CN110003401A - A kind of clear-water concrete low entraining type polycarboxylate water-reducer and preparation method thereof - Google Patents
A kind of clear-water concrete low entraining type polycarboxylate water-reducer and preparation method thereof Download PDFInfo
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- CN110003401A CN110003401A CN201910276284.XA CN201910276284A CN110003401A CN 110003401 A CN110003401 A CN 110003401A CN 201910276284 A CN201910276284 A CN 201910276284A CN 110003401 A CN110003401 A CN 110003401A
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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
- C04B24/243—Phosphorus-containing polymers
- C04B24/246—Phosphorus-containing polymers containing polyether side chains
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
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- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
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Abstract
The invention discloses a kind of clear-water concrete low entraining type polycarboxylate water-reducer, including bottom material, A liquid, B liquid and neutralizer, the bottom material raw material is as follows by weight: 200-300 parts of conventional polyether monomer, 20-100 parts of block polyether monomer, 2-8 parts of phosphate, 2-5 parts of oxidant, 200 parts of water；The A liquid raw material is as follows by weight: 0.5-1.2 parts of reducing agent, 1.5-3.0 parts of chain-transferring agent, 120 parts of water；The B liquid raw material is as follows by weight: 20-30 parts of unsaturated carboxylic acid, 15-20 parts of esters of unsaturated carboxylic acids, 80 parts of water, the neutralizer raw material is as follows by weight: 3-6 parts of neutralizer, 200-300 parts of water.Clear-water concrete low entraining type polycarboxylate water-reducer prepared by the present invention, introduces EO/PO block polyether, surface tension is lower than conventional polyether, under the same conditions, low surface tension biggish bubble easy to form, therefore bubble is easier to be crushed, and advantageously reduces the bleed of water-reducing agent.
Description
Technical field
The present invention relates to water-reducing agent technical field more particularly to a kind of clear-water concrete low entraining type polycarboxylate water-reducer and
Preparation method.
Background technique
In recent years, with the development of concrete technology, clear-water concrete using more more and more universal, engineer application is no longer
It is confined to bridge and airport, more and more industry and civil buildings also begin to use clear-water concrete.With normal concrete phase
The phenomenon that requiring appearance luster uniform, smooth beautiful, without voids and pits than, clear-water concrete, this is to the preparation of concrete and applies
Work management is a very big challenge.Polycarboxylate water-reducer is as latest generation water-reducing agent, with water-reducing rate is high, volume is low, protects and collapses
Property it is good and good with cement adaptability the features such as, be widely used in various concrete works.
Since polycarboxylate water-reducer has certain bleed, many clear-water concretes are in match ratio trial process
In, although often there is the Indexes Comparisons such as the concrete working performance prepared ideal, since air content is bigger than normal, concrete surface
Phenomena such as bubble is more, low strength.It is general to be disappeared by the way that defoaming agent is added in order to solve the problems, such as that concrete 's air-containing is excessive
Bubble, there are the problem of first is that the defoaming agent of entirely appropriate polycarboxylate water-reducer is few or defoaming agent and polycarboxylate water-reducer phase
Capacitive is poor or defoaming effect is undesirable；Second is that not can solve concrete 's air-containing big for defoaming agent in practice for many engineerings
Problem.Therefore, preparation low entraining type polycarboxylate water-reducer can fundamentally solve the problems, such as that concrete 's air-containing is excessively high, especially suitable
For requiring lower engineering to concrete 's air-containing as clear-water concrete this kind.Since polycarboxylate water-reducer contains long gather
Ether side-chain structure easily makes the bleed of water-reducing agent excessive, causes the problems such as concrete 's air-containing is high, hardening strength is low.From existing
Research from the point of view of, two kinds can be divided into the conclusion of the low air-entraining performance comprehensive study of polycarboxylate water-reducer both at home and abroad at present: 1) physical method:
Water-reducing agent and defoaming agent carry out physical compounding；2) chemical method: defoaming group is introduced in polycarboxylate water-reducer molecule, and adjusts and subtracts
The ratio of polar group and nonpolar base in aqua side chain.By Molecular Design, the polyethers side for having EO/PO block is introduced
Chain has the bound phosphate groups of defoaming function, and the acrylate monomer with hydrophobic alkyl chain, and by adjusting poly- carboxylic
The ratio of EO/PO block chain, phosphate and acrylate in sour diminishing agent molecule, to realize low entraining type polycarboxylate water-reducer
High water reduction, high-thin arch dam and low entraining high performance.
Summary of the invention
The purpose of the present invention is to solve disadvantage existing in the prior art, and a kind of clear-water concrete for proposing is low draws
Gas type polycarboxylate water-reducer and preparation method thereof.
To achieve the goals above, present invention employs following technical solutions:
A kind of clear-water concrete low entraining type polycarboxylate water-reducer, including bottom material, A liquid, B liquid and neutralizer, the bottom material
Raw material is as follows by weight: 200-300 parts of conventional polyether monomer, 20-100 parts of block polyether monomer, and 2-8 parts of phosphate, oxidation
2-5 parts of agent, 200 parts of water；The A liquid raw material is as follows by weight: 0.5-1.2 parts of reducing agent, 1.5-3.0 parts of chain-transferring agent, and water
120 parts；The B liquid raw material is as follows by weight: 20-30 parts of unsaturated carboxylic acid, 15-20 parts of esters of unsaturated carboxylic acids, and 80 parts of water, institute
It is as follows by weight to state neutralizer raw material: 3-6 parts of neutralizer, 200-300 parts of water.
Preferably, the conventional polyether polymeric monomer be methyl allyl alcohol polyoxyethylene ether or isoamyl alcohol polyoxyethylene ether,
Molecular weight is (2400-3000) dalton.
Preferably, the disodium hydrogen phosphate and sodium dihydrogen phosphate are anhydrous state.
Preferably, the block polyether monomer is EO/PO block polyether, and the EO/PO degree of polymerization is 10-30, and molecular structure is such as
Under:
Preferably, the phosphate is 2-hydroxyethyl methacrylate phosphate (HEMAP) or 1- hydroxyl ethyl ester methyl-prop
Olefin(e) acid ester phosphate (UPE), molecular structure is as follows:
Preferably, the oxidant be concentration be 27.5% hydrogen peroxide, ammonium persulfate, one of potassium peroxydisulfate or more
Kind.
Preferably, the reducing agent is one of the anti-sepsis acid of L-, sodium formaldehyde sulfoxylate and sodium sulfite or a variety of, and the chain turns
Moving agent is mercaptopropionic acid or thioacetic acid.
Preferably, the insatiable hunger carboxylic acid is one of acrylic acid, methacrylic acid or a variety of, the esters of unsaturated carboxylic acids
For one of ethyl acrylate, isopropyl acrylate and isobutyl acrylate or a variety of, the neutralizer is sodium hydroxide, hydrogen
One of potassium oxide is a variety of.
Preferably, the water is the industry water of deionized water or conductivity less than 20 μ S/cm.
The present invention also provides a kind of preparation methods of clear-water concrete low entraining type polycarboxylate water-reducer, including walk as follows
It is rapid:
S1: it prepares bottom material: conventional polyether monomer, block polyether monomer, phosphate and deionized water is added in reaction kettle,
It is stirred under room temperature, is completely dissolved raw material, obtain reaction bottom material；
S2: it prepares dropping liquid A: load weighted reducing agent and chain-transferring agent being added in deionized water, stirs evenly, obtains
Dropping liquid A；
S3: it prepares dropping liquid B: load weighted unsaturated carboxylic acid, esters of unsaturated carboxylic acids being added in deionized water, stirring is equal
It is even, obtain dropping liquid B；
S4: load weighted oxidant is added in bottom material, is stirred 5-10 minutes, is then at the uniform velocity added dropwise into reaction kettle respectively
A liquid, B liquid, control A liquid time for adding 3.5-4.0h, B liquid time for adding are 3.0-3.5h, drip subsequent continuation of insurance temperature 1.0-
2.0h；
S5: after the reaction was completed, neutralizer is added and deionized water adjusts pH value of solution as 5-7, obtaining solid content is 40%
Clear-water concrete low entraining type polycarboxylate water-reducer.
Compared with prior art the invention has the benefit that
1, clear-water concrete low entraining type polycarboxylate water-reducer prepared by the present invention, introduces EO/PO block polyether, table
Face warp tension ratio conventional polyether is low, under the same conditions, low surface tension biggish bubble easy to form, and therefore bubble is easier to break
It is broken, advantageously reduce the bleed of water-reducing agent.
2, clear-water concrete low entraining type polycarboxylate water-reducer prepared by the present invention, also introduces the phosphoric acid with defoaming function
Ester monomer and acrylate monomer with hydrophobic alkyl chain, the on the one hand amphipathic property of adjustable diminishing agent molecule
Can, the bleed effect of water-reducing agent is reduced, while can also reduce concrete viscosity, is conducive to the evolution of bubble；Another aspect phosphoric acid
Ester and acrylate hydrolyze in cement alkaline environment releases phosphate radical and carboxylate radical, is adsorbed in cement particle surface again,
Lasting peptizaiton is played, the guarantor for being conducive to improve polycarboxylate water-reducer is collapsed effect.
3, low entraining type polycarboxylate water-reducer prepared by the present invention only needs a step to be made by Raolical polymerizable, and
And without heating, simple process, energy conservation and environmental protection, raw materials used to be easy to get extensively, cost is relatively low, is suitble to industrialized production, product
It can stablize, bleed is low, water-reducing rate is high and guarantor is collapsed, and effect is preferable, has a good application prospect.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
Embodiment 1
A kind of preparation method of clear-water concrete low entraining type polycarboxylate water-reducer, includes the following steps:
S1: bottom material is prepared: by 220 parts of methyl allyl polyoxyethylene ethers (2400), 30 parts of block polyether monomer (EO/PO
The degree of polymerization be 10), 3 parts of 2-hydroxyethyl methacrylate phosphates (HEMAP) and 200 parts of deionized waters be added in reaction kettles,
It is stirred under room temperature, is completely dissolved raw material, obtain reaction bottom material；
S2: it prepares dropping liquid A: the anti-sepsis acid of 0.7 part of L- and 1.6 parts of thioacetic acid being added in 120 parts of deionized waters, stirred
It mixes uniformly, obtains dropping liquid A；
S3: it prepares dropping liquid B: 20 parts of acrylic acid, 15 parts of ethyl acrylates being added in 80 parts of deionized waters, stirring is equal
It is even, obtain dropping liquid B；
S4: 3 parts of hydrogen peroxide are added in bottom material, stir 5-10 minutes, A liquid, B is then at the uniform velocity added dropwise into reaction kettle respectively
Liquid, control A liquid time for adding 3.5h, B liquid time for adding are 3.0h, drip subsequent continuation of insurance temperature 1.0h；
S5: after the reaction was completed, 3 parts of sodium hydroxides is added and 50 parts of deionized waters adjust pH value of solution as 5-7, obtain solid content
For 40% clear-water concrete low entraining type polycarboxylate water-reducer.
Embodiment 2
A kind of preparation method of clear-water concrete low entraining type polycarboxylate water-reducer, includes the following steps:
S1: prepare bottom material: by 250 parts of isoamyl alcohol polyoxyethylene ethers (2400), (EO/PO is poly- for 50 parts of block polyether monomers
It is right be 20), 5 parts of 1- hydroxyl ethyl ester methacrylate phosphates (UPE) and 200 parts of deionized waters be added in reaction kettles, room temperature
Lower stirring, is completely dissolved raw material, obtains reaction bottom material；
S2: it prepares dropping liquid A: 0.9 part of sodium formaldehyde sulfoxylate and 2.2 parts of mercaptopropionic acids being added in 120 parts of deionized waters, stirring is equal
It is even, obtain dropping liquid A；
S3: it prepares dropping liquid B: 25 parts of methacrylic acids, 20 parts of isopropyl acrylates being added in 80 parts of deionized waters, are stirred
It mixes uniformly, obtains dropping liquid B；
S4: 4 parts of ammonium persulfates are added in bottom material, stir 5-10 minutes, A is then at the uniform velocity added dropwise into reaction kettle respectively
Liquid, B liquid, control A liquid time for adding 3.5h, B liquid time for adding are 3.0h, drip subsequent continuation of insurance temperature 1.0h；
S5: after the reaction was completed, adding 4 parts of potassium hydroxide and 150 parts of deionized waters to adjust pH value of solution is 5-7, obtains solid content
For 40% clear-water concrete low entraining type polycarboxylate water-reducer.
Embodiment 3
A kind of preparation method of clear-water concrete low entraining type polycarboxylate water-reducer, includes the following steps:
S1: prepare bottom material: by 280 parts of isoamyl alcohol polyoxyethylene ethers (3000), (EO/PO is poly- for 80 parts of block polyether monomers
It is right be 30), 7 parts of 2-hydroxyethyl methacrylate phosphates (HEMAP) and 200 parts of deionized waters be added in reaction kettles, often
The lower stirring of temperature, is completely dissolved raw material, obtains reaction bottom material；
S2: it prepares dropping liquid A: 1.2 parts of sodium sulfites and 2.7 parts of mercaptopropionic acids being added in 120 parts of deionized waters, stirring
Uniformly, dropping liquid A is obtained；
S3: it prepares dropping liquid B: 30 parts of acrylic acid, 35 parts of isobutyl acrylates being added in 80 parts of deionized waters, stirring is equal
It is even, obtain dropping liquid B；
S4: 5 parts of potassium peroxydisulfates are added in bottom material, stir 5-10 minutes, A is then at the uniform velocity added dropwise into reaction kettle respectively
Liquid, B liquid, control A liquid time for adding 3.5h, B liquid time for adding are 3.0h, drip subsequent continuation of insurance temperature 1.0h；
S5: after the reaction was completed, 6 parts of sodium hydroxides is added and 250 parts of deionized waters adjust pH value of solution as 5-7, obtain containing solid
The clear-water concrete low entraining type polycarboxylate water-reducer that amount is 40%.
Below by way of description of test beneficial effects of the present invention:
3 kinds of clear-water concrete low entraining type polycarboxylate water-reducer samples that embodiment 1-3 is synthesized carry out concrete performance
Test, and compared with commercially available routine plain edition polycarboxylate water-reducer PCE-1.
Concrete test reference standard GB/T 50080-2011 " Standard for test methods of properties of ordinary concrete mixture standard ",
GB/T 50081-2016 " standard for test methods of mechanical properties of ordinary concrete ".Concrete design strength grade is common C30,
Folk prescription match ratio are as follows: cement 270kg, flyash 70kg, sand 830kg, stone 1060kg, water 160kg, water-reducing agent roll over solid volume and be
0.20%.Cement is 42.5 cement of Yumen PO；Flyash is easy day second class powered coal ash；Sand is river sand, and fineness mould degree is 2.6；
Stone is (5-25) mm continuous grading rubble.Test data is shown in Table 1.
The comparison of 1 concrete test of table
Clear-water concrete low entraining type polycarboxylate water-reducer of the invention is compared with plain edition polycarboxylate water-reducer, identical
Roll under solid volume, concrete slump and it is slump-retaining more preferably and air content is substantially reduced, compression strength is also mentioned
It is high.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of clear-water concrete low entraining type polycarboxylate water-reducer, including bottom material, A liquid, B liquid and neutralizer, it is characterised in that:
The bottom material raw material is as follows by weight: 200-300 parts of conventional polyether monomer, 20-100 parts of block polyether monomer, and phosphate 2-8
Part, 2-5 parts of oxidant, 200 parts of water；The A liquid raw material is as follows by weight: 0.5-1.2 parts of reducing agent, chain-transferring agent 1.5-
3.0 parts, 120 parts of water；The B liquid raw material is as follows by weight: 20-30 parts of unsaturated carboxylic acid, 15-20 parts of esters of unsaturated carboxylic acids,
80 parts of water, the neutralizer raw material is as follows by weight: 3-6 parts of neutralizer, 200-300 parts of water.
2. a kind of clear-water concrete low entraining type polycarboxylate water-reducer according to claim 1, it is characterised in that: described normal
Advising polyether macromonomer is methyl allyl alcohol polyoxyethylene ether or isoamyl alcohol polyoxyethylene ether, and molecular weight is the road (2400-3000)
Er Dun.
3. a kind of clear-water concrete low entraining type polycarboxylate water-reducer according to claim 1, it is characterised in that: the phosphorus
Sour disodium hydrogen and sodium dihydrogen phosphate are anhydrous state.
4. a kind of clear-water concrete low entraining type polycarboxylate water-reducer according to claim 1, it is characterised in that: described embedding
Section polyether monomer is EO/PO block polyether, and the EO/PO degree of polymerization is 10-30, and molecular structure is as follows:
5. a kind of clear-water concrete low entraining type polycarboxylate water-reducer according to claim 1, it is characterised in that: the phosphorus
Acid esters be 2-hydroxyethyl methacrylate phosphate (HEMAP) or 1- hydroxyl ethyl ester methacrylate phosphate (UPE), point
Minor structure is as follows:
6. a kind of clear-water concrete low entraining type polycarboxylate water-reducer according to claim 1, it is characterised in that: the oxygen
Agent be concentration be 27.5% hydrogen peroxide, ammonium persulfate, one of potassium peroxydisulfate or a variety of.
7. a kind of clear-water concrete low entraining type polycarboxylate water-reducer according to claim 1, it is characterised in that: described to go back
Former agent is one of the anti-sepsis acid of L-, sodium formaldehyde sulfoxylate and sodium sulfite or a variety of, and the chain-transferring agent is mercaptopropionic acid or sulfydryl
Acetic acid.
8. a kind of clear-water concrete low entraining type polycarboxylate water-reducer according to claim 1, it is characterised in that: it is described not
Full carboxylic acid is one of acrylic acid, methacrylic acid or a variety of, and the esters of unsaturated carboxylic acids is ethyl acrylate, acrylic acid is different
One of propyl ester and isobutyl acrylate are a variety of, and the neutralizer is one of sodium hydroxide, potassium hydroxide or a variety of.
9. a kind of clear-water concrete low entraining type polycarboxylate water-reducer according to claim 1, it is characterised in that: the water
Industry water for deionized water or conductivity less than 20 μ S/cm.
10. a kind of preparation method of clear-water concrete low entraining type polycarboxylate water-reducer described in claim 1, feature exist
In: include the following steps:
S1: it prepares bottom material: conventional polyether monomer, block polyether monomer, phosphate and deionized water being added in reaction kettle, room temperature
Lower stirring, is completely dissolved raw material, obtains reaction bottom material；
S2: it prepares dropping liquid A: load weighted reducing agent and chain-transferring agent being added in deionized water, stirs evenly, is added dropwise
Liquid A；
S3: it prepares dropping liquid B: load weighted unsaturated carboxylic acid, esters of unsaturated carboxylic acids being added in deionized water, stirred evenly,
Obtain dropping liquid B；
S4: by load weighted oxidant be added bottom material in, stir 5-10 minutes, be then at the uniform velocity added dropwise into reaction kettle respectively A liquid,
B liquid, control A liquid time for adding 3.5-4.0h, B liquid time for adding are 3.0-3.5h, drip subsequent continuation of insurance temperature 1.0-2.0h；
S5: after the reaction was completed, neutralizer is added and deionized water adjusts pH value of solution as 5-7, obtains the clear water that solid content is 40%
Concrete low entraining type polycarboxylate water-reducer.
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| CN111303352A (en) * | 2020-03-04 | 2020-06-19 | 山西佳维新材料股份有限公司 | Polycarboxylate superplasticizer and preparation method thereof |
| CN111333361A (en) * | 2020-03-10 | 2020-06-26 | 刘翠芬 | High belite sulphoaluminate cement concrete additive |
| CN111439947A (en) * | 2020-03-26 | 2020-07-24 | 浙江和业科技有限公司 | Low-air-entraining slow-setting type polycarboxylate superplasticizer and preparation method thereof |
| CN113200703A (en) * | 2021-05-12 | 2021-08-03 | 北京金隅水泥节能科技有限公司 | Low-air-entraining polycarboxylic acid type water reducing agent and preparation method thereof |
| WO2022142125A1 (en) * | 2020-12-29 | 2022-07-07 | 江苏尼高科技有限公司 | Viscosity reduction type concrete polycarboxylic acid water-reducing agent and preparation method therefor |
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| CN111303352A (en) * | 2020-03-04 | 2020-06-19 | 山西佳维新材料股份有限公司 | Polycarboxylate superplasticizer and preparation method thereof |
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| WO2022142125A1 (en) * | 2020-12-29 | 2022-07-07 | 江苏尼高科技有限公司 | Viscosity reduction type concrete polycarboxylic acid water-reducing agent and preparation method therefor |
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