0.000 claims description 7
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 7
- 229930003268 Vitamin C Natural products 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 239000001488 sodium phosphate Substances 0.000 claims description 7
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 7
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 7
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 7
- 235000019154 vitamin C Nutrition 0.000 claims description 7
- 239000011718 vitamin C Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000001035 drying Methods 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 2
- DTWFIRNUMVLRHU-UHFFFAOYSA-N 2-methyldodecan-2-yl prop-2-enoate Chemical compound CCCCCCCCCCC(C)(C)OC(C=C)=O DTWFIRNUMVLRHU-UHFFFAOYSA-N 0.000 claims description 2
- BYDRTKVGBRTTIT-UHFFFAOYSA-N 2-methylprop-2-en-1-ol Chemical compound CC(=C)CO BYDRTKVGBRTTIT-UHFFFAOYSA-N 0.000 claims description 2
- RZVINYQDSSQUKO-UHFFFAOYSA-N 2-phenoxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC1=CC=CC=C1 RZVINYQDSSQUKO-UHFFFAOYSA-N 0.000 claims description 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- AOJOEFVRHOZDFN-UHFFFAOYSA-N benzyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC1=CC=CC=C1 AOJOEFVRHOZDFN-UHFFFAOYSA-N 0.000 claims description 2
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 2
- 125000001844 prenyl group Chemical group [H]C([*])([H])C([H])=C(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- WAYJYHNFFMNZJA-UHFFFAOYSA-M 3-[2-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-ylmethyl)-1,3-dioxolan-4-yl]-2,4-dimethylbenzenesulfonate Chemical compound CC1=CC=C(S([O-])(=O)=O)C(C)=C1C1OC(CN2N=CN=C2)(C=2C(=CC(Cl)=CC=2)Cl)OC1 WAYJYHNFFMNZJA-UHFFFAOYSA-M 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000005660 chlorination reaction Methods 0.000 abstract 1
- 238000007334 copolymerization reaction Methods 0.000 abstract 1
- 125000005496 phosphonium group Chemical group 0.000 abstract 1
- QVDTXNVYSHVCGW-ONEGZZNKSA-N isopentenol Chemical compound CC(C)\C=C\O QVDTXNVYSHVCGW-ONEGZZNKSA-N 0.000 description 5
- 238000011068 loading method Methods 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004927 clay Substances 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- WVYSWPBECUHBMJ-UHFFFAOYSA-N 2-methylprop-1-en-1-ol Chemical compound CC(C)=CO WVYSWPBECUHBMJ-UHFFFAOYSA-N 0.000 description 1
- WAYJYHNFFMNZJA-UHFFFAOYSA-N 3-[2-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-ylmethyl)-1,3-dioxolan-4-yl]-2,4-dimethylbenzenesulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C(C)=C1C1OC(CN2N=CN=C2)(C=2C(=CC(Cl)=CC=2)Cl)OC1 WAYJYHNFFMNZJA-UHFFFAOYSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram 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
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 238000005954 phosphonylation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention discloses a preparation method of a mud-resistant polycarboxylate water reducer, which is prepared in two steps, wherein in the first step, 1, 4-dibromobutane and triphenylphosphine are taken as raw materials, dissolved in organic solvents such as ethanol or acetonitrile and the like, and subjected to quaternary phosphonium chlorination reaction at the temperature of 60-80 ℃ to prepare a mud-resistant factor; and the second step is to take acrylic acid, polyoxyethylene ether macromonomer, acrylic ester, sulfonate and mud-resistant factor as main raw materials, and carry out free copolymerization reaction under the conditions of chain transfer agent and redox to obtain the polycarboxylic acid water reducing agent with good mud-resistant effect. The raw reducing material prepared by the method is cheap and easy to obtain, the reaction condition is mild, the synthesis step is simple and convenient, the post-treatment is easy, the slump loss resistance is good, the stability is good, the preparation process is simple, and the method is safe and environment-friendly and is suitable for mixing concrete with high mud content.
Description
Technical Field
The invention relates to the technical field of concrete admixtures and surfactants, in particular to a preparation method of a mud-resistant factor and mud-resistant polycarboxylic acid water reducer.
Background
The concrete admixture is a kind of chemical building material, and can change the physical and chemical properties of concrete, such as raising concrete strength, raising concrete workability, reducing water consumption and cement quantity, and can make concrete reach a new height in the directions of quality, workability, stability, durability, energy-saving and environment-protecting property, so that it can play the role of concrete process, and can be extensively used as new high-effective building material.
However, concrete admixtures are sensitive to the amount of mud in the aggregate, especially clay in the sand. Due to the fact that sand resources are deteriorated in recent years and the clay content in sand is high, the effect of the polycarboxylate superplasticizer in concrete application hardly meets the construction requirement, and even if the concrete meets the construction requirement, the cost of using the polycarboxylate superplasticizer in the concrete is greatly increased. Researches find that the montmorillonite in the clay has the largest negative effect on the water reducing agent, and the main measures adopted at present comprise washing aggregate, doping an excess water reducing agent and compounding an anti-mud external additive and the water reducing agent, wherein the washing aggregate can damage the aggregate structure and is not easy to realize in construction; the excessive water reducing agent is doped to cause concrete bleeding and segregation, and the slump and the strength of the concrete are negatively affected; the anti-mud external additive and the water reducing agent are compounded to achieve a certain anti-mud effect, but the effect is general.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the preparation method of the anti-mud factor and anti-mud polycarboxylic acid water reducer, and the prepared product has the characteristics of simple synthesis process, low cost of raw materials, long mud resistance time, good stability, simple preparation process, safety, environmental protection and the like, and is suitable for mixing concrete with higher mud content.
In order to achieve the purpose, the invention adopts the technical scheme that:
the preparation method of the anti-mud factor comprises the following steps:
1) preparing and weighing raw materials of each component;
2) putting 1, 4-dibromobutane, triphenylphosphine and an organic solvent into a three-neck flask provided with a stirring rod and a condenser tube, heating to 60-80 ℃, and reacting for 8-9 h to obtain a mixed solution I;
3) filtering the mixed solution I to remove redundant organic solvent to obtain an anti-mud factor crude product II;
4) and mixing and separating the crude product II of the anti-mud factor by using ethyl acetate, and filtering and drying to obtain the anti-mud factor.
Further, the mass ratio of the 1, 4-dibromobutane to the triphenylphosphine to the organic solvent is 1 (2-2.45): (1.5-1.85).
Further, the organic solvent is any one of acetonitrile, ethanol and methanol.
Further, the mass percentage of the anti-mud factor in the anti-mud polycarboxylic acid water reducer is 0.495-0.986%.
A preparation method of a mud-resistant polycarboxylate superplasticizer comprises the following steps:
1) preparing and weighing raw materials of each component;
2) putting the anti-mud factor, the polyoxyethylene ether macromonomer, the acrylate, the sulfonate, the chain transfer agent, the oxidant, the ammonium persulfate and the water into a four-neck flask with a stirrer, heating and stirring until the components are completely dissolved to obtain a first solution;
3) mixing acrylic acid and water, and stirring to obtain a second solution;
4) mixing a reducing agent and water, and stirring until the reducing agent and the water are completely dissolved to obtain a third solution;
5) slowly dripping the second solution and the third solution into the first solution under the stirring state of the first solution,
the dropping time is controlled to be 2.5 h-3 h, after the dropping is finished, 2-acrylamide-2-methylpropanesulfonic acid is added, the temperature is heated to 85 ℃ to 90 ℃, the stirring is continued for 2 h-3 h, and the pH value is adjusted to be 6.0-7.0 by using 1 percent trisodium phosphate aqueous solution to prepare the anti-mud polycarboxylic acid water reducer.
Further, the polyoxyethylene ether macromonomer is any one of prenyl polyoxyethylene ether TPEG, isobutenol polyoxyethylene ether HPEG and methallyl alcohol polyoxyethylene ether VPEG.
Further, the acrylate is one or more of 2-phenoxyethyl acrylate, lauryl methacrylate, dimethylaminoethyl methacrylate, 2-methyl-2-acrylic acid (2-dimethylamino) ethyl ester, 2-methyl-2-dodecyl acrylate, 2-methyl-2-methyl acrylate and benzyl methacrylate.
Further, the sulfonate is one or two of tetraethylene glycol di-p-toluenesulfonate and 3- [2- (2, 4-dichlorophenyl) -2- (1, 2, 4-triazole-1-ylmethyl) -1, 3-dioxolane-4-yl ] -2, 4-dimethylbenzenesulfonate.
Further, the chain transfer agent is one or more of thioglycolic acid, mercaptopropionic acid, isopropanol and sodium hypophosphite.
Furthermore, the oxidant is one or two of sodium persulfate and hydrogen peroxide, and the reducing agent is one or two of vitamin C, sodium hypophosphite and sodium bisulfite.
The invention has the following effects:
(1) the anti-mud factor is synthesized through the condensation reaction of the 1, 4-dibromobutane and triphenylphosphine, and the synthesized anti-mud factor is added into the water reducing agent, so that the water reducing agent has the advantages of low mixing amount, high water reducing rate, simple preparation process, safety, environmental protection, long anti-mud time, strong adaptability to various concrete materials and the like;
(2) the concrete performance comparison test is carried out on the anti-mud type polycarboxylate water reducer prepared by doping the anti-mud factors with different dosages, and the optimal dosage and the optimal anti-mud effect of the anti-mud factors are determined according to the test result, so that the application cost of the anti-mud type polycarboxylate water reducer is greatly reduced.
Drawings
FIG. 1 is a schematic structural diagram of an anti-mud factor.
Figure 2 is a synthetic scheme for anti-mud factor.
Detailed Description
The following examples are intended to illustrate the present invention in further detail, it being understood that the examples are given by way of illustration only and are not to be construed as limitations on the scope of the invention, as some insubstantial modifications and variations of the invention may be made by those skilled in the art in light of the above teachings.
Example 1:
the preparation method of the anti-mud factor of the embodiment is as follows:
1) adding 1, 4-dibromobutane (100 mmol, 21.4 g), triphenylphosphine (200 mmol, 52.4 g) and organic solvent absolute ethyl alcohol (50 ml, 39.5 g) into a three-neck flask provided with a stirring rod and a condensing tube, heating to 60-80 ℃, carrying out quaternary phosphonylation reaction for 8-9 h, and obtaining mixed solution I after the reaction is finished;
2) filtering the mixed solution I to remove redundant ethanol to obtain a crude product II;
3) and (3) separating out the crude product II by using ethyl acetate, and filtering and drying to obtain the diphosphorus cation anti-mud factor.
As shown in fig. 1 and fig. 2, in this embodiment, the anti-mud factor is synthesized through a condensation reaction between 1, 4-dibromobutane and triphenylphosphine, and after the synthesized anti-mud factor is added to the water reducing agent, the anti-mud effect of the water reducing agent can be obviously increased.
Example 2:
the preparation method of the anti-mud polycarboxylic acid water reducer comprises the following steps:
1) respectively putting 170.0g of methyl allyl polyoxyethylene ether, 170.0g of isopentenol polyoxyethylene ether, 125.0g of dimethylaminoethyl methacrylate, 32.5g of sodium hypophosphite, 10.8g of isopropanol, 65.0g of tetraethyleneglycol di-p-toluenesulfonate, 10.0g of H2O2 with the concentration of 30%, 10.0g of ammonium persulfate, 0g of the anti-mud factor in the embodiment 1 and 148.0g of water into a four-mouth flask, starting stirring, starting condensed water, and heating to 65-70 ℃ until all the substances are dissolved;
2) respectively dropwise adding a mixed solution containing 60.0g of acrylic acid and 44.6g of water and a mixed aqueous solution containing 2.35g of vitamin C and 131.4g of water into a four-neck flask, controlling the dropwise adding time to be 2.5-3 h, adding 24.5g of 2-acrylamide-2-methylpropanesulfonic acid after the dropwise adding is finished, heating to 85-90 ℃, continuously stirring for 2-3 h, and adjusting the pH to be 6.0-7.0 by using a 1% trisodium phosphate aqueous solution to prepare the anti-mud polycarboxylic acid water reducer LJ-I.
Example 3:
the preparation method of the anti-mud polycarboxylic acid water reducer comprises the following steps:
1) respectively loading 170.0g of methyl allyl polyoxyethylene ether, 170.0g of isopentenol polyoxyethylene ether, 125.0g of dimethylaminoethyl methacrylate, 32.5g of sodium hypophosphite, 10.8g of isopropanol, 65.0g of tetraethyleneglycol di-p-toluenesulfonate, 10.0g of H2O2 with the concentration of 30%, 10.0g of ammonium persulfate, 5.0g of the anti-mud factor in the embodiment 1 and 148.0g of water into a four-neck flask, starting stirring, starting condensed water, and heating to 65-70 ℃ until all the components are dissolved;
2) respectively dropwise adding a mixed solution containing 60.0g of acrylic acid and 44.6g of water and a mixed aqueous solution containing 2.35g of vitamin C and 131.4g of water into a four-neck flask, controlling the dropwise adding time to be 2.5-3 h, adding 24.5g of 2-acrylamide-2-methylpropanesulfonic acid after the dropwise adding is finished, heating to 85-90 ℃, continuously stirring for 2-3 h, and adjusting the pH to be 6.0-7.0 by using a 1% trisodium phosphate aqueous solution to prepare the anti-mud polycarboxylic acid water reducer LJ-II.
Example 4:
1) respectively loading 170.0g of methyl allyl polyoxyethylene ether, 170.0g of isopentenol polyoxyethylene ether, 125.0g of dimethylaminoethyl methacrylate, 32.5g of sodium hypophosphite, 10.8g of isopropanol, 65.0g of tetraethyleneglycol di-p-toluenesulfonate, 10.0g of H2O2 with the concentration of 30%, 10.0g of ammonium persulfate, 10.0g of the anti-mud factor in the embodiment 1 and 148.0g of water into a four-neck flask, starting stirring, starting condensed water, and heating to 65-70 ℃ until all the components are dissolved;
2) respectively dropwise adding a mixed solution containing 60.0g of acrylic acid and 44.6g of water and a mixed aqueous solution containing 2.35g of vitamin C and 131.4g of water into a four-neck flask, controlling the dropwise adding time to be 2.5-3 h, adding 24.5g of 2-acrylamide-2-methylpropanesulfonic acid after the dropwise adding is finished, heating to 85-90 ℃, continuously stirring for 2-3 h, and adjusting the pH to be 6.0-7.0 by using a 1% trisodium phosphate aqueous solution to prepare the anti-mud polycarboxylic acid water reducer LJ-III.
Example 5:
1) respectively loading 170.0g of methyl allyl polyoxyethylene ether, 170.0g of isopentenol polyoxyethylene ether, 125.0g of dimethylaminoethyl methacrylate, 32.5g of sodium hypophosphite, 10.8g of isopropanol, 65.0g of tetraethyleneglycol di-p-toluenesulfonate, 10.0g of H2O2 with the concentration of 30%, 10.0g of ammonium persulfate, 15.0g of the anti-mud factor in the embodiment 1 and 148.0g of water into a four-neck flask, starting stirring, starting condensed water, and heating to 65-70 ℃ until all the components are dissolved;
2) respectively dropwise adding a mixed solution containing 60.0g of acrylic acid and 44.6g of water and a mixed aqueous solution containing 2.35g of vitamin C and 131.4g of water into a four-neck flask, controlling the dropwise adding time to be 2.5-3 h, adding 24.5g of 2-acrylamide-2-methylpropanesulfonic acid after the dropwise adding is finished, heating to 85-90 ℃, continuously stirring for 2-3 h, and adjusting the pH to be 6.0-7.0 by using a 1% trisodium phosphate aqueous solution to prepare the anti-mud polycarboxylic acid water reducer LJ-IV.
Example 6:
1) respectively loading 170.0g of methyl allyl polyoxyethylene ether, 170.0g of isopentenol polyoxyethylene ether, 125.0g of dimethylaminoethyl methacrylate, 32.5g of sodium hypophosphite, 10.8g of isopropanol, 65.0g of tetraethyleneglycol di-p-toluenesulfonate, 10.0g of H2O2 with the concentration of 30%, 10.0g of ammonium persulfate, 20.0g of the anti-mud factor in the embodiment 1 and 148.0g of water into a four-neck flask, starting stirring, starting condensed water, and heating to 65-70 ℃ until all the components are dissolved;
2) respectively dropwise adding a mixed solution containing 60.0g of acrylic acid and 44.6g of water and a mixed aqueous solution containing 2.35g of vitamin C and 131.4g of water into a four-neck flask, controlling the dropwise adding time to be 2.5-3 h, adding 24.5g of 2-acrylamide-2-methylpropanesulfonic acid after the dropwise adding is finished, heating to 85-90 ℃, continuously stirring for 2-3 h, and adjusting the pH to be 6.0-7.0 by using a 1% trisodium phosphate aqueous solution to prepare the anti-mud polycarboxylic acid water reducer LJ-V.
Concrete performance comparison tests are carried out on the anti-mud polycarboxylic acid water reducing agent prepared in the plurality of examples according to GB 8076 and 2018 of concrete admixture, the concrete admixture is shown in Table 1, and the test results are shown in Table 2.
TABLE 1 concrete ratio
| Cement (kg/m)3） | Sand (kg/m)3） | Pebble (kg/m)3） | Water (kg/m)3） |
| 340 | 800 | 980 | 175 |
TABLE 2 concrete Properties of anti-sludging polycarboxylic acid water reducers incorporating the different examples
From table 2, it can be known that after the anti-mud factor is added, the anti-mud effect of the polycarboxylate superplasticizer is obviously improved on the whole, but the influence of different anti-mud factor dosages on the anti-mud effect of the polycarboxylate superplasticizer is different, when the anti-mud factor dosage is less than or equal to 10g, the slump and compressive strength ratio of concrete is increased along with the increase of the dosage of the anti-mud factor, when the anti-mud factor dosage is greater than 10g, the slump of concrete is reduced along with the increase of the dosage of the anti-mud factor, and the compressive strength ratio cannot be increased along with the increase of the dosage of the anti-mud factor, so that the optimal dosage of the anti-mud factor is about 10g, and the percentage of the optimal dosage of the anti-mud factor in the quality of the anti-mud polycarboxylate superplasticizer is about 0.986%.
The above description is only for the purpose of illustrating the present invention and should not be taken as limiting the scope of the present invention, i.e., the changes and modifications of the parameters made by reference to the present invention are all within the scope of the present invention.
Claims (10)
1. The preparation method of the anti-mud factor is characterized by comprising the following steps:
1) preparing and weighing raw materials of each component;
2) putting 1, 4-dibromobutane, triphenylphosphine and an organic solvent into a three-neck flask provided with a stirring rod and a condenser tube, heating to 60-80 ℃, and reacting for 8-9 h to obtain a mixed solution I;
3) filtering the mixed solution I to remove redundant organic solvent to obtain an anti-mud factor crude product II;
4) and mixing and separating the crude product II of the anti-mud factor by using ethyl acetate, and filtering and drying to obtain the anti-mud factor.
2. The method for preparing the mud-resisting factor according to claim 1, wherein the mass ratio of the 1, 4-dibromobutane to the triphenylphosphine to the organic solvent is 1 (2-2.45): (1.5-1.85).
3. The method for preparing an anti-mud factor according to claim 1 or 2, wherein the organic solvent is any one of acetonitrile, ethanol and methanol.
4. The preparation method of the anti-mud polycarboxylate superplasticizer is characterized by comprising the following steps:
1) preparing and weighing raw materials of each component;
2) respectively putting the anti-mud factor, the polyoxyethylene ether macromonomer, the acrylate, the sulfonate, the chain transfer agent, the oxidant, the ammonium persulfate and the water of any one of claims 1-3 into a four-neck flask provided with a stirrer and a condenser pipe, heating and stirring until the components are completely dissolved to obtain a first solution;
3) mixing acrylic acid and water, and stirring to obtain a second solution;
4) mixing a reducing agent and water, and stirring until the reducing agent and the water are completely dissolved to obtain a third solution;
5) and respectively and slowly dripping the second solution and the third solution into the first solution under the stirring state of the first solution, controlling the dripping time to be 2.5-3 h, adding 2-acrylamide-2-methylpropanesulfonic acid after the dripping is finished, heating to 85-90 ℃, continuously stirring for 2-3 h, and adjusting the pH value to be 6.0-7.0 by using a trisodium phosphate aqueous solution to prepare the anti-mud polycarboxylic acid water reducer.
5. The preparation method of the anti-mud type polycarboxylate water reducer as claimed in claim 4, wherein the mass percentage of the anti-mud factor in the anti-mud type polycarboxylate water reducer is 0.495-0.986%.
6. The method for preparing the mud-resistant polycarboxylate water reducer as claimed in claim 4 or 5, wherein the polyoxyethylene ether macromonomer is any one of prenyl polyoxyethylene ether TPEG, isobutenyl polyoxyethylene ether HPEG and methallyl alcohol polyoxyethylene ether VPEG.
7. The method for preparing the mud-resistant type polycarboxylate water reducer as claimed in claim 4 or 5, wherein the acrylate is one or more of 2-phenoxyethyl acrylate, lauryl methacrylate, dimethylaminoethyl methacrylate, 2-methyl-2-acrylic acid (2-dimethylamino) ethyl ester, 2-methyl-2-dodecyl acrylate, 2-methyl-2-acrylic acid methyl ester and benzyl methacrylate.
8. The method for preparing the anti-mud type polycarboxylate water reducer as claimed in claim 4 or 5, wherein the sulfonate is one or two of tetraethylene glycol di-p-toluenesulfonate and 3- [2- (2, 4-dichlorophenyl) -2- (1, 2, 4-triazol-1-ylmethyl) -1, 3-dioxolan-4-yl ] -2, 4-dimethylbenzenesulfonate.
9. The preparation method of the anti-mud type polycarboxylate water reducer as claimed in claim 4 or 5, wherein the chain transfer agent is one or more of thioglycolic acid, mercaptopropionic acid, isopropanol and sodium hypophosphite.
10. The method for preparing the anti-mud type polycarboxylate water reducer as claimed in claim 4 or 5, wherein the oxidant is one or two of sodium persulfate and hydrogen peroxide, and the reducing agent is one or two of vitamin C, sodium hypophosphite and sodium bisulfite.
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