CN113292687A - High-performance slump-retaining polycarboxylate superplasticizer and preparation method thereof - Google Patents
High-performance slump-retaining polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
- Publication number
- CN113292687A CN113292687A CN202110726401.5A CN202110726401A CN113292687A CN 113292687 A CN113292687 A CN 113292687A CN 202110726401 A CN202110726401 A CN 202110726401A CN 113292687 A CN113292687 A CN 113292687A
- Authority
- CN
- China
- Prior art keywords
- unsaturated
- solution
- slump
- water reducer
- retaining
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000008030 superplasticizer Substances 0.000 title claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 122
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 99
- 239000000178 monomer Substances 0.000 claims abstract description 68
- 239000008367 deionised water Substances 0.000 claims abstract description 49
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 49
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 37
- 229920000570 polyether Polymers 0.000 claims abstract description 37
- 239000002253 acid Substances 0.000 claims abstract description 31
- 150000002148 esters Chemical class 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000007800 oxidant agent Substances 0.000 claims abstract description 17
- 230000001590 oxidative effect Effects 0.000 claims abstract description 17
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 114
- 238000005303 weighing Methods 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 239000012295 chemical reaction liquid Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000006386 neutralization reaction Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- -1 hydroxypropyl Chemical group 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 4
- 150000008065 acid anhydrides Chemical class 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims description 2
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-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
- 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 2
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 2
- 230000002572 peristaltic effect Effects 0.000 claims description 2
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 2
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 2
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 9
- 230000000740 bleeding effect Effects 0.000 abstract description 7
- 238000005204 segregation Methods 0.000 abstract description 6
- 125000004185 ester group Chemical group 0.000 abstract description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract 1
- 229920006337 unsaturated polyester resin Polymers 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 20
- 239000003795 chemical substances by application Substances 0.000 description 20
- 238000012546 transfer Methods 0.000 description 20
- 239000004568 cement Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 18
- 239000004615 ingredient Substances 0.000 description 11
- 230000002194 synthesizing effect Effects 0.000 description 11
- 239000003513 alkali Substances 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 10
- 239000007858 starting material Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 6
- 238000010276 construction Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000007634 remodeling Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Images
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
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers 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
Abstract
The invention discloses a high-performance slump retaining type polycarboxylic acid water reducing agent and a preparation method thereof, and solves the technical problems that the water reducing agent in the prior art is high in production cost, short in slump retaining time, easy to separate bleeding and high in engineering problem risk. The high-performance slump-retaining type polycarboxylate water reducer comprises a high-performance slump-retaining type polycarboxylate water reducer and a preparation method of the water reducer, wherein the molecular weight of the water reducer is 20000-50000, ester groups are introduced, and a molecular structure of the water reducer also has functional groups such as ether bonds, hydroxyl groups, ester groups and the like, and the formula of the water reducer comprises the following steps: the low-temperature-resistant unsaturated polyester resin comprises a saturated small monomer, an unsaturated polyether macromonomer, a chain transfer agent, an oxidant, a reducing agent, an unsaturated ester monomer and deionized water. Compared with the commercial water reducer, the water reducer prepared by the invention has good slump retaining effect, can effectively control the segregation and bleeding phenomenon and the slump loss phenomenon at the initial stage of concrete mixing, and has higher market potential.
Description
Technical Field
The invention relates to a slump-retaining water reducer, and particularly relates to a high-performance slump-retaining polycarboxylic acid water reducer and a preparation method thereof.
Background
With the rapid development of concrete technology, the application of concrete in roads, bridges, dams, civil buildings and other aspects is becoming more extensive, and the demand of concrete for both national projects and civil projects is rising year by year. Because of the great difference of concrete raw materials, the phenomenon of too fast concrete slump loss can often occur in the concrete transportation and construction process, and the difficulty is increased for concrete construction and quality control.
In the construction process, the most common treatment mode is to add water into the concrete for remodeling, so that the technical problem that the slump loss of the concrete is too fast is solved, the concrete has good fluidity again, and pumping and pouring in construction are facilitated, but the water addition for remodeling can change the water-cement ratio and the air content of the concrete, reduce the impermeability of the concrete, and seriously influence the strength of the concrete.
In addition, the concrete can also recover better working performance by increasing the using amount of the water reducing agent in the concrete or remolding the concrete by adding or reducing the water reducing agent before construction, but the phenomena of segregation, bleeding and the like of the concrete can be caused by increasing the using amount of the water reducing agent in the initial stirring stage, the uniformity of the concrete is damaged, the strength of each part of the concrete has larger difference, and the compressive strength of the concrete is reduced. Particularly, the use amount of the slump-retaining water reducer is increased, so that the loss of slump is reduced, but the fluidity of the concrete at the early stage is easily increased, segregation and bleeding are easily caused, or the initial water reducing rate of the water reducer is insufficient, the fluidity is too low, and the production efficiency is influenced.
Disclosure of Invention
The invention aims to provide a high-performance slump-retaining polycarboxylic acid water reducing agent and a preparation method thereof, and aims to solve the technical problems that the water reducing agent in the prior art cannot meet the requirements of customers on slump-retaining time, is easy to separate and bleed during slump retaining and increases the risk of engineering problems.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a high-performance slump-retaining type polycarboxylic acid water reducing agent, which has the structural formula shown as the following formula:
wherein a, b, c, m and n are positive integers, R1Hydrogen atom or methyl group, R2Is methyl, hydroxyethyl or hydroxypropyl, and the molecular weight of the high-performance slump-retaining type polycarboxylate superplasticizer is 20000-50000.
Further, the high-performance slump-retaining type polycarboxylate water reducer comprises the following raw materials: the mass ratio of the unsaturated small monomer to the unsaturated polyether large monomer is 1: 1-5: 1; the amount of the chain transfer agent substance is 0.1 to 2.5 percent of the total amount of the unsaturated small monomer and the unsaturated polyether macromonomer; the oxidant accounts for 1 to 15 percent of the amount of the unsaturated small monomer substances; the dosage of the reducing agent is 1 to 15 percent of the dosage of the unsaturated small monomer substance; the ratio of the amount of the unsaturated ester monomer to the amount of the unsaturated polyether macromonomer is 1:1 to 4: 1; the amount of deionized water was 20 mol.
Further, the unsaturated ester monomer is at least one of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate and methyl methacrylate.
Further, the unsaturated small monomer is unsaturated acid and/or unsaturated acid anhydride.
Further, the unsaturated polyether macromonomer is at least one of 4-hydroxybutyl vinyl polyoxyethylene ether, methyl allyl polyoxyethylene ether and 3-methyl-3-butylene-1-polyoxyethylene ether, and the relative molecular weight of the unsaturated polyether macromonomer is 600-3200.
Further, the unsaturated polyether macromonomer has a relative molecular weight of 2400.
Further, the chain transfer agent is at least one of mercaptoethanol, mercaptoacetic acid, mercaptopropionic acid, sodium hypophosphite and trisodium phosphate.
Further, the reducing agent is at least one of sodium formaldehyde sulfoxylate, Vc and tartaric acid; the oxidant is hydrogen peroxide.
The invention provides a preparation method of a high-performance slump-retaining type polycarboxylate water reducer, which comprises the following steps:
s1: calculating and weighing the unsaturated small monomer, the chain transfer agent, the unsaturated ester monomer and the deionized water according to the proportion, and uniformly mixing to prepare solution A; calculating and weighing a reducing agent and deionized water according to the proportion, and uniformly mixing to prepare a solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with deionized water, pouring the mixture into a reaction container, and controlling the mixed solution to stir;
s3: keeping the temperature constant at 20-80 ℃ in the reaction process, adding an oxidant into the mixed solution obtained in the step S2, reacting for 5-10 minutes, and then dropping the solution A and the solution B into the three-neck flask obtained in the step S2 at a constant speed within a controlled time;
s4: and (5) after the liquid A and the liquid B are dripped in the step S3, continuously keeping the temperature of 20-80 ℃ and stirring for 20-90min, after the reaction is finished, cooling the reaction liquid in the three-neck flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH value to 6-7 to obtain the high-performance slump-retaining polycarboxylic acid water reducer.
Further, in step S3, the control time of both solution a and solution B is 30-150min, and the control time is controlled by any one of an automatic dropping apparatus, a peristaltic pump and a syringe pump.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
(1) the high-performance slump-retaining type polycarboxylate water reducer provided by the invention has the advantages that the molecular structure of the water reducer is adjusted by introducing ester groups and other non-hydrophilic groups, so that the non-hydrophilic groups are continuously hydrolyzed into carboxylic acid hydrophilic groups under the alkaline action of a cement paste solution, the adsorption capacity of the carboxylic acid hydrophilic groups on the surfaces of cement particles is gradually increased, and the slow release effect along with time is shown. Meanwhile, the molecular structure of the water reducing agent also has functional groups such as ether bonds, hydroxyl groups, ester groups and the like, EPO side chains provide strong steric hindrance, and the ether bonds and water molecules form hydrogen bonds and form a hydrophilic three-dimensional protective film, so that the distance between cement particles is increased, intermolecular force is weakened, and the dispersibility and the dispersion retentivity of the water reducing agent are remarkably improved; hydrophilic hydroxyl enables the surface of cement particles to form a thick hydration film and provides stronger steric hindrance repulsion; the ester group can be hydrolyzed under the alkaline condition of the concrete to release carboxylic acid products containing carboxyl, so that the synthesized water reducing agent can play a role of long-lasting slump retention.
(2) The high-performance slump-retaining type polycarboxylate water reducer provided by the invention adjusts the release rate of the water reducer by changing the quantity, the type and the initiation system of unsaturated ester monomers, and synthesizes high-performance slump-retaining mother liquor with different slump-retaining effects by using different unsaturated ester monomers in the synthesis process, so that the high-performance slump-retaining type polycarboxylate water reducer has the advantages of improving the heat release process of hydration heat reaction of concrete, and effectively controlling the segregation bleeding phenomenon and the slump loss phenomenon at the initial stage of concrete mixing.
(3) The high-performance slump-retaining type polycarboxylate water reducer provided by the invention controls the dispersion effect of water reducer molecules on cement particles through chemical action, and slowly and continuously releases the cement particles, so that the slump loss is reduced. The water reducer has a good slump retaining effect, the slump retaining time of concrete is 2-3 hours, and the water reducer has a wide market application prospect. In addition, this water-reducing agent can make the inner structure of concrete gel more compact, stable, prolongs the solidification process of concrete for later stage concrete structure has higher intensity. The polycarboxylate superplasticizer has high conversion rate, good stability and excellent slump retaining effect.
Drawings
FIG. 1 is a graph showing the comparison of initial fluidity and post-fluidity at 120min for comparative sample SJ concrete;
FIG. 2 is a graph comparing the initial and post 120min flow of example SJ1 concrete.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
First, preparation example
Example 1:
1.1 starting materials
Table 1 example 1 ingredient table
1.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, chain transfer agents and unsaturated ester monomers in 19 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 40 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 29-31 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the liquid A and the liquid B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the liquid A is 120min, and the dropping time of the liquid B is 150 min;
s4: after the addition of the liquid A and the liquid B in the step S3 is completed, continuously keeping the temperature of 29-31 ℃ and stirring for 60min, after the reaction is completed, cooling the reaction liquid in the three-necked flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali liquor and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 1, wherein the sample number is SJ 1.
Example 2:
2.1 starting materials
Table 2 example 2 ingredient table
2.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 25 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 39 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant temperature magnetic stirrer by using an iron support, and respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask; and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 39-41 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the liquid A and the liquid B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the liquid A is 120min, and the dropping time of the liquid B is 150 min;
s4: after the addition of the liquid A and the liquid B in the step S3 is completed, continuously keeping the temperature of 39-41 ℃ and stirring for 60min, after the reaction is completed, cooling the reaction liquid in the three-necked flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali liquor and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 2, wherein the sample number is SJ 2.
Example 3:
3.1 starting materials
Table 3 example 3 ingredient table
3.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 25 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 40 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 79-81 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the solution A and the solution B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the solution A is 100min, and the dropping time of the solution B is 100 min;
s4: after the addition of the solution A and the solution B in the step S3 is completed, continuously maintaining the temperature of 79-81 ℃ and stirring for 60min, after the reaction is completed, cooling the reaction solution in the three-necked flask to normal temperature, adding a neutralization solution into the reaction solution, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali solution and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 3, wherein the sample number is SJ 3.
Example 4:
4.1 starting materials
Table 4 example 4 ingredient table
4.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 24 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 40 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 59-61 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the solution A and the solution B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the solution A is 100min, and the dropping time of the solution B is 80 min;
s4: after the addition of the solution A and the solution B in the step S3 is completed, continuously maintaining the temperature of 59-61 ℃ and stirring for 60min, after the reaction is completed, cooling the reaction solution in the three-necked flask to normal temperature, adding a neutralization solution into the reaction solution, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali solution and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer of the embodiment 4, wherein the sample number is SJ 4.
Example 5:
5.1 starting materials
Table 5 example 5 ingredient table
5.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 28 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 38 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 49-51 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the solution A and the solution B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the solution A is 100min, and the dropping time of the solution B is 80 min;
s4: after the addition of the liquid A and the liquid B in the step S3 is completed, continuously keeping stirring at 49-51 ℃ for 60min, after the reaction is completed, cooling the reaction liquid in the three-necked flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali liquor and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 5, wherein the sample number is SJ 5.
Example 6
6.1 starting materials
Table 6 example 6 ingredient table
6.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 25 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 35 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 49-51 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the solution A and the solution B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the solution A is 100min, and the dropping time of the solution B is 80 min;
s4: after the addition of the liquid A and the liquid B in the step S3 is completed, continuously keeping stirring at 49-51 ℃ for 60min, after the reaction is completed, cooling the reaction liquid in the three-necked flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali liquor and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 6, wherein the sample number is SJ 6.
Example 7
7.1 starting materials
Table 7 example 7 ingredient table
7.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 19 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 29 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 49-51 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the solution A and the solution B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the solution A is 100min, and the dropping time of the solution B is 80 min;
s4: after the addition of the solution A and the solution B in the step S3 is completed, continuously maintaining the temperature of 49-51 ℃ and stirring for 60min, after the reaction is completed, cooling the reaction solution in the three-necked flask to normal temperature, adding a neutralization solution into the reaction solution, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali solution and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 7, wherein the sample number is SJ 7.
Example 8:
8.1 starting materials
Table 8 example 8 ingredient table
8.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 22 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 35 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 49-51 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the solution A and the solution B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the solution A is 100min, and the dropping time of the solution B is 80 min;
s4: after the addition of the liquid A and the liquid B in the step S3 is completed, continuously keeping stirring at 49-51 ℃ for 60min, after the reaction is completed, cooling the reaction liquid in the three-necked flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali liquor and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 8, wherein the sample number is SJ 8.
Example 9:
9.1 starting Material
Compared with example 1, only the kind of the unsaturated ester monomer was changed.
Table 9 example 9 ingredient table
9.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 20 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 36 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 49-51 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the solution A and the solution B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the solution A is 100min, and the dropping time of the solution B is 80 min;
s4: after the addition of the liquid A and the liquid B in the step S3 is completed, continuously keeping stirring at 49-51 ℃ for 60min, after the reaction is completed, cooling the reaction liquid in the three-necked flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali liquor and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 9, wherein the sample number is SJ 9.
Example 10:
10.1 starting materials
Table 10 example 10 ingredient table
10.2 preparation method
The specific steps for synthesizing 1000 parts by weight of the high-performance slump-retaining polycarboxylic acid water reducer are as follows:
s1: calculating and weighing unsaturated small monomers, chain transfer agents and unsaturated ester monomers according to a batching table, and dissolving the unsaturated small monomers, the chain transfer agents and the unsaturated ester monomers in 22 parts by weight of deionized water to prepare solution A; calculating and weighing a reducing agent according to a batching table, and dissolving the reducing agent into 34 parts by weight of deionized water to prepare solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with 320 parts by weight of deionized water, pouring the mixture into a 2000ml three-neck flask, fixing the three-neck flask on a constant-temperature magnetic stirrer by using an iron support, respectively installing a temperature sensor, a conduit for titrating the solution A and a rubber plug of a conduit for titrating the solution B on three frosted openings of the three-neck flask, and starting the constant-temperature magnetic stirrer;
s3: starting the constant-temperature magnetic stirrer in the step S2, keeping the temperature constant at 49-51 ℃, adding an oxidant according to a batching table, reacting for 10min, and then uniformly dropping the solution A and the solution B into the three-neck flask in the step S2 within a controlled time, wherein the dropping time of the solution A is 100min, and the dropping time of the solution B is 80 min;
s4: after the addition of the liquid A and the liquid B in the step S3 is completed, continuously keeping stirring at 49-51 ℃ for 60min, after the reaction is completed, cooling the reaction liquid in the three-necked flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH to 6-7 (or adding 10 parts by weight of alkali liquor and 180 parts by weight of deionized water), thereby obtaining the high-performance slump-retaining polycarboxylic acid water reducer in the embodiment 10, wherein the sample number is SJ 10.
II, comparison example:
a sample of a commercially available slump-retaining type polycarboxylate superplasticizer is KH-6 slump-retaining type polycarboxylate superplasticizer mother liquor of Wuhan Huaxuan high and new technology Limited company, and the sample number is SJ.
Third, Experimental example
1. Neat paste fluidity test
The water reducing agent samples SJ1-SJ10 produced by implementation and the commercial sample SJ in the comparative example were subjected to a net slurry fluidity test according to GBT8077-2012 "concrete admixture test method".
The cement paste comprises the following ingredients: the water-reducing agent comprises 300g of omei cement P.O 42.5.5, 82g of water and 5g of water-reducing agent diluent with the mass percentage of 5%. The results of the cement paste fluidity test are shown in Table 11.
TABLE 11 Cement Net paste fluidity results
SL0、SL60、SL120The fluidity of the cement paste is 0min, 60min and 120min after the cement paste is prepared.
As can be seen from Table 12, although samples SJ8 and SJ9 of the examples of this patent had initial fluidity SL of cement neat pastes0Greater than comparative sample SJ and the remaining samples are less than comparative sample SJ; however, the increase of the fluidity of the cement paste of the samples of the patent examples at 60min and 120min is far greater than that of the samples of the comparative examples SJ; comparative sample SJ Cement Net flow SL at 120min120Loss begins to occur and the net cement flow SL for all the example samples120Still presents a great increasing trend, which shows that the high-performance slump-retaining type polycarboxylate superplasticizer synthesized by the invention has excellent slump-retaining performance.
2. Determination of concrete slump and expansion
The water reducing agent samples SJ1-SJ10 produced in the embodiment of the invention and the commercial samples SJ in the comparative example are applied to concrete test preparation, and the slump and the expansion of the concrete are measured.
Concrete proportion and material: 1m3The concrete comprises: 955Kg of stones, 955Kg of sands, (machine-made sands), 250Kg of Emei cement, 80Kg of Hebang fly ash, 180Kg of water and 6.2Kg of water reducing agent.
The results of the experiment are shown in table 12:
TABLE 12 concrete test evaluation results
As can be seen from comparison of Table 12, the initial concrete expansion values of inventive example samples SJ1-SJ10 were not much different from comparative example sample SJ, but after 120min of loss, the concrete expansion values of the example samples were much higher than the expansion of the comparative example sample SJ; there was no major difference in slump.
From the concrete test result, no matter the type and the quantity of the unsaturated ester monomers are changed or an initiation system required for synthesizing the polycarboxylate superplasticizer is changed, the high-performance slump-retaining polycarboxylate superplasticizer disclosed by the patent, namely the example sample, has better performance than the comparative sample.
3. Segregation and bleeding phenomena
Based on the blended concrete in the experimental example 2, the segregation and water-leaching phenomena of the concrete of the comparative example sample and the concrete of the example sample SJ1 are respectively observed, the bleeding phenomenon of the concrete of the comparative example sample can be seen through the graph in FIG. 1, the concrete fluidity at 120min is lower, and the slump retaining effect of the example sample SJ1 is obviously better than that of the comparative example because the initial concrete fluidity of the example sample SJ1 is not greatly changed from that of the concrete at 120 min.
4. Reinforcement for concrete structures
The strength of the concrete of comparative example and the concrete of example samples SJ1 to SJ10 after 3, 7 and 28 days, respectively, was measured based on the concrete formulated in experimental example 2.
TABLE 13 concrete strength comparison table
As can be seen from Table 13, the samples of examples had a minimum strength of SJ4 of 32.43MPa which was higher than that of comparative example sample by 1.15MPa, the samples of examples had a maximum strength of SJ3 of 35.44MPa which was higher than that of comparative example sample by 4.16MPa, and the concrete of comparative example samples had lower three-day and seven-day strengths than the samples of examples, indicating that the water-reducing agent samples SJ1 to SJ10 produced in the examples of the high-performance slump-retaining polycarboxylic acid water-reducing agent of the present invention had better effects in concrete applications than the commercial sample SJ in the comparative example.
In the above embodiments, the kinds of raw materials such as the unsaturated polyether macromonomer, the unsaturated acid small monomer or the unsaturated acid anhydride small monomer, and the chain transfer agent can be arbitrarily selected and adjusted within the range defined in the summary of the invention of the specification as needed, and the reaction time, the titration time, the temperature, the holding time, and the like can also be arbitrarily adjusted within the range defined in the summary of the invention of the specification as needed.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. A high-performance slump-retaining polycarboxylate superplasticizer is characterized in that: the structural formula of the high-performance slump-retaining polycarboxylate superplasticizer is shown as the following formula:
wherein a, b, c, m and n are positive integers, R1Hydrogen atom or methyl group, R2Is methyl, hydroxyethyl or hydroxypropyl, and the molecular weight of the high-performance slump-retaining type polycarboxylate superplasticizer is 20000-50000.
2. The high-performance slump-retaining type polycarboxylate water reducer according to claim 1, characterized by comprising the following raw material components: the mass ratio of the unsaturated small monomer to the unsaturated polyether large monomer is 1: 1-5: 1; the amount of the chain transfer agent substance is 0.1 to 2.5 percent of the total amount of the unsaturated small monomer and the unsaturated polyether macromonomer; the oxidant accounts for 1 to 15 percent of the amount of the unsaturated small monomer substances; the dosage of the reducing agent is 1 to 15 percent of the dosage of the unsaturated small monomer substance; the ratio of the amount of the unsaturated ester monomer to the amount of the unsaturated polyether macromonomer is 1:1 to 4: 1; the amount of deionized water was 20 mol.
3. The high-performance slump-retaining type polycarboxylic acid water reducing agent according to claim 2, which is characterized in that: the unsaturated ester monomer is at least one of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate and methyl methacrylate.
4. The high-performance slump-retaining type polycarboxylate water reducer according to claim 2, characterized in that: the unsaturated small monomer is unsaturated acid and/or unsaturated acid anhydride.
5. The high-performance slump-retaining type polycarboxylate water reducer according to claim 2, characterized in that: the unsaturated polyether macromonomer is at least one of 4-hydroxybutyl vinyl polyoxyethylene ether, methyl allyl polyoxyethylene ether and 3-methyl-3-butylene-1-polyoxyethylene ether; and the relative molecular weight of the unsaturated polyether macromonomer is 600-3200.
6. The high-performance slump-retaining type polycarboxylate water reducer according to claim 2, characterized in that: the chain transfer agent is at least one of mercaptoethanol, mercaptoacetic acid, mercaptopropionic acid, sodium hypophosphite and trisodium phosphate.
7. The high-performance slump-retaining type polycarboxylate water reducer according to claim 2, characterized in that: the reducing agent is at least one of sodium formaldehyde sulfoxylate, Vc and tartaric acid; the oxidant is hydrogen peroxide.
8. The preparation method of the high-performance slump-retaining type polycarboxylate water reducer as claimed in any one of claims 1-7, wherein the preparation method comprises the following steps: the method comprises the following steps:
s1: calculating and weighing the unsaturated small monomer, the chain transfer agent, the unsaturated ester monomer and the deionized water according to the proportion, and uniformly mixing to prepare solution A; calculating and weighing a reducing agent and deionized water according to the proportion, and uniformly mixing to prepare a solution B;
s2: weighing unsaturated polyether macromonomer, uniformly mixing the unsaturated polyether macromonomer with deionized water, pouring the mixture into a reaction container, and controlling the mixed solution to stir;
s3: keeping the temperature constant at 20-80 ℃ in the reaction process, adding an oxidant into the mixed solution obtained in the step S2, reacting for 5-10 minutes, and then dropping the solution A and the solution B into the three-neck flask obtained in the step S2 at a constant speed within a controlled time;
s4: and (5) after the liquid A and the liquid B are dripped in the step S3, continuously keeping the temperature of 20-80 ℃ and stirring for 20-90min, after the reaction is finished, cooling the reaction liquid in the three-neck flask to normal temperature, adding a neutralization solution into the reaction liquid, and adjusting the pH value to 6-7 to obtain the finished product of the high-performance slump-retaining polycarboxylic acid water reducer.
9. The preparation method of the high-performance slump-retaining type polycarboxylate water reducer as claimed in claim 8, wherein the preparation method comprises the following steps: in step S3, the control time of the solution A and the solution B is 30-150min, and the control time is controlled by any one of an automatic dropping apparatus, a peristaltic pump and a syringe pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110726401.5A CN113292687A (en) | 2021-06-29 | 2021-06-29 | High-performance slump-retaining polycarboxylate superplasticizer and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110726401.5A CN113292687A (en) | 2021-06-29 | 2021-06-29 | High-performance slump-retaining polycarboxylate superplasticizer and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113292687A true CN113292687A (en) | 2021-08-24 |
Family
ID=77329912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110726401.5A Pending CN113292687A (en) | 2021-06-29 | 2021-06-29 | High-performance slump-retaining polycarboxylate superplasticizer and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113292687A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325236A (en) * | 2017-07-15 | 2017-11-07 | 刘翠芬 | A kind of non-soil responsive type polycarboxylate water-reducer and preparation method thereof |
| CN108707211A (en) * | 2018-07-09 | 2018-10-26 | 山西佳维新材料股份有限公司 | A kind of collapse protection type solid polycarboxylic acid water reducing agent and preparation method thereof |
| CN108794700A (en) * | 2018-07-09 | 2018-11-13 | 福建路桥翔通建材科技有限公司 | A kind of carboxylic acid group polymer and preparation method thereof and sustained-release polycarboxylic water reducer |
| CN111333787A (en) * | 2020-03-24 | 2020-06-26 | 湖北西建新材料科技有限公司 | Gradient release type long-acting slump loss resistant polycarboxylic acid water reducing agent and preparation and application thereof |
| CN111607039A (en) * | 2019-09-11 | 2020-09-01 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Slow-release high slump loss resistant polycarboxylic acid concrete water reducer and preparation method thereof |
-
2021
- 2021-06-29 CN CN202110726401.5A patent/CN113292687A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325236A (en) * | 2017-07-15 | 2017-11-07 | 刘翠芬 | A kind of non-soil responsive type polycarboxylate water-reducer and preparation method thereof |
| CN108707211A (en) * | 2018-07-09 | 2018-10-26 | 山西佳维新材料股份有限公司 | A kind of collapse protection type solid polycarboxylic acid water reducing agent and preparation method thereof |
| CN108794700A (en) * | 2018-07-09 | 2018-11-13 | 福建路桥翔通建材科技有限公司 | A kind of carboxylic acid group polymer and preparation method thereof and sustained-release polycarboxylic water reducer |
| CN111607039A (en) * | 2019-09-11 | 2020-09-01 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Slow-release high slump loss resistant polycarboxylic acid concrete water reducer and preparation method thereof |
| CN111333787A (en) * | 2020-03-24 | 2020-06-26 | 湖北西建新材料科技有限公司 | Gradient release type long-acting slump loss resistant polycarboxylic acid water reducing agent and preparation and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 赖广兴: "高适应型聚羧酸减水剂的合成及性能研究", 《新型建筑材料》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105110687B (en) | A kind of anti-mud collapse protective poly-carboxylic acid water reducing agent and preparation method thereof | |
| CN110938176B (en) | Super-long slump loss resistant cement-based polycarboxylate superplasticizer mother liquor and application thereof | |
| CN109824836A (en) | Workability is good, wide adaptability polycarboxylate water-reducer and preparation method thereof | |
| CN106188423B (en) | A kind of sustained-release polycarboxylic super plasticizer and preparation method thereof | |
| CN110358026B (en) | Viscosity-reducing polycarboxylate superplasticizer and preparation method thereof | |
| CN109880020B (en) | Concrete workability regulator and preparation method thereof | |
| CN109627397A (en) | A kind of polycarboxylate water-reducer and preparation method thereof improving cement slurry rheological behavior | |
| CN109879629A (en) | A kind of high-thin arch dam synergist and its preparation method and application | |
| CN111592272A (en) | Polycarboxylate superplasticizer for machine-made sand concrete prestressed component and preparation method thereof | |
| CN111333787A (en) | Gradient release type long-acting slump loss resistant polycarboxylic acid water reducing agent and preparation and application thereof | |
| CN114230726A (en) | Polycarboxylate superplasticizer with strong adsorption and fast dispersion and preparation method thereof | |
| CN110305261A (en) | A kind of C50-70 self-compacting concrete Early-strength polycarboxylate superplasticizer | |
| EP2292567B1 (en) | Dispersant for a hydraulic composite | |
| CN110643003A (en) | Preparation method of retarding type ester polycarboxylate superplasticizer | |
| CN111019061A (en) | Polycarboxylate superplasticizer, high-stone-powder concrete and preparation method thereof | |
| CN111087552A (en) | Synthetic method of polycarboxylic acid water reducer with high water reducing rate and mud resistance | |
| CN113929837B (en) | Shrinkage-reducing polycarboxylic acid water reducing agent, and preparation method and application thereof | |
| CN113292687A (en) | High-performance slump-retaining polycarboxylate superplasticizer and preparation method thereof | |
| CN108219079B (en) | Polycarboxylic acid water reducing agent, and preparation method and use method thereof | |
| CN114044859A (en) | Mud-resistant slump-retaining polycarboxylate superplasticizer mother solution and preparation method thereof | |
| CN112500534A (en) | Amphoteric polycarboxylate superplasticizer and preparation method thereof | |
| CN113683736A (en) | Viscosity reduction type polycarboxylate superplasticizer for high-strength concrete and preparation method thereof | |
| CN109111556B (en) | Ester ether crosslinking polycarboxylic acid workability regulator and preparation method thereof | |
| CN113201101A (en) | Viscosity-reducing water reducer and preparation method and application thereof | |
| CN111100252A (en) | Synthetic method of polycarboxylic acid water reducer with high water reducing rate and super slump retaining property |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210824 |