CN109021181A - A kind of poly carboxylic acid series water reducer and preparation method thereof for having both viscosity reduction and protecting function of collapsing - Google Patents
A kind of poly carboxylic acid series water reducer and preparation method thereof for having both viscosity reduction and protecting function of collapsing Download PDFInfo
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- CN109021181A CN109021181A CN201810948450.1A CN201810948450A CN109021181A CN 109021181 A CN109021181 A CN 109021181A CN 201810948450 A CN201810948450 A CN 201810948450A CN 109021181 A CN109021181 A CN 109021181A
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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
- C04B24/24—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
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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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Abstract
The invention discloses a kind of poly carboxylic acid series water reducers and preparation method thereof for having both viscosity reduction and protecting function of collapsing, and belong to building material technical field.Poly carboxylic acid series water reducer in the present invention is by unsaturated polyether monomer I, unsaturated block modified polyether monomer II, unsaturated carboxylic acid class monomer, unsaturated carboxylic acid alkyl ester, unsaturated phosphate ester class monomer, chain-transferring agent, oxidant, reducing agent and deionized water at 15~30 DEG C, polymerize by aqueous free radical, then plus lye adjust pH moisturizing be prepared.It can not only meet high-strength concrete diminishing and it is slump-retaining can requirement, concrete viscosity can more be greatly lowered, hence it is evident that the working performance for improving high-strength concrete, solving the problems, such as previous polycarboxylate water-reducer to collapse, to damage fast and viscosity excessive.Preparation method can be not necessarily to heat source in ordinary temperature production in the present invention, have many advantages, such as that production equipment is simple, rational technology, easy to operate, high production efficiency, suitable industrialized production and popularization.
Description
Technical field
The invention belongs to technical field of concrete additives, and in particular to a kind of poly- carboxylic for having both viscosity reduction and protecting function of collapsing
Sour based water reducer and preparation method thereof.
Background technique
With the rapid development of our country's economy with the raising of building level, concrete quality is required also higher and higher.It is poly-
Carboxylic acid series high-performance dehydragent is a new generation's building water-reducing agent that China occurs and applies in recent years, with water-reducing rate height, is mixed
It measures that low, concrete slump loss is small, a series of excellent properties such as environmentally protective, has adapted to the development of high performance concrete, mesh
Before be widely used to the engineering fields such as real estate building, highway, railway, bridge, water conservancy and water power.
With the development of concrete technology, concrete is gradually strided forward to the direction that high-strength, superelevation is strengthened.High grade coagulation
Soil usually obtains the intensity and endurance quality of superelevation by reducing water-cement ratio, in high-speed rail, bridge, dam and aerospace
Application in building has become extensive.Although high-grade concrete has preferable mechanical property, the concrete prepared often is deposited
In the problem that large viscosity, flow velocity are slow, it is unfavorable for the transport and construction of concrete, therefore the additive of concrete batching is proposed
Higher requirement.
Currently, generalling use the volume for improving cement water reducing agent, especially to solve the viscosity problem of high-grade concrete
It is more higher, better poly carboxylic acid series water reducers of collapse protection type using water-reducing rate.But common poly carboxylic acid series water reducer is gone back at present
In the presence of it is more sensitive to construction material and environment, compared with the effect of cement the deficiencies of lag, common poly carboxylic acid series water reducer
It is too long gently then to occur concrete coagulating time when volume is excessive, influences construction speed, it is heavy then cause later concrete bleeding tight
Weight, seriously endangers the construction quality of concrete.Therefore, a kind of to be both able to satisfy high-strength concrete diminishing and slump-retaining energy
It is required that the poly carboxylic acid series water reducer that can reduce high-strength concrete viscosity to a certain extent again seems especially urgent.
In order to solve the above problem, domestic also to have carried out a series of research inventions, CN105924592A discloses a kind of viscosity reduction type
Poly carboxylic acid series water reducer and preparation method thereof, design synthesizes two class water-reducing agent of A, B, and is compounded.This method preparation
The reaction temperature of A class polycarboxylate water-reducer is 30~65 DEG C, and the thermotonus temperature of B class water-reducing agent is 40~65 DEG C, reaction temperature
Degree is higher, and production cost is higher, and the production cycle is longer, and the polyether monomer TPEG molecular weight of A class polycarboxylate water-reducer is
600, intensity is influenced.103865007 A of CN discloses a kind of viscosity reduction type poly carboxylic acid series water reducer preparation method, with nothing
Rule polyoxyalkylenes ether unsaturated acid ester, unsaturated modified polyoxyethylene ether, unsaturated acids Arrcostab, (methyl) acrylic acid exist
Under initiator and molecular weight regulator effect, alkali neutralization is added to be prepared again by aqueous solution copolymerization.The invention is total in carboxylic acid
A certain amount of hydrophobic units and hydrophobic grouping are introduced and controlled in polymers molecular structure, and playing the role of, which reduces the water-reducing agent, is lauched
The effect of cement-based material viscosity, but this method reaction temperature is 50~70 DEG C, and reaction temperature is higher, and production is difficult to control.
Summary of the invention
In view of the deficiency of the prior art, the present invention provides a kind of polycarboxylic-acid for having both viscosity reduction and protecting function of collapsing
Water-reducing agent, the water-reducing agent can be used alone, and can also be used in compounding with common high-performance water reducing agent, and the present invention is in polycarboxylic acids point
A certain amount of hydrophobic grouping and eluting group are introduced in minor structure, have both been able to satisfy high-strength concrete diminishing and the slump is kept
Performance requirement, and the viscosity of high-strength concrete can be reduced to a certain extent.
Meanwhile the present invention also provides the preparation method for having both viscosity reduction with the poly carboxylic acid series water reducer for protecting function of collapsing, the party
Method be not necessarily to heat source, can in ordinary temperature production, have many advantages, such as production equipment simply, rational technology, easy to operate, high production efficiency,
It is suitble to industrialized production and popularization.
The technical scheme adopted by the invention is that: a kind of poly carboxylic acid series water reducer for having both viscosity reduction and protecting function of collapsing is provided,
Poly carboxylic acid series water reducer is reacted by the raw material of following mass fraction to be made: 350~380 parts of comonomer, oxidant 3.0~4.0
Part, 0.5~1.5 part of reducing agent, 1.5~2.0 parts of chain-transferring agent, 450~500 parts of deionized water；The comonomer includes not
It is saturated polyether monomer I, unsaturated block modified polyether monomer II, unsaturated carboxylic acid class monomer, unsaturated carboxylic acid alkyl ester and not
Be saturated phosphoric acid ester monomer, wherein the amounts of two kinds of unsaturated polyether monomer total materials, the amount of unsaturated carboxylic acid class monomeric substance,
The amount of unsaturated carboxylic acid alkyl ester substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.0~3.5:0.2
~0.5:0.5~1.0.
The present invention based on the above technical solution, can do improvement further below:
Further, unsaturated polyether monomer I is isoamyl alcohol polyoxyethylene ether, in isobutene alcohol polyoxyethylene ether
One or two, molecular weight are 1000~1200.
Further, unsaturated block modified polyether monomer II is prenol polyoxyethylene poly-oxygen propylene aether, molecule
For structure by ethylene oxide and propylene oxide molecule segment block, molecular weight is 4000~4500.
Further, unsaturated carboxylic acid class monomer is acrylic acid, methacrylic acid, maleic anhydride, fumaric acid and itaconic acid
One of or it is a variety of, its quality proportioning is arbitrary when multiple combinations.
Further, unsaturated carboxylic acid alkyl ester is methyl acrylate, methyl methacrylate, ethyl acrylate, methyl
One of ethyl acrylate, propyl acrylate, propyl methacrylate, butyl acrylate and butyl methacrylate are more
Kind, its quality proportioning is arbitrary when multiple combinations.
Further, unsaturated phosphate ester class monomer is vinyl phosphoric acid dimethyl ester, allyl dimethyl phosphate and methyl
One of acrylic acid -2- hydroxyl ethyl ester phosphate is a variety of, its quality proportioning is arbitrary when multiple combinations.
Further, chain-transferring agent is one of mercaptopropionic acid, thioacetic acid, mercaptoethanol and lauryl mercaptan
Or it is a variety of, its quality proportioning is arbitrary when multiple combinations, and the dosage of chain-transferring agent is preferably unsaturated polyether monomer gross mass
The 0.5~1.0% of (the block modified unsaturated polyether monomer II of low molecular weight unsaturated polyether I+high molecular weight of monomer).
Further, oxidant is one of hydrogen peroxide, ammonium persulfate, potassium peroxydisulfate and sodium peroxydisulfate or a variety of, more
Kind combination when its quality proportioning be arbitrary, the dosage of oxidant be preferably unsaturated polyether monomer gross mass 1.0~
1.5%.
Further, reducing agent is vitamin C, sodium formaldehyde sulfoxylate, green vitriol, frerrous chloride, sodium sulfite, sulphur
One of sodium thiosulfate, sodium hypophosphite, sodium hydrogensulfite, sodium dithionate and sodium pyrosulfite are a variety of, their quality
Proportion is arbitrary；The dosage of reducing agent is the 0.2~0.5% of unsaturated polyether monomer gross mass.
Had both in the present invention viscosity reduction and protect collapse function poly carboxylic acid series water reducer preparation method the following steps are included:
1. by unsaturated polyether monomer I, unsaturated block modified polyether monomer II and part unsaturated carboxylic acid class monomer
It is added in reaction kettle with deionized water, stirring and dissolving is uniform, is configured to the primer solution that mass fraction is 50~60%；
2. reducing agent, chain-transferring agent and deionized water are mixed, it is configured to the solution A that mass fraction is 1.0~2.5%；
Remaining unsaturated carboxylic acid class monomer, unsaturated carboxylic acid alkyl ester and unsaturated phosphate ester class monomer and deionized water are mixed
It closes, is configured to the solution B that mass fraction is 40~55%；
3. being added into reaction kettle by the mass fraction that oxidant and remaining deionized water mixing are made into is 7.5~15%
Solution, and stir 2~5min, obtain mixing primer solution；
4. solution A is first added drop-wise to step 3. mixing obtained at 15~30 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 2.5~3.0h, starts to be added dropwise solution B again to step after 5~10min is added dropwise
Suddenly 3. in mixing primer solution obtained, the time for adding for controlling solution B is 2.0~2.5h, after two kinds of solution are added dropwise,
Continuing 1.0~1.5h of stirring, the sodium hydroxide solution for being finally 30% with mass fraction adjusts solution ph to 5.0~7.0,
Moisturizing is uniformly mixing to obtain the poly carboxylic acid series water reducer for having both viscosity reduction and protecting function of collapsing that solid content is 40wt%.
The beneficial effects of the present invention are:
(1) poly carboxylic acid series water reducer for having both viscosity reduction and protecting function of collapsing of the invention is poly- using the unsaturation of low molecular weight
Ether monomer and the progress of the block unsaturated polyether monomer of high molecular weight are free-radical polymerized, and introducing is certain in the molecular structure hates
Water base group reduces its hydrophilic lipophilic balance (HLB value), reduces it with water generation and is combined water, releases more Free waters.
(2) introducing in the poly carboxylic acid series water reducer molecular structure for having both viscosity reduction and protecting function of collapsing of the invention has sustained release
The phosphate group of function makes with phosphate radical on polycarboxylate water-reducer molecule side chain, and there are two negative electrical charges for phosphate radical tool, to water
Mud has stronger adsorption capacity, improves the competitive Adsorption ability with the sulfate ion in cement, improves dispersibility, both
It is able to satisfy high-strength concrete diminishing and slump-retaining energy requires, and high-grade concrete can be reduced to a certain extent
Viscosity.
(3) present invention is synthesized with room temperature, using water soluble oxidized-reduction initiating system, by adjusting oxidationreduction body
Oxidant and reducing agent dosage, reduce decomposition of initiator into the activation energy of free radical, to realize under normal cryogenic conditions in system
Raolical polymerizable.
(4) poly carboxylic acid series water reducer prepared by the present invention for having both viscosity reduction and protecting function of collapsing, can be used alone, can also
To be used in compounding with common high-performance water reducing agent, it can be substantially reduced the viscosity of high-strength concrete to a certain extent, mix simultaneously
Solidifying soil is slump-retaining can be good.
(5) the preparation method production equipment of the invention is simple, rational technology, strong operability, high production efficiency, fits
Close industrialized production and popularization.
Specific embodiment
The present invention is higher in order to solve the problems, such as strong concrete viscosity, provides that one kind has both viscosity reduction and guarantor is collapsed function
Poly carboxylic acid series water reducer and preparation method thereof, the water-reducing agent in the present invention is by comonomer, oxidant, reducing agent, chain tra nsfer
Agent and deionized water are made by polymerization reaction, wherein comonomer includes unsaturated polyether monomer I, unsaturated block modified
Polyether monomer II, unsaturated carboxylic acid class monomer, unsaturated carboxylic acid alkyl ester and unsaturated phosphate ester class monomer, unsaturation are poly-
Ether monomer I is one of isoamyl alcohol polyoxyethylene ether and isobutene alcohol polyoxyethylene ether or two kinds, and molecular weight is
1000~1200, preferably 1200；Unsaturated block modified polyether monomer II is prenol polyoxyethylene poly-oxygen propylene aether,
For its molecular structure by ethylene oxide and propylene oxide molecule segment block, molecular weight is 4000~4500, preferably 4000；
The dosage of chain-transferring agent is preferably the 0.5~1.0% of unsaturated polyether monomer gross mass, and the dosage of oxidant is preferably insatiable hunger
With the 1.0~1.5% of polyether monomer gross mass, the dosage of reducing agent be preferably unsaturated polyether monomer gross mass 0.2~
0.5%.
Below with reference to embodiment, specific embodiments of the present invention will be described in detail.
Embodiment 1
Present embodiments provide it is a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, the water-reducing agent by
357.4g comonomer, 3.6g oxidant, 0.6g reducing agent, 1.56g chain-transferring agent and 465g deionized water pass through polymerization reaction
It is made, amount, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid alkane of two of them unsaturated polyether monomer total material
The amount of base ester substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.45:0.28:0.82, chain-transferring agent
Dosage is the 0.52% of unsaturated polyether monomer gross mass, and the dosage of oxidant is unsaturated polyether monomer gross mass
1.2%, the dosage of reducing agent is the 0.2% of unsaturated polyether monomer gross mass.
Above-mentioned poly carboxylic acid series water reducer specific for having both viscosity reduction and protecting function of collapsing the preparation method is as follows:
1. by 120g molecular weight be 1200 isobutene alcohol polyoxyethylene ether, 180g molecular weight be 4000 prenol
Polyoxyethylene poly-oxygen propylene aether, 8.6g acrylic acid and 260g deionized water are added in reaction kettle, and stirring and dissolving is uniform；
2. 0.35g vitamin C, 0.25g sodium hydrogensulfite and 1.56g mercaptopropionic acid and 125g deionized water are mixed, match
Solution A is made；27.5g acrylic acid, 3.5g methyl acrylate and 17.8g allyl dimethyl phosphate and 60g deionized water are mixed
It closes, is configured to solution B；
3. the solution being made of 1.2g hydrogen peroxide, 2.4g ammonium persulfate and 20g deionized water is added into reaction kettle, and
3min is stirred, mixing primer solution is obtained；
4. solution A is first added drop-wise to step 3. mixing obtained at 20~25 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 3.0h, and it is 3. obtained to step to start dropwise addition solution B again after dropwise addition 5min
It mixes in primer solution, the time for adding for controlling solution B is 2.5h, after two kinds of solution are added dropwise, continues to stir 1.0h, most
The sodium hydroxide solution for being afterwards 30% with mass fraction adjusts solution ph to 5.0~7.0, and moisturizing is uniformly mixing to obtain and contains admittedly
The poly carboxylic acid series water reducer product (number JL-PCE-1) for having both viscosity reduction and protecting function of collapsing that amount is 40wt%.
Embodiment 2
Present embodiments provide it is a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, the water-reducing agent by
370.7g comonomer, 4.0g oxidant, 0.65g reducing agent, 1.56g chain-transferring agent and 465g deionized water are anti-by polymerization
It should be made, amount, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid of two of them unsaturated polyether monomer total material
The amount of Arrcostab substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.2:0.31:0.52, chain-transferring agent
Dosage be the 0.64% of unsaturated polyether monomer gross mass, the dosage of oxidant is unsaturated polyether monomer gross mass
1.33%, the dosage of reducing agent is the 0.22% of unsaturated polyether monomer gross mass.
Above-mentioned poly carboxylic acid series water reducer specific for having both viscosity reduction and protecting function of collapsing the preparation method is as follows:
1. by 180g molecular weight be 1200 isoamyl alcohol polyoxyethylene ether, 120g molecular weight be 4000 prenol
Polyoxyethylene poly-oxygen propylene aether, 8g maleic anhydride and 255g deionized water are added in reaction kettle, and stirring and dissolving is uniform；
2. 0.45g vitamin C, 0.2g sodium hypophosphite, 1.92g thioacetic acid and 130g deionized water are mixed, prepare
At solution A；By 35.6g acrylic acid, 5.6g methyl methacrylate and 21.5g 2-hydroxyethyl methacry-late phosphate and
The mixing of 55g deionized water, is configured to solution B；
3. the solution being made of 2.4g hydrogen peroxide, 1.6g potassium peroxydisulfate and 25g deionized water is added into reaction kettle, and
2min is stirred, mixing primer solution is obtained；
4. solution A is first added drop-wise to step 3. mixing obtained at 20~25 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 3.0h, and it is 3. obtained to step to start dropwise addition solution B again after dropwise addition 8min
It mixes in primer solution, the time for adding for controlling solution B is 2.5h, after two kinds of solution are added dropwise, continues to stir 1.0h, most
The sodium hydroxide solution for being afterwards 30% with mass fraction adjusts solution ph to 5.0~7.0, and moisturizing is uniformly mixing to obtain and contains admittedly
The poly carboxylic acid series water reducer product (number JL-PCE-2) for having both viscosity reduction and protecting function of collapsing that amount is 40wt%.
Embodiment 3
Present embodiments provide it is a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, the water-reducing agent by
368.5g comonomer, 4.2g oxidant, 1.21g reducing agent, 1.6g chain-transferring agent and 470g deionized water pass through polymerization reaction
It is made, amount, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid alkane of two of them unsaturated polyether monomer total material
The amount of base ester substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.22:0.27:0.58, chain-transferring agent
Dosage is the 0.53% of unsaturated polyether monomer gross mass, and the dosage of oxidant is unsaturated polyether monomer gross mass
1.4%, the dosage of reducing agent is the 0.4% of unsaturated polyether monomer gross mass.
Above-mentioned poly carboxylic acid series water reducer specific for having both viscosity reduction and protecting function of collapsing the preparation method is as follows:
1. by 200g molecular weight be 1200 isobutene alcohol polyoxyethylene ether, 100g molecular weight be 4000 prenol
Polyoxyethylene poly-oxygen propylene aether, 9.6g fumaric acid and 240g deionized water are added in reaction kettle, and stirring and dissolving is uniform；
2. 1.2g sodium formaldehyde sulfoxylate, 0.01g green vitriol, 0.4g thioacetic acid, 1.2g mercaptopropionic acid and 135g are gone
Ionized water mixing, is configured to solution A；By 38.5g acrylic acid, 5.2g ethyl acrylate and 15.2 g vinyl phosphoric acid dimethyl esters and
The mixing of 60g deionized water, is configured to solution B；
3. the solution being made of 2.4g hydrogen peroxide, 1.8g sodium peroxydisulfate and 25g deionized water is added into reaction kettle, and
4min is stirred, mixing primer solution is obtained；
4. solution A is first added drop-wise to step 3. mixing obtained at 15~25 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 2.5h, and it is 3. obtained to step to start dropwise addition solution B again after dropwise addition 6min
It mixes in primer solution, the time for adding for controlling solution B is 2.0h, after two kinds of solution are added dropwise, continues to stir 1.5h, most
The sodium hydroxide solution for being afterwards 30% with mass fraction adjusts solution ph to 5.0~7.0, and moisturizing is uniformly mixing to obtain and contains admittedly
The poly carboxylic acid series water reducer product (number JL-PCE-3) for having both viscosity reduction and protecting function of collapsing that amount is 40wt%.
Embodiment 4
Present embodiments provide it is a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, the water-reducing agent by
360.9g comonomer, 4.2g oxidant, 0.88g reducing agent, 1.58g chain-transferring agent and 470g deionized water are anti-by polymerization
It should be made, amount, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid of two of them unsaturated polyether monomer total material
The amount of Arrcostab substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.23:0.28:0.61, chain-transferring agent
Dosage be the 0.53% of unsaturated polyether monomer gross mass, the dosage of oxidant is unsaturated polyether monomer gross mass
1.4%, the dosage of reducing agent is the 0.29% of unsaturated polyether monomer gross mass.
Above-mentioned poly carboxylic acid series water reducer specific for having both viscosity reduction and protecting function of collapsing the preparation method is as follows:
1. by 100g molecular weight be 1200 isoamyl alcohol polyoxyethylene ether, 200g molecular weight be 4000 prenol
Polyoxyethylene poly-oxygen propylene aether, 7.5g maleic anhydride and 250g deionized water are added in reaction kettle, and stirring and dissolving is uniform；
2. 0.32g vitamin C, 0.56g sodium sulfite, 1.58g mercaptopropionic acid and 125g deionized water are mixed, prepare
At solution A；By 30.5g methacrylic acid, 4.3g propyl acrylate, 18.6g 2-hydroxyethyl methacry-late phosphate and 65g
Deionized water mixing, is configured to solution B；
3. the solution being made of 1.8g hydrogen peroxide, 2.4g potassium peroxydisulfate and 30g deionized water is added into reaction kettle, and
4min is stirred, mixing primer solution is obtained；
4. solution A is first added drop-wise to step 3. mixing obtained at 20~30 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 2.5h, and it is 3. obtained to step to start dropwise addition solution B again after dropwise addition 6min
It mixes in primer solution, the time for adding for controlling solution B is 2.0h, after two kinds of solution are added dropwise, continues to stir 1.5h, most
The sodium hydroxide solution for being afterwards 30% with mass fraction adjusts solution ph to 5.0~7.0, and moisturizing is uniformly mixing to obtain and contains admittedly
The poly carboxylic acid series water reducer product (number JL-PCE-4) for having both viscosity reduction and protecting function of collapsing that amount is 40wt%.
Embodiment 5
Present embodiments provide it is a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, the water-reducing agent by
359.7g comonomer, 4.2g oxidant, 1.21g reducing agent, 2.0g chain-transferring agent and 480g deionized water pass through polymerization reaction
It is made, amount, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid alkane of two of them unsaturated polyether monomer total material
The amount of base ester substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.0:0.2:0.6, the use of chain-transferring agent
Amount is the 0.67% of unsaturated polyether monomer gross mass, and the dosage of oxidant is the 1.4% of unsaturated polyether monomer gross mass,
The dosage of reducing agent is the 0.4% of unsaturated polyether monomer gross mass.
Above-mentioned poly carboxylic acid series water reducer specific for having both viscosity reduction and protecting function of collapsing the preparation method is as follows:
1. by 120g molecular weight be 1200 isoamyl alcohol polyoxyethylene ether, 180g molecular weight be 4000 prenol
Polyoxyethylene poly-oxygen propylene aether, 10.2g itaconic acid and 260g deionized water are added in reaction kettle, and stirring and dissolving is uniform；
2. by 0.8g sodium formaldehyde sulfoxylate, 0.4g sodium pyrosulfite, 0.01g green vitriol, 2.0g mercaptoethanol and 130g
Deionized water mixing, is configured to solution A；By 28.8g acrylic acid, 4.8g butyl acrylate, 15.9g allyl dimethyl phosphate
It is mixed with 65g deionized water, is configured to solution B；
3. the solution being made of 4.2g ammonium persulfate and 25g deionized water is added into reaction kettle, and 5min is stirred, obtained
To mixing primer solution；
4. solution A is first added drop-wise to step 3. mixing obtained at 15~25 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 3.0h, and it is 3. obtained to step to start dropwise addition solution B again after dropwise addition 5min
It mixes in primer solution, the time for adding for controlling solution B is 2.5h, after two kinds of solution are added dropwise, continues to stir 1.0h, most
The sodium hydroxide solution for being afterwards 30% with mass fraction adjusts solution ph to 5.0~7.0, and moisturizing is uniformly mixing to obtain and contains admittedly
The poly carboxylic acid series water reducer product (number JL-PCE-5) for having both viscosity reduction and protecting function of collapsing that amount is 40wt%.
Embodiment 6
Present embodiments provide it is a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, the water-reducing agent by
362.5g comonomer, 3.6g oxidant, 0.75g reducing agent, 1.86g chain-transferring agent and 465g deionized water are anti-by polymerization
It should be made, amount, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid of two of them unsaturated polyether monomer total material
The amount of Arrcostab substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.3:0.22:0.62, chain-transferring agent
Dosage be the 0.62% of unsaturated polyether monomer gross mass, the dosage of oxidant is unsaturated polyether monomer gross mass
1.2%, the dosage of reducing agent is the 0.25% of unsaturated polyether monomer gross mass.
Above-mentioned poly carboxylic acid series water reducer specific for having both viscosity reduction and protecting function of collapsing the preparation method is as follows:
1. by 180g molecular weight be 1200 isobutene alcohol polyoxyethylene ether, 120g molecular weight be 4000 prenol
Polyoxyethylene poly-oxygen propylene aether, 7.6g acrylic acid and 250g deionized water are added in reaction kettle, and stirring and dissolving is uniform；
2. 0.55g vitamin C, 0.2g sodium thiosulfate, 1.86g thioacetic acid and 125g deionized water are mixed, prepare
At solution A；By 35.2g acrylic acid, 4.5g ethyl methacrylate, 15.2g vinyl phosphoric acid dimethyl ester and 60g deionized water
Mixing, is configured to solution B；
3. the solution being made of 3.6g ammonium persulfate and 30g deionized water is added into reaction kettle, and 4min is stirred, obtained
To mixing primer solution；
4. solution A is first added drop-wise to step 3. mixing obtained at 15~25 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 2.5h, and it is 3. obtained to step to start dropwise addition solution B again after dropwise addition 6min
It mixes in primer solution, the time for adding for controlling solution B is 2.0h, after two kinds of solution are added dropwise, continues to stir 1.5h, most
The sodium hydroxide solution for being afterwards 30% with mass fraction adjusts solution ph to 5.0~7.0, and moisturizing is uniformly mixing to obtain and contains admittedly
The poly carboxylic acid series water reducer product (number JL-PCE-6) for having both viscosity reduction and protecting function of collapsing that amount is 40wt%.
Embodiment 7
Present embodiments provide it is a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, the water-reducing agent by
379.8g comonomer, 4.5g oxidant, 0.8g reducing agent, 2.1g chain-transferring agent and 465g deionized water pass through polymerization reaction
It is made, amount, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid alkane of two of them unsaturated polyether monomer total material
The amount of base ester substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.11:0.21:0.6, chain-transferring agent
Dosage is the 0.7% of unsaturated polyether monomer gross mass, and the dosage of oxidant is the 1.5% of unsaturated polyether monomer gross mass,
The dosage of reducing agent is the 0.27% of unsaturated polyether monomer gross mass.
Above-mentioned poly carboxylic acid series water reducer specific for having both viscosity reduction and protecting function of collapsing the preparation method is as follows:
1. by 220g molecular weight be 1200 isobutene alcohol polyoxyethylene ether, 80g molecular weight be 4000 prenol gather
Ethylene oxide polyethenoxy ether, 11.8g acrylic acid and 250g deionized water are added in reaction kettle, and stirring and dissolving is uniform；
2. 0.56g vitamin C, 0.24g sodium dithionite, 2.1g lauryl mercaptan and 125g deionized water are mixed
It closes, is configured to solution A；By 42g acrylic acid, 6.5g butyl acrylate, 19.5g vinyl phosphoric acid dimethyl ester and 60g deionized water
Mixing, is configured to solution B；
3. the solution being made of 2.4g hydrogen peroxide, 2.1g ammonium persulfate and 25g deionized water is added into reaction kettle, and
3min is stirred, mixing primer solution is obtained；
4. solution A is first added drop-wise to step 3. mixing obtained at 20~25 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 3.0h, and it is 3. obtained to step to start dropwise addition solution B again after dropwise addition 7min
It mixes in primer solution, the time for adding for controlling solution B is 2.5h, after two kinds of solution are added dropwise, continues to stir 1.0h, most
The sodium hydroxide solution for being afterwards 30% with mass fraction adjusts solution ph to 5.0~7.0, and moisturizing is uniformly mixing to obtain and contains admittedly
The poly carboxylic acid series water reducer product (number JL-PCE-7) for having both viscosity reduction and protecting function of collapsing that amount is 40wt%.
Embodiment 8
Present embodiments provide it is a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, the water-reducing agent by
355.8g comonomer, 3.6g oxidant, 0.66g reducing agent, 1.56g chain-transferring agent and 460g deionized water are anti-by polymerization
It should be made, amount, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid of two of them unsaturated polyether monomer total material
The amount of Arrcostab substance and the ratio between the amount of unsaturated phosphate ester class monomeric substance are as follows: 1.0:3.25:0.22:0.61, chain-transferring agent
Dosage be the 0.52% of unsaturated polyether monomer gross mass, the dosage of oxidant is unsaturated polyether monomer gross mass
1.2%, the dosage of reducing agent is the 0.22% of unsaturated polyether monomer gross mass.
Above-mentioned poly carboxylic acid series water reducer specific for having both viscosity reduction and protecting function of collapsing the preparation method is as follows:
1. by 80g molecular weight be 1000 isobutene alcohol polyoxyethylene ether, 220g molecular weight be 4000 prenol gather
Ethylene oxide polyethenoxy ether, 7.2g methacrylic acid and 250g deionized water are added in reaction kettle, and stirring and dissolving is uniform；
2. 0.36g vitamin C, 0.28g sodium hypophosphite, 1.56g mercaptopropionic acid and 125g deionized water are mixed, match
Solution A is made；By 25.6g acrylic acid, 4.2g butyl methacrylate, 18.8g 2-hydroxyethyl methacry-late phosphate and
The mixing of 60g deionized water, is configured to solution B；
3. the solution being made of 3.6g ammonium persulfate and 25g deionized water is added into reaction kettle, and 5 min are stirred, obtained
To mixing primer solution；
4. solution A is first added drop-wise to step 3. mixing obtained at 20~25 DEG C, using constant flow pump by reactor temperature
In primer solution, the time for adding for controlling solution A is 3.0h, and it is 3. obtained to step to start dropwise addition solution B again after dropwise addition 5min
It mixes in primer solution, the time for adding for controlling solution B is 2.5h, after two kinds of solution are added dropwise, continues to stir 1.0h, most
The sodium hydroxide solution for being afterwards 30% with mass fraction adjusts solution ph to 5.0~7.0, and moisturizing is uniformly mixing to obtain and contains admittedly
The poly carboxylic acid series water reducer product (number JL-PCE-8) for having both viscosity reduction and protecting function of collapsing that amount is 40wt%.
Test example
Water-reducing agent in the present invention can be used separately as water-reducing agent, and can also compound with common high-performance water reducing agent makes
With.The present invention in use, identical as the conventional application method of polycarboxylate water-reducer, that is, is added into separately as water-reducing agent
Into concrete, volume is 0.10%~0.30% (rolling over solid percentage volume) of cementitious material.The present invention and common diminishing
When agent is used in compounding, it can be compounded by a certain percentage with common high-performance water reducing agent, the water-reducing agent after compounding gathers with conventional
The application method of carboxylic acid water reducer is identical, i.e., the water-reducing agent after compounding is added in concrete, and volume is cementitious material
0.10%~0.30% (rolling over solid percentage volume).
The poly carboxylic acid series water reducer produced by the present invention for having both viscosity reduction and protecting function of collapsing is tested as follows below:
(1) cement mortar fluidity is tested
1. the initial fluidity of cement mortar and through when mobility referring to GB 50119-2013 " concrete admixture application
Technical specification " it is tested, the match ratio of mortar is shown in Table 1, and fixed water-cement ratio is 0.4, and the initial flow degree of cement mortar controls
In 200~250mm.Test that cement mortar is initial, fluidity performance of 1h, 2h, V funnel testing referring to CECS203:2006 " from
Air-free concrete application technology regulation " in method test mortar pass through funnel flow time.
1 mortar mix ratio of table
2. the performance of the poly carboxylic acid series water reducer for having both viscosity reduction and protecting function of collapsing synthesized in evaluation Examples 1 to 8, choosing
With Sichuan Tong Zhou Chemical Industry Science Co., Ltd produce the common water reducing type high-performance water reducing agent of polycarboxylic acids series TZ-GC, by its with
Poly carboxylic acid series water reducer, the commercially available viscosity reduction type polycarboxylate water-reducer for having both viscosity reduction and protecting function of collapsing synthesized in Examples 1 to 8
JL-PCE-A (solid content is 40%) is as a comparison sample and compounds sample, and water-reducing agent is mixed when being used alone and being used in compounding
Amount is 0.12% (rolling over solid percentage volume).Test result see the table below 2 and table 3.
Mortar'S Flowability variation and flow time when table 2 is used alone
Mortar'S Flowability variation and flow time when table 3 is used in compounding
(2) concrete application performance and Mechanics Performance Testing
The test of concrete application performance is referring to " the Standard for test methods of properties of ordinary concrete mixture of GB/T 50080-2002
Standard " it carries out, concrete mix is shown in Table 4, selects the polycarboxylic acids series TZ- of Sichuan Tong Zhou Chemical Industry Science Co., Ltd production
The polycarboxylic-acid diminishing for having both viscosity reduction and protecting function of collapsing synthesized in the common high-performance water reducing agent mother liquor of GC and Examples 1 to 8
Agent, commercially available viscosity reduction type polycarboxylate water-reducer JL-PCE-A (solid content is 40%) compare test under the same conditions, press
Mass ratio 7:3 is used in compounding, and water-reducing agent volume is 0.20% (rolling over solid percentage volume), the initial flow degree control of concrete
In 550~590mm.Concrete mixture characteristic survey is carried out according to JGJ 281-2012 " high-strength concrete application technology regulation "
(the emptying of product configuration concrete viscosity situation is evaluated in examination using the emptying time of the measurement bucket of falling slump concrete mix
Time is shorter, and concrete viscosity is smaller, and viscosity reducing effect is more significant).
The slump and divergence of initial 0h, 1h, 2h of record test concrete mix respectively, unit mm, simultaneously
Record the state of concrete.Mechanical performance of concrete is according to " the normal concrete mechanical property test side GB/T50081-2002
Method " test, test sample dimensions are 3d, 7d, 28d compression strength of the body concrete of 150mm × 150mm × 150mm cubes, are tried
It tests and the results are shown in Table 5.
4 C60 concrete experiments match ratio (kg/m of table3)
The test of 5 working performance of concrete of table
From 5 concrete test result of table, having both viscosity reduction and protecting for synthesizing in the embodiment of the present invention 1~8 is collapsed function
Poly carboxylic acid series water reducer is used in compounding with common high-performance water reducing agent, has both been able to satisfy high-strength concrete diminishing and the slump is protected
Performance requirement is held, and the viscosity of high-strength concrete can be reduced to a certain extent.
Although be described in detail to a specific embodiment of the invention in conjunction with the embodiments, should not be construed as pair
The restriction of the protection scope of this patent.In range described by claims, those skilled in the art are without creative labor
The dynamic various modifications that can be made and deformation still belong to the protection scope of this patent.
Claims (10)
1. a kind of have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, which is characterized in that the poly carboxylic acid series water reducer by
The raw material reaction of following mass fraction is made: 350~380 parts of comonomer, 3.0~4.0 parts of oxidant, and reducing agent 0.5~1.5
Part, 1.5~2.0 parts of chain-transferring agent, 450~500 parts of deionized water；The comonomer includes unsaturated polyether monomer I, insatiable hunger
With block modified polyether monomer II, unsaturated carboxylic acid class monomer, unsaturated carboxylic acid alkyl ester and unsaturated phosphate ester class monomer,
In, the amount of two kinds of unsaturated polyether monomer total materials, the amount of unsaturated carboxylic acid class monomeric substance, unsaturated carboxylic acid alkyl ester substance
Amount and unsaturated phosphate ester class monomeric substance the ratio between amount are as follows: 1.0:3.0~3.5:0.2~0.5:0.5~1.0.
2. according to claim 1 have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, it is characterised in that: it is described not
Saturation polyether monomer I is one or both of isoamyl alcohol polyoxyethylene ether, isobutene alcohol polyoxyethylene ether, and molecular weight is
1000~1200.
3. according to claim 1 have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, it is characterised in that: it is described not
Being saturated block modified polyether monomer II is prenol polyoxyethylene poly-oxygen propylene aether, and molecular structure is by ethylene oxide and epoxy
Propane molecule segment block, molecular weight are 4000~4500.
4. according to claim 1 have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, it is characterised in that: it is described not
Saturated carboxylic acid class monomer is one of acrylic acid, methacrylic acid, maleic anhydride, fumaric acid and itaconic acid or a variety of.
5. according to claim 1 have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, it is characterised in that: it is described not
Saturated carboxylic acid Arrcostab is methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, acrylic acid third
One of ester, propyl methacrylate, butyl acrylate and butyl methacrylate are a variety of.
6. according to claim 1 have both viscosity reduction and protect the poly carboxylic acid series water reducer of function of collapsing, it is characterised in that: it is described not
Saturation phosphoric acid ester monomer is vinyl phosphoric acid dimethyl ester, allyl dimethyl phosphate and 2-hydroxyethyl methacry-late phosphoric acid
One of ester is a variety of.
7. the poly carboxylic acid series water reducer according to claim 1 for having both viscosity reduction and protecting function of collapsing, it is characterised in that: the chain
Transfer agent is one of mercaptopropionic acid, thioacetic acid, mercaptoethanol and lauryl mercaptan or a variety of, and dosage is unsaturation
The 0.5~1.0% of polyether monomer gross mass.
8. the poly carboxylic acid series water reducer according to claim 1 for having both viscosity reduction and protecting function of collapsing, it is characterised in that: the oxygen
Agent is one of hydrogen peroxide, ammonium persulfate, potassium peroxydisulfate and sodium peroxydisulfate or a variety of, and dosage is unsaturated polyether monomer
The 1.0~1.5% of gross mass.
9. the poly carboxylic acid series water reducer according to claim 1 for having both viscosity reduction and protecting function of collapsing, it is characterised in that: described to go back
Former agent be vitamin C, sodium formaldehyde sulfoxylate, green vitriol, frerrous chloride, sodium sulfite, sodium thiosulfate, sodium hypophosphite,
One of sodium hydrogensulfite, sodium dithionate and sodium pyrosulfite are a variety of, and dosage is unsaturated polyether monomer gross mass
0.2~0.5%.
10. the preparation side of the poly carboxylic acid series water reducer as described in any one of claims 1 to 9 for having both viscosity reduction and protecting function of collapsing
Method, which comprises the following steps:
1. by unsaturated polyether monomer I, unsaturated block modified polyether monomer II and part unsaturated carboxylic acid class monomer and going
Ionized water is added in reaction kettle, and stirring and dissolving is uniform, is configured to the primer solution that mass fraction is 50~60%；
2. reducing agent, chain-transferring agent and deionized water are mixed, it is configured to the solution A that mass fraction is 1.0~2.5%；It will be remaining
Under unsaturated carboxylic acid class monomer, unsaturated carboxylic acid alkyl ester and unsaturated phosphate ester class monomer and deionized water mixing, match
The solution B that mass fraction is 40~55% is made；
3. be added into reaction kettle by the mass fraction that oxidant and the mixing of remaining deionized water are made into be 7.5~15% it is molten
Liquid, and 2~5min is stirred, obtain mixing primer solution；
4. solution A is first added drop-wise to by reactor temperature at 15~30 DEG C, using constant flow pump, step is 3. obtained to mix bottom material
In solution, the time for adding for controlling solution A is 2.5~3.0h, starts dropwise addition solution B after 5~10min of dropwise addition again and 3. makes to step
In the mixing primer solution obtained, the time for adding for controlling solution B is that 2.0~2.5h continues to stir after two kinds of solution are added dropwise
1.0~1.5h finally adjusts solution ph to 5.0~7.0 with the sodium hydroxide solution that mass fraction is 30%, and moisturizing is stirred
Uniformly obtain the poly carboxylic acid series water reducer for having both viscosity reduction and protecting function of collapsing that solid content is 40wt%.
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| CN115806402B (en) * | 2022-12-21 | 2023-08-22 | 四川同舟化工科技有限公司 | Special high-dispersion plastic-retaining polycarboxylate superplasticizer for phosphogypsum and preparation method thereof |
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Application publication date: 20181218 |