CN111592627A - Viscosity reduction type water reducer and preparation method thereof - Google Patents
Viscosity reduction type water reducer and preparation method thereof Download PDFInfo
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- CN111592627A CN111592627A CN202010454184.4A CN202010454184A CN111592627A CN 111592627 A CN111592627 A CN 111592627A CN 202010454184 A CN202010454184 A CN 202010454184A CN 111592627 A CN111592627 A CN 111592627A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 32
- 230000009467 reduction Effects 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims description 11
- 239000000178 monomer Substances 0.000 claims abstract description 93
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 28
- 239000003999 initiator Substances 0.000 claims abstract description 23
- -1 hydroxybutyl vinyl Chemical group 0.000 claims abstract description 17
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 15
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 15
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 13
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000001603 reducing effect Effects 0.000 claims abstract description 11
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- NXBXJOWBDCQIHF-UHFFFAOYSA-N 2-[hydroxy-[2-(2-methylprop-2-enoyloxy)ethoxy]phosphoryl]oxyethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOP(O)(=O)OCCOC(=O)C(C)=C NXBXJOWBDCQIHF-UHFFFAOYSA-N 0.000 claims abstract description 8
- SEILKFZTLVMHRR-UHFFFAOYSA-N 2-phosphonooxyethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOP(O)(O)=O SEILKFZTLVMHRR-UHFFFAOYSA-N 0.000 claims abstract description 8
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims abstract description 6
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims abstract description 5
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 5
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims abstract description 5
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims abstract description 5
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims abstract description 5
- 239000011976 maleic acid Substances 0.000 claims abstract description 5
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 37
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- 229920000151 polyglycol Polymers 0.000 claims description 15
- 239000010695 polyglycol Substances 0.000 claims description 15
- 238000006116 polymerization reaction Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 239000011790 ferrous sulphate Substances 0.000 claims description 10
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 10
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 10
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002202 Polyethylene glycol Substances 0.000 abstract description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 abstract description 5
- 229920001223 polyethylene glycol Polymers 0.000 abstract description 5
- 239000004567 concrete Substances 0.000 description 19
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- 239000002253 acid Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000010276 construction Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 239000004568 cement Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000011372 high-strength concrete Substances 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 125000004185 ester group Chemical group 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method 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
- 239000012028 Fenton's reagent Substances 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 229940017705 formaldehyde sulfoxylate Drugs 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- SBGKURINHGJRFN-UHFFFAOYSA-N hydroxymethanesulfinic acid Chemical compound OCS(O)=O SBGKURINHGJRFN-UHFFFAOYSA-N 0.000 description 1
- 238000012994 industrial processing Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- XONPDZSGENTBNJ-UHFFFAOYSA-N molecular hydrogen;sodium Chemical compound [Na].[H][H] XONPDZSGENTBNJ-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012546 transfer Methods 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
- C04B24/24—Macromolecular compounds
- C04B24/243—Phosphorus-containing polymers
- C04B24/246—Phosphorus-containing polymers 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
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The viscosity reduction type water reducer comprises the following components in parts by weight: 25-45 parts of a monomer A, 3-5 parts of a monomer B, 2-4 parts of a monomer C, 0.1-0.3 part of a chain transfer agent, 0.4-1 part of an initiator and 50-60 parts of water, wherein the monomer A is any one or more of methyl alkenyl polyoxyethylene ether, isobutylene polyoxyethylene ether, hydroxybutyl vinyl polyethylene glycol ether, ethoxy vinyl polyethylene glycol ether and allyl polyethylene glycol ether, the monomer B is any one or more of acrylic acid, maleic acid and itaconic acid, the monomer C is any one or more of methacryloyloxyethyl phosphate, di (methacryloyloxyethyl) hydrogen phosphate and hydroxyethyl methacrylate, the initiator is a composition of an oxidizing component and a reducing component, and the chain transfer agent is any one or more of mercaptopropionic acid, thioglycolic acid and mercaptoethanol. The water reducer disclosed by the invention can release free water to the maximum extent by reducing the combination with water, increase the water-gel ratio, and has the advantages of obvious viscosity reduction effect and wide adaptability.
Description
Technical Field
The invention relates to the field of building materials, and particularly relates to a viscosity-reducing water reducer and a preparation method thereof.
Background
With the rapid development of the building industry, modern buildings tend to be high-rise, light-weighted and large-span, and high-strength concrete is widely applied to national infrastructure due to the characteristics of high strength, good integrity, small self weight and the like. In order to make the concrete reach high strength or ultrahigh strength grade, a large amount of cementing materials and a low water-cement ratio are needed, so that the problems of high viscosity and low flowing speed of fresh concrete are caused, the construction difficulty is high, particularly the problem of high viscosity of ultrahigh-strength concrete is particularly serious in pumping construction in China, and engineering accidents are caused frequently.
At present, the viscosity reduction method of high-strength concrete mainly adopts the steps of increasing the mixing amount of a water reducing agent and optimizing the grain composition by adopting high-quality superfine powder. The viscosity reduction method has the advantages that the cost is increased on the first aspect, the excessive slow-setting effect is caused on the second aspect, the formwork removal period is prolonged, the problems of bleeding, bottom scraping and the like of newly mixed concrete on the third aspect occur, and certain difficulty is caused to construction.
Therefore, how to reduce the viscosity of high-strength concrete with low cost and high efficiency is an urgent problem to be solved by those skilled in the art.
Disclosure of Invention
One of the purposes of the invention is to provide a viscosity-reducing type water reducer aiming at the defects of the prior art, which can release free water to the maximum extent by reducing the combination with water, increase the water-to-gel ratio, and has obvious viscosity reducing effect and wide adaptability.
The invention also aims to provide the preparation method of the viscosity-reducing water reducer, which has the advantages of simple and convenient preparation process and mild process parameters and is suitable for industrial processing production.
The technical scheme for realizing one purpose of the invention is as follows: the viscosity reduction type water reducer comprises the following components in parts by weight:
25 to 45 portions of monomer A, 3 to 5 portions of monomer B, 2 to 4 portions of monomer C, 0.1 to 0.3 portion of chain transfer agent, 0.4 to 1 portion of initiator and 50 to 60 portions of water,
the monomer A is any one or more of methyl alkenyl polyoxyethylene ether, isobutylene polyoxyethylene ether, hydroxybutyl vinyl polyglycol ether, ethoxy vinyl polyglycol ether and allyl polyglycol ether, the monomer B is any one or more of acrylic acid, maleic acid and itaconic acid, the monomer C is any one or more of methacryloyloxyethyl phosphate, di (methacryloyloxyethyl) hydrogen phosphate and hydroxyethyl methacrylate, the initiator is a composition of an oxidation component and a reduction component, and the chain transfer agent is any one or more of mercaptopropionic acid, mercaptoacetic acid and mercaptoethanol.
The invention also provides another viscosity reduction type water reducer which comprises the following components in parts by weight:
25 to 45 portions of monomer A, 3 to 5 portions of monomer B, 2 to 4 portions of monomer C, 0.1 to 0.3 portion of chain transfer agent, 0.4 to 1 portion of initiator and 50 to 60 portions of water,
the monomer A is any one or more of methyl alkenyl polyoxyethylene ether, isobutylene polyoxyethylene ether, hydroxybutyl vinyl polyglycol ether, ethoxy vinyl polyglycol ether and allyl polyglycol ether, the monomer B is any one or more of acrylic acid, maleic acid and itaconic acid, the monomer C is any one or more of methacryloyloxyethyl phosphate, di (methacryloyloxyethyl) hydrogen phosphate and hydroxyethyl methacrylate, the initiator is azobisisobutyramidine hydrochloride and/or ammonium persulfate, and the chain transfer agent is any one or more of mercaptopropionic acid, thioglycolic acid and mercaptoethanol.
Further, the viscosity reduction type water reducer comprises the following components in parts by weight:
28 to 38 portions of monomer A, 3 to 4.5 portions of monomer B, 2 to 3.1 portions of monomer C, 0.1 to 0.2 portion of chain transfer agent, 0.4 to 0.6 portion of initiator and 55 to 60 portions of water,
preferably, the composition comprises the following components in parts by weight:
35 parts of monomer A, 3.5 parts of monomer B, 3 parts of monomer C, 0.2 part of chain transfer agent, 0.4 part of initiator and 57.9 parts of water
Preferably, the polymerization degree of the monomer A is 30 to 60.
Further, the oxidizing component is hydrogen peroxide, the reducing component is a mixture of VC and/or ferrous sulfate and sodium formaldehyde sulfoxylate, the hydrogen peroxide is a 30 wt% aqueous solution, and the mass ratio of the hydrogen peroxide to the ferrous sulfate to the sodium formaldehyde sulfoxylate is 1: 0.1: 0.4.
the second technical scheme for realizing the aim of the invention is as follows: the preparation method of the viscosity-reducing water reducer comprises the following steps:
1) taking materials according to a proportion;
2) dissolving 2/3 monomer B and monomer C in partial water to obtain monomer solution;
3) dissolving a chain transfer agent and a reducing component in part of water to obtain a chain transfer agent solution;
4) dissolving the monomer A in the rest water, heating to 20-50 ℃, adding the oxidation component, stirring, adding the rest 1/3 monomer B, then synchronously dropwise adding the monomer solution and the chain transfer agent solution until the reaction is finished, adjusting the pH value to 6-8, and discharging to obtain the product.
The preparation method of the viscosity reduction type water reducer comprises the following steps:
1) taking materials according to a proportion;
2) dissolving 2/3 monomer B, monomer C and chain transfer agent in part of water to obtain monomer solution;
3) dissolving an initiator in part of water to obtain an initiator solution;
4) dissolving the monomer A in the rest water, heating to 20-50 ℃, dropwise adding the initiator solution, stirring, adding the rest 1/3 monomer B, dropwise adding the monomer solution till the reaction is finished, adjusting the pH value to 6-9, and discharging to obtain the product.
Preferably, step 4) is heated to 20-40 ℃.
Preferably, the dropping time of the monomer solution in the step 4) is 0.5-3.5 h.
Preferably, after the monomer solution in the step 4) is dripped, the reaction is carried out for 0.5 to 3 hours under the condition of heat preservation till the reaction is finished, and preferably, the reaction is carried out for 0.5 to 2 hours under the condition of heat preservation till the reaction is finished.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the unsaturated small monomer containing phosphate group is introduced into the functional group of the viscosity-reducing water reducer, so that the viscosity-reducing water reducer has stronger adsorption and dispersion effects, can be quickly dispersed and adsorbed in concrete, and simultaneously has stronger adsorption capacity, so that the thickness of the adsorption layer of polycarboxylic acid molecules on the surface of cement particles can be increased, and more free water is released; the small monomer for preparing the water reducing agent contains methyl and ester groups which are two hydrophobic groups, so that the HLB value of polycarboxylic acid molecules can be effectively reduced, the generation of combined water by the polycarboxylic acid molecules and water is reduced, and free water is further released; by reducing the combination with water, the free water is released to the maximum extent, the water-gel ratio of a concrete system can be effectively increased, and the viscosity reduction effect is obvious.
2. In the invention, the monomer A is polymerized with the monomer C and the monomer B to form the polycarboxylic acid water reducer under the action of an initiator or an initiating system, and the polycarboxylic acid water reducer has steric hindrance effect in premixed concrete to endow the polycarboxylic acid with water reducing and dispersing functions; by controlling the polymerization temperature to be 20-50 ℃, the energy consumption can be effectively reduced on the premise of meeting the normal reaction, if the process temperature is higher than 50 ℃, polyether degradation can be caused to influence the reaction process, and if the process temperature is lower than 20 ℃, the monomer activity is insufficient, so that the polymerization degree of a side chain is reduced; VC or ferrous sulfate, sodium formaldehyde sulfoxylate and hydrogen peroxide form a redox initiation system, azodiisobutyl amidine hydrochloride or ammonium persulfate is a self-decomposition initiation system, and the initiation system excites free radicals to carry out reaction; mercaptopropionic acid, mercaptoacetic acid and mercaptoethanol are chain transfer agents to control the molecular weight of the target polymer; the monomer B contains one or more carboxyl groups, so that polycarboxylic acid molecules are adsorbed to cement particles; the monomer C is a functional monomer, the HLB value of the polycarboxylic acid molecule can be effectively reduced by methyl and ester groups in the molecular structure of the monomer C, the adsorption capacity of the polycarboxylic acid molecule can be effectively improved by phosphate groups, and the viscosity reduction function of the polycarboxylic acid is endowed under the synergistic effect of all functional groups.
3. In the preparation process, part of the monomer B is preferentially dripped to reduce the influence of a polymerization inhibitor doped by a manufacturer in the macromonomer A on the polymerization reaction; after the monomer A is completely dissolved, the mixture of hydrogen peroxide and ferrous sulfate is added, and a Fenton reagent is formed by the hydrogen peroxide and the ferrous sulfate, so that the oxidizing capability of an oxidizing agent of a redox system can be improved, the generation speed of free radicals can be increased, and the reaction conditions of low reaction temperature and short reaction time can be adapted.
4. The applicant tests and verifies that compared with the concrete added with the conventional water reducing agent on the market, the concrete added with the viscosity-reducing water reducing agent has greatly reduced viscosity, the cylinder pouring time is shortened to 31.8 percent of that of the concrete added with the conventional water reducing agent on the market, and the requirement of concrete pumping construction can be effectively met.
The following description will be further described with reference to specific embodiments.
Detailed Description
In the present invention, the polyether of the company such as aoke, Shanghai Dongke, etc. in Liaoning, and the small monomer of the company such as Lanzhou petrochemical, refined chemical, giant special chemical, etc. are used for the experiment.
Example 1
27g of acrylic acid and 30g of hydrogen phosphate di (methacryloyloxyethyl) ester are dissolved in 40g of deionized water and are uniformly stirred to obtain a monomer solution for later use; dissolving 2g of mercaptopropionic acid and 1.06g of sodium formaldehyde sulfoxylate in 59.2g of deionized water, and uniformly stirring to obtain a chain transfer agent solution for later use; 200g of methyl alkenyl polyoxyethylene ether with the polymerization degree of 54 and the molecular weight of 2400, 150g of hydroxybutyl vinyl polyethylene glycol ether with the polymerization degree of 56 and the molecular weight of 2400 and 120g of deionized water are put into a reaction vessel to be heated and dissolved, after the methyl alkenyl polyoxyethylene ether, the hydroxybutyl vinyl polyethylene glycol ether and the deionized water are completely dissolved and the temperature reaches 20 ℃, a mixed solution of 2.67g of hydrogen peroxide and 0.27g of ferrous sulfate is added, the mixture is stirred for 5min under heat preservation, 14g of acrylic acid is then added, after 5min, the monomer solution and the chain transfer agent solution are dropwise added at a constant speed, the reaction is continued for 1h after 0.5h, after the reaction is finished, the sodium hydroxide aqueous solution is added to adjust the pH value of.
Example 2
Dissolving 35g of acrylic acid and 20g of methacryloyloxyethyl phosphate in 42g of deionized water, and uniformly stirring to obtain a monomer solution for later use; dissolving 1g of mercaptopropionic acid and 2.66g of sodium hydrogen formaldehyde sulfoxylate in 60g of deionized water, and uniformly stirring to obtain a chain transfer agent solution for later use; adding 200g of ethoxyvinyl polyglycol ether with the polymerization degree of 60 and the molecular weight of 3000, 160g of isobutenol polyoxyethylene ether with the polymerization degree of 60 and the molecular weight of 3000 and 120g of deionized water into a reaction container, heating for dissolving, adding a mixed solution of 2.66g of hydrogen peroxide and 0.26g of ferrous sulfate after the materials are completely dissolved and the temperature reaches 25 ℃, keeping the temperature and stirring for 3min, then adding 20g of acrylic acid, dropwise adding a monomer solution and a chain transfer agent solution at a constant speed after 5min, finishing dropping for 0.45h, continuing to keep the temperature and react for 1.5h, adding a sodium hydroxide solution after the reaction is finished, adjusting the pH value of the system to 7.6, and discharging to obtain the product.
Example 3
20g of acrylic acid, 12g of hydrogen phosphate di (methacryloyloxyethyl) ester and 12g of methacryloyloxyethyl phosphate are dissolved in 350g of deionized water and are uniformly stirred to obtain a monomer solution for later use; dissolving 3g of mercaptopropionic acid, 3.2g of sodium formaldehyde sulfoxylate and 0.8g of ferrous sulfate in 50g of deionized water, and uniformly stirring to obtain a chain transfer agent solution for later use; putting 220g of hydroxybutyl vinyl polyglycol ether with the polymerization degree of 34 and the molecular weight of 2000, 230g of ethoxyl vinyl polyglycol ether with the polymerization degree of 60 and the molecular weight of 3000 and 100g of deionized water into a reaction vessel, heating for dissolving, adding 4g of hydrogen peroxide solution and keeping the temperature and stirring for 6min after the materials are completely dissolved and the temperature reaches 20 ℃, then adding 12g of acrylic acid, beginning to dropwise add the monomer solution and the chain transfer agent solution at a constant speed after 5min, finishing dropping for 1h, continuing to keep the temperature and react for 1.5h, adding the potassium hydroxide solution after the reaction is finished, adjusting the pH value of the system to 7.2, and discharging to obtain the product.
Example 4
Dissolving 25g of acrylic acid, 10g of di (methacryloyloxyethyl) hydrogen phosphate, 15g of methacryloyloxyethyl phosphate and 3g of mercaptopropionic acid in 350g of deionized water, and uniformly stirring to obtain a monomer solution for later use; dissolving 7g of azodiisobutyramidine hydrochloride and 1g of ammonium persulfate in 50g of deionized water, and uniformly stirring to obtain an initiator solution for later use; 220g of methyl alkenyl polyoxyethylene ether with the polymerization degree of 34 and the molecular weight of 2000, 230g of methyl methacrylate polyoxyethylene ether with the polymerization degree of 60 and the molecular weight of 3000 and 100g of deionized water are put into a reaction vessel for heating and dissolving, after complete dissolution and the temperature reaches 50 ℃, initiator solution is dropwise added at a constant speed for 3.3h, 12g of acrylic acid is added after stirring for 6min under heat preservation, monomer solution is dropwise added at a constant speed after 5min, 3h of dropwise addition is completed, then heat preservation reaction is continued for 1.5h, potassium hydroxide aqueous solution is added after the reaction is completed to adjust the pH value of the system to 7.0, and the product is obtained after discharging.
The application example is as follows:
the influence of the polycarboxylate water reducer on fresh concrete is determined by referring to related regulations JC 473-: cement 440, fly ash 30, sand 666, large stone 888, small stone 296 and water 132. The results of the experiment are shown in table 1.
Table 1 results of performance testing
As can be seen from Table 1, in the case that the mixing amount of the concrete in the examples 1 to 4 is the same as that of the common water reducing agent sold in the market, the performance (slump and expansion) of the concrete is slightly higher than the comparison ratio; the cylinder pouring time of the concrete in the embodiments 1-4 is obviously shortened compared with that of the concrete in the comparative example, which shows that the viscosity of the concrete doped with the viscosity-reducing water reducer disclosed by the patent application is greatly reduced, and the concrete can effectively meet the requirement of concrete pumping construction. In addition, the gas contents of the examples 1 to 4 are not obviously improved compared with the comparative example, which shows that the viscosity reduction type water reducing agent of the invention does not cause the problem of excessive gas contents on the premise of high water reduction and high viscosity reduction.
Claims (10)
1. The viscosity reduction type water reducer is characterized by comprising the following components in parts by weight:
25 to 45 portions of monomer A, 3 to 5 portions of monomer B, 2 to 4 portions of monomer C, 0.1 to 0.3 portion of chain transfer agent, 0.4 to 1 portion of initiator and 50 to 60 portions of water,
the monomer A is any one or more of methyl alkenyl polyoxyethylene ether, isobutylene polyoxyethylene ether, hydroxybutyl vinyl polyglycol ether, ethoxy vinyl polyglycol ether and allyl polyglycol ether, the monomer B is any one or more of acrylic acid, maleic acid and itaconic acid, the monomer C is any one or more of methacryloyloxyethyl phosphate, di (methacryloyloxyethyl) hydrogen phosphate and hydroxyethyl methacrylate, the initiator is a composition of an oxidizing component and a reducing component, and the chain transfer agent is any one or more of mercaptopropionic acid, mercaptoacetic acid and mercaptoethanol.
2. The viscosity reduction type water reducer is characterized by comprising the following components in parts by weight:
25 to 45 portions of monomer A, 3 to 5 portions of monomer B, 2 to 4 portions of monomer C, 0.1 to 0.3 portion of chain transfer agent, 0.4 to 1 portion of initiator and 50 to 60 portions of water,
the monomer A is any one or more of methyl alkenyl polyoxyethylene ether, isobutylene polyoxyethylene ether, hydroxybutyl vinyl polyglycol ether, ethoxy vinyl polyglycol ether and allyl polyglycol ether, the monomer B is any one or more of acrylic acid, maleic acid and itaconic acid, the monomer C is any one or more of methacryloyloxyethyl phosphate, di (methacryloyloxyethyl) hydrogen phosphate and hydroxyethyl methacrylate, the initiator is azodiisobutyl amidine hydrochloride and/or ammonium persulfate, and the chain transfer agent is any one or more of mercaptopropionic acid, mercaptoacetic acid and mercaptoethanol.
3. The viscosity-reducing water reducer according to claim 1 or 2, characterized by comprising the following components in parts by weight:
28-38 parts of monomer A, 3-4.5 parts of monomer B, 2-3.1 parts of monomer C, 0.1-0.2 part of chain transfer agent, 0.4-0.6 part of initiator and 55-60 parts of water,
preferably, the composition comprises the following components in parts by weight:
35 parts of monomer A, 3.5 parts of monomer B, 3 parts of monomer C, 0.2 part of chain transfer agent, 0.4 part of initiator and 57.9 parts of water.
4. The viscosity-reducing water reducer according to claim 1 or 2, wherein the degree of polymerization of the monomer A is 30-60.
5. The viscosity reduction type water reducer according to claim 1, wherein the oxidizing component is hydrogen peroxide, the reducing component is a mixture of VC and/or ferrous sulfate and sodium formaldehyde sulfoxylate, the hydrogen peroxide is a 30 wt% aqueous solution, and the mass ratio of the hydrogen peroxide to the ferrous sulfate to the sodium formaldehyde sulfoxylate is 1: 0.1: 0.4.
6. the preparation method of the viscosity reduction type water reducer of claim 1 is characterized by comprising the following steps:
1) taking materials according to a proportion;
2) dissolving 2/3 monomer B and monomer C in partial water to obtain monomer solution;
3) dissolving a chain transfer agent and a reducing component in part of water to obtain a chain transfer agent solution;
4) dissolving the monomer A in the rest water, heating to 20-50 ℃, adding the oxidation component, stirring, adding the rest 1/3 monomer B, then synchronously dropwise adding the monomer solution and the chain transfer agent solution until the reaction is finished, adjusting the pH value to 6-8, and discharging to obtain the product.
7. The preparation method of the viscosity reduction type water reducer of claim 2 is characterized by comprising the following steps:
1) taking materials according to a proportion;
2) dissolving 2/3 monomer B, monomer C and chain transfer agent in part of water to obtain monomer solution;
3) dissolving an initiator in part of water to obtain an initiator solution;
4) dissolving the monomer A in the rest water, heating to 20-50 ℃, dropwise adding an initiator solution, stirring, adding the rest 1/3 monomer B, dropwise adding a monomer solution till the reaction is finished, adjusting the pH value to 6-9, and discharging to obtain the product.
8. The method according to claim 6 or 7, wherein the heating in step 4) is carried out at 20 to 40 ℃.
9. The production method according to claim 6 or 7, wherein the dropping time of the monomer solution in the step 4) is 0.5 to 3.5 hours.
10. The preparation method according to claim 6 or 7, wherein after the monomer solution is added dropwise in the step 4), the reaction is carried out for 0.5 to 3 hours until the reaction is finished, preferably for 0.5 to 2 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113087433A (en) * | 2021-03-26 | 2021-07-09 | 唐山冀东水泥外加剂有限责任公司 | Viscosity-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN113583194A (en) * | 2021-08-27 | 2021-11-02 | 中铁建设集团建筑发展有限公司 | Concrete performance regulator and preparation method thereof |
| CN113880998A (en) * | 2021-09-30 | 2022-01-04 | 重庆三圣实业股份有限公司 | Anti-mud polycarboxylate superplasticizer and preparation method thereof |
| CN113980206A (en) * | 2021-12-10 | 2022-01-28 | 南京师范大学 | Preparation method of anti-mud slow-release polycarboxylate superplasticizer |
| CN114195954A (en) * | 2021-12-17 | 2022-03-18 | 广州泰祥实业新材料科技（新丰）有限公司 | Surfactant, regulator for improving strength and workability of concrete and preparation process |
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| CN103275280A (en) * | 2013-06-17 | 2013-09-04 | 武汉东彭科技发展有限公司 | Synthetic method for polycarboxylate type high slump-retaining water reducing agent at normal temperature |
| CN104261719A (en) * | 2014-08-06 | 2015-01-07 | 中交武汉港湾工程设计研究院有限公司 | High-performance polycarboxylate water reducing agent and preparation method thereof |
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| CN103275280A (en) * | 2013-06-17 | 2013-09-04 | 武汉东彭科技发展有限公司 | Synthetic method for polycarboxylate type high slump-retaining water reducing agent at normal temperature |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113087433A (en) * | 2021-03-26 | 2021-07-09 | 唐山冀东水泥外加剂有限责任公司 | Viscosity-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN113583194A (en) * | 2021-08-27 | 2021-11-02 | 中铁建设集团建筑发展有限公司 | Concrete performance regulator and preparation method thereof |
| CN113583194B (en) * | 2021-08-27 | 2024-01-16 | 中铁建设集团建筑发展有限公司 | Concrete performance regulator and preparation method thereof |
| CN113880998A (en) * | 2021-09-30 | 2022-01-04 | 重庆三圣实业股份有限公司 | Anti-mud polycarboxylate superplasticizer and preparation method thereof |
| CN113980206A (en) * | 2021-12-10 | 2022-01-28 | 南京师范大学 | Preparation method of anti-mud slow-release polycarboxylate superplasticizer |
| CN114195954A (en) * | 2021-12-17 | 2022-03-18 | 广州泰祥实业新材料科技（新丰）有限公司 | Surfactant, regulator for improving strength and workability of concrete and preparation process |
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Application publication date: 20200828 |