CN106397683B - A kind of polycarboxylate water-reducer and preparation method thereof reducing high-grade concrete viscosity - Google Patents
A kind of polycarboxylate water-reducer and preparation method thereof reducing high-grade concrete viscosity Download PDFInfo
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- CN106397683B CN106397683B CN201610772437.6A CN201610772437A CN106397683B CN 106397683 B CN106397683 B CN 106397683B CN 201610772437 A CN201610772437 A CN 201610772437A CN 106397683 B CN106397683 B CN 106397683B
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- polycarboxylate water
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- 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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- 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
- C04B24/2641—Polyacrylates; Polymethacrylates
- C04B24/2647—Polyacrylates; Polymethacrylates containing polyether side chains
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- 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
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- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
A kind of polycarboxylate water-reducer and preparation method thereof reducing high-grade concrete viscosity, polycarboxylate water-reducer monomer end alkenyl polyoxyethylene ether as shown in formula (1), unsaturated acids and beta-unsaturated esters, initiator is added, random copolymerization reaction is carried out by aqueous solution at normal temperature, then viscosity reduction regulator progress molecular rearrangement is added and alkaline conditioner adjusting is made to neutrality.The invention also includes the preparation methods for the polycarboxylate water-reducer for reducing high-grade concrete viscosity.The polycarboxylate water-reducer water-reducing rate of the present invention is high, and it is good in high-grade concrete viscosity reducing effect to apply, and adaptability is good, and air content is low, and retentivity is good, has good pumping.
Description
Technical field
The present invention relates to a kind of polycarboxylate water-reducers and preparation method thereof, and in particular to a kind of reduction high-grade concrete is viscous
Polycarboxylate water-reducer of degree and preparation method thereof.
Background technique
Polycarboxylate water-reducer generates simple process because it has, and water-reducing rate is high, and the slump is kept, environmental-friendly etc. excellent
Point has become the water-reducing agent generally used.But when encountering C50 or more high-grade concrete, concrete will appear viscosity
The problems such as increase, flowing velocity is slow, difficulty is brought to construction.Be under normal conditions reduce viscosity by improving volume, however
Due to easily generating bleeding under low water binder ratio state, and it must be added to viscosity modifier and air entraining agent to improve.Adaptation difficulty adds
Greatly.
CN 103865007A discloses a kind of viscosity reduction type poly carboxylic acid series water reducer preparation method, which passes through in carboxylic acid
A certain amount of hydrophobic units and hydrophobic grouping are introduced and controlled in copolymer molecule structure, and playing the role of, which reduces the water-reducing agent, is lauched
The effect of cement-based material viscosity.Have many advantages, such as that viscosity reducing effect is obvious, dispersibility is high, good with cement adaptability, is particularly suitable for
Prepare high-strength concrete, self-compacting concrete and low water binder ratio high additive mineral admixture concrete etc..However the invention is dropped
Viscous effect is not too obvious, and does not refer to the influence of concrete retentivity.CN 104262550A discloses a kind of poly- carboxylic of viscosity reduction type
The preparation method of sour based water reducer, the invention use unsaturated primary amine class minor comonomer, have the small organic molecule of epoxy group and contain
Unsaturated quaternary ammonium salt is made in halogen group, is then copolymerized with unsaturated acids, the viscosity reduction type poly carboxylic acid series water reducer tool of preparation
Have the advantages that reaction is simple, easily controllable, at low cost.Meanwhile, it is capable to reduce concrete viscosity, improve slump-retaining etc. ask
Topic, however halogen group has been introduced in the invention, reduces concrete to the corrosion resistance of reinforcing bar.CN 104371081A is disclosed
A kind of preparation method of rapid dispersion viscosity reduction type poly-carboxylic-acid cement dispersant, the invention is based on using the unsaturation of tertiary-amino-containing big
Molecule monomer obtains hyperbranched poly-carboxylic-acid cement dispersant as the reducing agent that may participate in polymerization, provides a kind of rapid dispersion
The preparation method of viscosity reduction type poly-carboxylic-acid cement dispersant has life although the invention has larger improvement to concrete viscosity
Produce more complex, the disadvantages of reaction time is longer.
Summary of the invention
It is high, anti-that the technical problem to be solved by the invention is to provide a kind of water-reducing rates for reducing high-grade concrete viscosity
Clay soils are good, cement adaptability is good, the polycarboxylate water-reducer that air content is low and preparation method thereof.
The technical solution used to solve the technical problems of the present invention is that a kind of polycarboxylic acids for reducing high-grade concrete viscosity
Initiator is added, normal in water-reducing agent, monomer end alkenyl polyoxyethylene ether, unsaturated acids and beta-unsaturated esters as shown in formula (1)
Temperature is lower to carry out random copolymerization reaction by aqueous solution, and viscosity reduction regulator is then added and carries out molecular rearrangement and alkaline conditioner
Neutrality is adjusted to be made, shown in the polycarboxylate water-reducer host molecule structure such as formula (2):
In formula (1), R1 is hydrogen or methyl；M is 1~5, n is 1~15；
In formula (2), R1 is hydrogen or methyl, and R2 is carboxyl, phenyl, p-sulfonic acid phenyl or to formic acid phenyl, and R3 is hydrogen, first
Base, sulfonic group or carboxyl, R4 are hydrogen or methyl, ethoxy, hydroxypropyl, hydroxyl butyl；A is 6~30, b is 3~15, c is 6~30.
Further, the weight average molecular weight of the polycarboxylate water-reducer is 5500~25000.
Further, the weight average molecular weight of the end alkenyl polyoxyethylene ether is 200~1000.
Further, the end alkenyl polyoxyethylene ether is allyl polyethenoxy ether, and methyl allyl polyoxyethylene ether is different
One or more of pentenyl polyoxyethylene ether, isohexenyl polyoxyethylene ether and iso-heptene base polyoxyethylene ether are mixed
Close object.
Further, the unsaturated acids be cinnamic acid, acrylic acid, to vinyl benzenesulfonic acid and to one kind of vinylbenzoic acid or
Two or more mixtures；The beta-unsaturated esters include methyl acrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate and acrylic acid
The mixture of one or more of hydroxy butyl ester.
Further, the initiator is isopropyl benzene hydroperoxide, ammonium persulfate, benzoyl peroxide and azodiisobutyronitrile
One or more of mixture；The reducing agent is tartaric acid, glucose, oxalic acid and N, in N- diethylaniline
One or more kinds of mixtures.
Further, the viscosity reduction regulator is glycerine, propylene diethanol, tannic acid sodium and 2- methyl -2- acrylamide
The mixture of one or more of base propane sulfonic acid.
The present invention further solve its technical problem the technical solution adopted is that, it is a kind of to reduce high-grade concrete viscosity
The preparation method of polycarboxylate water-reducer, monomer end alkenyl polyoxyethylene ether, unsaturated acids and unsaturation as shown in formula (1)
Initiator is added in ester, carries out random copolymerization reaction by aqueous solution at normal temperature, and viscosity reduction regulator is then added and carries out molecule weight
Row and alkaline conditioner adjusting is made to neutrality, wherein the end alkenyl polyoxyethylene ether, unsaturated acids, beta-unsaturated esters,
Initiator, reducing agent, viscosity reduction regulator mass parts ratio are 100:5~20:5~20:0.5~1.0:0.1~0.5:2~10.
Further, the synthesizing temperature optimal control is at 10~20 DEG C.
Further, the reaction time of the copolyreaction is 3 hours, keeps preferable reactivity worth.
The present invention is used from deisgn product monomer structure end alkenyl polyoxyethylene ether, can significantly reduce high-grade concrete
Viscosity is effectively improved skyscraper pumping effect；High-strength concrete, the water-reducing property requirement of super high strength concrete can be met；?
Can avoid in application process clay content in sand material it is excessively high caused by slump-loss problem；Simultaneously to the sand of each department
There is stronger adaptability with cement, there is better adaptability particularly with Machine-made Sand.
To sum up, the polycarboxylate water-reducer product viscosity reducing effect of the present invention is good, water-reducing rate is high, anti-clay soils are good, cement is suitable
Answering property is good, and retentivity is good, and air content is low, and production is simple and convenient, high-efficient, pollution-free.
Specific embodiment
The present invention is further illustrated below with reference to embodiment.
Embodiment 1
By 100 parts of methyl allyl polyoxyethylene ether, 15 parts of acrylic acid and 10 parts of hydroxy-ethyl acrylates, 80 parts of deionizations
Water, stirring is completely dissolved reactant at normal temperature, is added 1.0 parts of ammonium persulfates, be added dropwise again into container after 15min dissolved with
The aqueous solution of 0.5 part of tartaric acid controls rate of addition, drips off in 2h, and viscosity reduction regulator propyleneglycoles 5.5 are then added
Part, thermotonus 1h is kept, 30% sodium hydroxide solution is ultimately joined and adjusts pH=7.0, be diluted with water obtained 55% and contain admittedly
Liquor high performance water reducing agent of polyocarboxy acid (water can also be added to be diluted to any concentration) is to get product J NCR-P1.
Embodiment 2
By 100 parts of isopentene group polyoxyethylene ether, 10 pairs of vinyl benzenesulfonic acids and 12 parts of hydroxypropyl acrylates, 80 parts go from
Sub- water, stirring is completely dissolved reactant at normal temperature, and 0.8 part of azodiisobutyronitrile is added, is added dropwise again into container after 15min
Dissolved with the aqueous solution of 0.3 part of glucose, rate of addition is controlled, is dripped off in 2h, viscosity reduction regulator glycerine 4.5 is then added
Part, thermotonus 1h is kept, 30% sodium hydroxide solution is ultimately joined and adjusts pH=7.0, be diluted with water obtained 55% and contain admittedly
Liquor high performance water reducing agent of polyocarboxy acid (water can also be added to be diluted to any concentration) is to get product J NCR-P2.
Embodiment 3
By 100 parts of isohexenyl polyoxyethylene ether, 12 pairs of vinylbenzoic acids and 14 parts of methyl acrylates, 80 parts go from
Son, stirring is completely dissolved reactant at normal temperature, is added 1.0 parts of ammonium persulfates, be added dropwise again into container after 15min dissolved with
The aqueous solution of 0.5 part of oxalic acid controls rate of addition, drips off in 2h, and viscosity reduction regulator 2- methyl -2- acryloyl is then added
2.5 parts of amido propane sulfonic acid, keep thermotonus 1h.It ultimately joins 30% sodium hydroxide solution and adjusts pH=7.0, system is diluted with water
The 55% liquor high performance water reducing agent of polyocarboxy acid (water can also be added to be diluted to any concentration) contained admittedly is obtained to get product J NCR-
P3。
Embodiment 4
By 50 parts of methyl allyl polyoxyethylene ether and 50 parts of iso-heptene base polyoxyethylene ether, 14 cinnamic acids and 16 part third
Olefin(e) acid hydroxyl ethyl ester, 80 parts of deionized waters, stirring is completely dissolved reactant at normal temperature, and 1.0 parts of benzoyl peroxides are added,
The N dissolved with 0.1 part is added dropwise after 15min into container again, the aqueous solution of N- diethylaniline controls rate of addition, drips in 2h
It is complete, 3.5 parts of viscosity reduction regulator tannic acid sodium is then added, keeps thermotonus 1h, ultimately joins 30% sodium hydroxide solution tune
PH=7.0 is saved, the liquor high performance water reducing agent of polyocarboxy acid that obtained 55% contains admittedly, which is diluted with water, (can also add water to be diluted to any
Concentration) to get product J NCR-P4.
Embodiment 5
By 20 parts of allyl polyethenoxy ether and 80 parts of isohexenyl polyoxyethylene ether, 10 acrylic acid and 5 parts of acrylic acid
Hydroxy butyl ester, 80 parts of deionized waters, stirring is completely dissolved reactant at normal temperature, is added 1.0 parts of ammonium persulfates, after 15min again
The aqueous solution dissolved with 0.5 part of tartaric acid is added dropwise into container, controls rate of addition, is dripped off in 2h, viscosity reduction tune is then added
7.5 parts of agent propyleneglycoles of section keeps thermotonus 1h, ultimately joins 30% sodium hydroxide solution and adjusts pH=7.0, dilute with water
Liquor high performance water reducing agent of polyocarboxy acid (water can also be added to be diluted to any concentration) that obtained 55% contains admittedly is released to get product
JNCR-P5。
Application example 1
In order to evaluate dispersibility of the polycarboxylate water-reducer for reducing concrete viscosity to cement slurry of Examples 1 to 5 preparation
Can, referring to GB8077-2000 " Methods for testing uniformity of concrete admixture ", carried out only to sample is obtained made from Examples 1 to 5
Starch fluidity test.W/C (water-cement ratio) is 0.29, and admixture dosage is the 0.18% of cement consumption.By Bu Shi rotary viscosity
It counts the viscosity reducing effect for carrying out cement paste to sample to detect, commercially available concrete viscosity reduction polycarboxylate water-reducer work is selected to join
According to experimental result is shown in shown in the following table 1.
The paste flowing degree and gradual loss and viscosity of table 1- difference sample
As shown in Table 1, polycarboxylate water-reducer made from Examples 1 to 5 is preferable to cement paste dispersibility and retentivity, and
Viscosity decreases than commercial samples.As it can be seen that polycarboxylate water-reducer made from Examples 1 to 5 can be compared with making institute under low-dosage
The cement slurry of configuration has the fluidity holding capacity and viscosity reducing effect of long period.
Application example 2
To evaluate the polycarboxylate water-reducer of Examples 1 to 5 preparation to the air content of cement dispersants, retentivity and drop
Sticky energy, has carried out the measurement of air content according to the relevant regulations experimental method of GB8076-2008 " concrete admixture ".Reference
JC473-2001 " concrete pump-feed agent " relevant regulations determine the slump and slump-loss, and adjust water consumption, concrete
Match ratio is shown in Table 2.Flow time is tested using concrete inverted slump test tube to evaluate.Method particularly includes: slump cone is inverted,
Bottom seal cap is filled concrete and is smoothed out, slips off bottom cover rapidly, and with the time of stopwatch metering coagulation soil flow sky, concrete is fallen
Slump cone test flow time experimental result is shown in Table 3.
Table 2- concrete mix (KG/m3)
| Water | Cement | Flyash | Sand | Stone | Water-cement ratio |
| 138 | 400 | 90 | 684 | 1116 | 0.28 |
Table 3- concrete 's air-containing and slump ongoing change
As shown in Table 3, the concrete inverted slump test tube test stream that polycarboxylate water-reducer made from Examples 1 to 5 obtains is empty
Time is shorter than commercial product, can significantly reduce the viscosity of high-grade concrete, and there is preferable concrete divergence to keep
Ability and air content control effect.
Claims (9)
1. a kind of polycarboxylate water-reducer for reducing high-grade concrete viscosity, which is characterized in that the monomer end alkene as shown in formula (1)
Initiator is added in base polyoxyethylene ether, unsaturated acids and beta-unsaturated esters, and it is anti-to carry out random copolymerization by aqueous solution at normal temperature
It answers, viscosity reduction regulator progress molecular rearrangement is then added and alkaline conditioner adjusting is made to neutrality, the polycarboxylic acids diminishing
Shown in agent host molecule structure such as formula (2):
In formula (1), R is hydrogen or methyl；M is 1~5, n is 1~15；
In formula (2), R1 is hydrogen or methyl, and R2 is carboxyl, phenyl, p-sulfonic acid phenyl or to formic acid phenyl, and R3 is hydrogen, methyl, sulphur
Acidic group or carboxyl, R4 are methyl, ethoxy, hydroxypropyl, hydroxyl butyl；A is 6~30, b is 3~15, c is 6~30；
The viscosity reduction regulator is in glycerine, propylene diethanol, tannic acid sodium and 2- methyl -2- acryamidopropanesulfonic acid
One or more kinds of mixtures.
2. polycarboxylate water-reducer according to claim 1, which is characterized in that the weight average molecular weight of the polycarboxylate water-reducer
It is 5500~25000.
3. polycarboxylate water-reducer according to claim 1 again, which is characterized in that the end alkenyl polyoxyethylene ether is divided equally
Son amount is 200~1000.
4. polycarboxylate water-reducer according to claim 3, which is characterized in that the end alkenyl polyoxyethylene ether is allyl
Polyoxyethylene ether, methyl allyl polyoxyethylene ether, isopentene group polyoxyethylene ether, isohexenyl polyoxyethylene ether and iso-heptene
The mixture of one or more of base polyoxyethylene ether.
5. polycarboxylate water-reducer according to claim 1, which is characterized in that the unsaturated acids be cinnamic acid, acrylic acid,
To vinyl benzenesulfonic acid and to one or more kinds of mixtures of vinylbenzoic acid；The beta-unsaturated esters include acrylic acid first
The mixture of one or more of ester, hydroxy-ethyl acrylate, hydroxypropyl acrylate and hy-droxybutyl.
6. polycarboxylate water-reducer according to claim 1, which is characterized in that the initiator be isopropyl benzene hydroperoxide,
The mixture of one or more of ammonium persulfate, benzoyl peroxide and azodiisobutyronitrile；It is added to reaction system
Reducing agent, the reducing agent are tartaric acid, glucose, oxalic acid and N, the mixing of one or more of N- diethylaniline
Object.
7. a kind of preparation side of the polycarboxylate water-reducer of the reduction high-grade concrete viscosity as described in one of claim 1~6
Method, which is characterized in that monomer end alkenyl polyoxyethylene ether, unsaturated acids and beta-unsaturated esters as shown in formula (1) are added and cause
Agent carries out random copolymerization reaction by aqueous solution at normal temperature, and viscosity reduction regulator is then added and carries out molecular rearrangement, and alkalinity
Regulator adjusting is made to neutrality, wherein the end alkenyl polyoxyethylene ether, unsaturated acids, beta-unsaturated esters, initiator, reduction
Agent, viscosity reduction regulator mass parts ratio are 100:5~20:5~20:0.5~1.0:0.1~0.5:2~10.
8. the preparation method of the polycarboxylate water-reducer according to claim 7 for reducing high-grade concrete viscosity, feature
It is, the synthesizing temperature optimal control is at 10~20 DEG C.
9. the preparation method of the polycarboxylate water-reducer according to claim 7 for reducing high-grade concrete viscosity, feature
It is, the reaction time of the copolyreaction is 3 hours.
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| CN106967200A (en) * | 2017-03-31 | 2017-07-21 | 刘翠芬 | It is a kind of to have poly carboxylic acid series water reducer that guarantor is collapsed with viscosity-reducing performance and preparation method thereof concurrently |
| CN111377643B (en) | 2018-12-31 | 2021-09-28 | 江苏苏博特新材料股份有限公司 | High-adaptability viscosity-reduction type polycarboxylate superplasticizer and preparation method and application thereof |
| CN111116084B (en) * | 2019-12-30 | 2022-04-12 | 庐江县新创新型材料有限公司 | Concrete high-efficiency water-reducing additive and preparation method thereof |
| CN112390921A (en) * | 2020-11-05 | 2021-02-23 | 云南建投高分子材料有限公司 | Synthetic viscosity-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN113754361A (en) * | 2021-08-21 | 2021-12-07 | 徐振江 | Method for manufacturing viscosity-reducing concrete |
| CN116554413A (en) * | 2023-05-05 | 2023-08-08 | 贵州天威建材科技有限责任公司 | A kind of viscosity-reducing polycarboxylate water-reducer and its preparation method |
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| DE102004002192B4 (en) * | 2004-01-15 | 2006-09-21 | Hilti Ag | Use of ethylenically unsaturated isocyanate derivatives for the covalent bonding of active hydrogen-containing impurities in curable compositions |
| CN101492518B (en) * | 2009-02-27 | 2010-12-08 | 上海市建筑科学研究院(集团)有限公司 | Ethers polycarboxylic acid water reducing agent and preparation |
| CN101805146A (en) * | 2010-03-31 | 2010-08-18 | 华南理工大学 | Polycarboxylic acid water reducer and preparation method thereof |
| CN102503227A (en) * | 2011-10-27 | 2012-06-20 | 北京东方雨虹防水技术股份有限公司 | Early-strength polycarboxylic acid water reducing agent |
| CN102503216A (en) * | 2011-10-27 | 2012-06-20 | 北京东方雨虹防水技术股份有限公司 | Method for synthesizing universal polycarboxylic water reducer |
| CN103396031B (en) * | 2013-07-19 | 2016-03-02 | 北京东方雨虹防水技术股份有限公司 | A kind of carboxylic acid water reducer and preparation method thereof |
| CN104446093A (en) * | 2014-12-04 | 2015-03-25 | 河北铁园科技发展有限公司 | Polycarboxylate-based water reducing agent with integrated functions of water reduction and slump retaining |
| CN105367721B (en) * | 2015-11-30 | 2018-02-23 | 江苏苏博特新材料股份有限公司 | The preparation method and application of viscosity reduction type polycarboxylic acid super-plasticizer |
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