CN109626859A - A kind of anti-mud slow release slump retaining polycarboxylate water reducer and preparation method thereof - Google Patents
A kind of anti-mud slow release slump retaining polycarboxylate water reducer and preparation method thereof Download PDFInfo
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- CN109626859A CN109626859A CN201811579346.6A CN201811579346A CN109626859A CN 109626859 A CN109626859 A CN 109626859A CN 201811579346 A CN201811579346 A CN 201811579346A CN 109626859 A CN109626859 A CN 109626859A
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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
- 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
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
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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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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
- C08F220/285—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing a polyether chain in the alcohol moiety
- C08F220/286—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing a polyether chain in the alcohol moiety and containing polyethylene oxide in the alcohol moiety, e.g. methoxy polyethylene glycol (meth)acrylate
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- Materials Engineering (AREA)
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The present invention relates to technical field of concrete additives, more specifically, it is related to a kind of anti-mud slow release slump retaining polycarboxylate water reducer and preparation method thereof, using polyether macromonomer, unsaturated carboxylic acid, esters of unsaturated carboxylic acids, dibasic acid anhydride, crosslinking agent, amides monomer, unsaturated phosphate ester, phosphate, oxidant, reducing agent, chain-transferring agent, neutralizer and water as raw material, anti-mud slow release slump retaining polycarboxylate water reducer is synthesized at normal temperature.The present invention introduces ester group, amide groups and phosphate in polycarboxylate water-reducer molecule structure, and keep polycarboxylate water-reducer realization lightly crosslinked by long-chain esters crosslinking agent, make the water-reducing agent that there is good anti-mud and protects effect of collapsing, it is low with volume, water-reducing rate is high, to containing argillaceous sand stone it is adaptable, the advantages that function of slump protection is good, and polymerized at normal temperature is only needed, simple process, lower production costs are suitble to industrialized production.
Description
Technical field
The present invention relates to technical field of concrete additives, more specifically, are related to a kind of anti-mud sustained release poly- carboxylic of collapse protection type
Sour water-reducing agent and preparation method thereof.
Background technique
In recent years, polycarboxylate water-reducer has been widely applied, high water reducing rate, higher cost performance, excellent guarantor
It collapses the good workability of performance, mixture, is had been widely recognized in engineer application in recent years.However a large amount of engineering
It was verified that polycarboxylate water-reducer is more sensitive to clay content in sandstone, clay content is varied slightly, the slump of concrete mix
Degree loss will significantly improve, working performance degradation, and later concrete mechanical properties decrease.
As a large amount of exploitations of natural sand stone resource and the taboo in part river are adopted limit and dug, good sand and stone resources seriously lack
It is weary, therefore many concrete works have to result in viscous in sandstone using the higher sandstone of some clay contents or Machine-made Sand
Native content substantially exceeds prescribed limits.Currently, coping with the high clay content problem of sandstone in engineering, there are mainly two types of methods: first is that sand
Stone is cleaned, and sandstone clay content is reduced；Second is that the dosage of polycarboxylate water-reducer is increased, to supplement by mud absorption in sandstone
Water-reducing agent.Both methods can not fundamentally solve polycarboxylate water-reducer to sandstone clay content sensitive issue.Therefore, how
Polycarboxylate water-reducer is reduced to the susceptibility of sandstone clay content, it has also become an additive industry hot issue urgently to be resolved,
Be also polycarboxylate water-reducer can further genralrlization application a deciding factor.
Studies have shown that clay has suction-operated to polycarboxylate water-reducer in sandstone, and adsorption capacity is better than cement pair
The absorption of polycarboxylate water-reducer molecule, this competitive Adsorption reduce the polycarboxylate water-reducer molecule for dispersing cement, therefore
By reducing clay to the absorption of polycarboxylate water-reducer and improving absorption of the cement to polycarboxylate water-reducer, polycarboxylic acids can be improved
The anti-mud performance of water-reducing agent.The invention proposes a kind of preparing without heat source for anti-mud sustained release collapse protective poly-carboxylic acid high-performance water reducing agent
Method reduces absorption of the clay to polycarboxylate water-reducer, while introducing small carboxylic acid molecules' ester by introducing amide groups and phosphate
With the esters crosslinking agent that can be hydrolyzed under alkaline environment, make polycarboxylate water-reducer that there is good anti-mud effect and long-acting slow-release function
Can, meet concrete mix requirement slump-retaining for a long time.
Summary of the invention
In the presence of overcoming the shortcomings of the prior art, the present invention provide a kind of pair of sandstone aggregate it is adaptable, protect collapse
Performance is good, simple process, lower-cost anti-mud slow release slump retaining polycarboxylate water reducer and preparation method thereof, solves existing sandstone
Clay content is high, polycarboxylate water-reducer bad adaptability, the big problem of concrete slump loss.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is as follows:
A kind of anti-mud slow release slump retaining polycarboxylate water reducer by copolyreaction and is neutralized anti-by bottom material, A liquid, B liquid and neutralizer
It should be made；
The bottom material is composed of the following raw materials by weight: 340-380 parts of polyether macromonomer, 3-8 parts of dibasic acid anhydride, and phosphate 3-6
Part, 2-5 parts of oxidant, 200 parts of water；
The A liquid is composed of the following raw materials 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 is composed of the following raw materials by weight: 15-30 parts of unsaturated carboxylic acid, 20-40 parts of esters of unsaturated carboxylic acids, and crosslinking agent
3-8 parts, 5-12 parts of amides monomer, 5-15 parts of unsaturated phosphate ester, 80 parts of water；
The neutralizer is composed of the following raw materials by weight: 3-6 parts of neutralizer, 200-300 parts of water.
Further, the molecular weight of the anti-mud slow release slump retaining polycarboxylate water reducer is 30000-80000.
Further, the molecular structural formula of the anti-mud slow release slump retaining polycarboxylate water reducer are as follows:
。
Further, the polyether macromonomer is isoamyl alcohol polyoxyethylene ether or methyl allyl alcohol polyoxyethylene ether, is divided
Son amount is (2400-3000) dalton；The dibasic acid anhydride is maleic anhydride or itaconic anhydride；The phosphate is ortho phosphorous acid
Sodium；The oxidant is hydrogen peroxide (27.5%), ammonium persulfate, in potassium peroxydisulfate and one or more mixtures.
Further, the reducing agent is one of ascorbic acid, sodium formaldehyde sulfoxylate and sodium sulfite or a variety of mixtures；Institute
Stating chain-transferring agent is mercaptopropionic acid or thioacetic acid.
Further, the insatiable hunger carboxylic acid is one of acrylic acid, methacrylic acid, fumaric acid or a variety of mixtures；
The esters of unsaturated carboxylic acids is methyl acrylate, hydroxy-ethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, methyl
One of hydroxypropyl acrylate or a variety of mixtures；The crosslinking agent is polyethyleneglycol diacrylate, polyethylene glycol diformazan
One of base acrylate, polyethylene glycol maleic acid diester, molecular weight are (400-600) dalton；The amides list
Body is acrylamide or 2- acrylamide-2-methyl propane sulfonic (AMPS)；The unsaturated phosphate ester is 2- hydroxyethyl methyl third
Olefin(e) acid ester phosphate (HEMAP) or 1- hydroxyl ethyl ester methacrylate phosphate (UPE).
Further, the neutralizer is one of sodium hydroxide, potassium hydroxide and ammonium hydroxide or a variety of mixtures.
Further, the water is the industry water of deionized water or conductivity less than 20 μ S/cm.
A kind of preparation method of anti-mud slow release slump retaining polycarboxylate water reducer, comprising the following steps:
S1. it prepares bottom material: polyether macromonomer, dibasic acid anhydride, phosphate and deionized water being added in reaction kettle, stirred under room temperature
It mixes, 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, is added dropwise
Liquid A；
S3. dropping liquid B is prepared: by load weighted unsaturated carboxylic acid, esters of unsaturated carboxylic acids, crosslinking agent, amides monomer and insatiable hunger
It is added in deionized water with phosphate, stirs evenly, obtain dropping liquid B；
S4. load weighted oxidant is added in bottom material, stirs (5-10) minute, A is then at the uniform velocity added dropwise into reaction kettle respectively
Liquid, B liquid, control A liquid time for adding (3.5-4.0) h, B liquid time for adding are (3.0-3.5) h, drip subsequent continuation of insurance temperature
(1.0-2.0)h；
S5. after the reaction was completed, neutralizer is added and deionized water adjusts pH value of solution as 5-7, it is slow to obtain the anti-mud that solid content is 40%
Release collapse protective poly-carboxylic acid water reducing agent.
Compared with prior art, the advantageous effect of present invention is that:
The present invention provides a kind of anti-mud slow release slump retaining polycarboxylate water reducers and preparation method thereof, in polycarboxylate water-reducer molecule
In structure, small carboxylic acid molecules' ester and amides monomer are not only introduced, also introduces phosphate, phosphate, carboxylate and amide
Base can hydrolyze under alkaline environment, but the hydrolysis time of phosphate is longer, and the phosphate anion after hydrolysis has
Two negative electrical charges have stronger adsorption capacity and dispersion performance compared to carboxylic acid ion, enhance the dispersibility of water-reducing agent,
Phosphate anion can react with hydrolysis product of cement simultaneously, thin in the phosphate that cement particle surface forms fine and close indissoluble
Layer, delays hydrated cementitious, so that water-reducing agent is protected the ability of collapsing and is substantially improved.In polycarboxylate water-reducer molecule structure, pass through phosphate
Chain transfer, introduce hypophosphorous acid root in polycarboxylate water-reducer molecule main chain terminal, while uniformly introducing acyl in main chain
Amido and phosphate, amide groups is positively charged under alkaline environment, can be adsorbed in clay particle surface formed one layer it is stable
Protective film is adsorbed, thus the phosphate radical and hypophosphorous acid root energy that prevent the further absorption of other water-reducing agents and moisture, and introduce
The adsorption capacity of Water-reducing Admixtures To Cements particle is significantly increased, competitive Adsorption ability of the cement with respect to clay is improved, the two is assigned jointly
The good anti-mud effect of water-reducing agent is given.Anti- mud slow release slump retaining polycarboxylate water reducer prepared by the present invention passes through free radical polymerization
Reaction only needs a step to be made, and without heating, simple process, energy conservation and environmental protection, raw materials used to be easy to get extensively, cost is relatively low, fits
Industrialized production is closed, properties of product are stablized, and anti-mud protects the excellent effect that collapses, and have a good application prospect.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
A kind of anti-mud slow release slump retaining polycarboxylate water reducer by copolyreaction and is neutralized anti-by bottom material, A liquid, B liquid and neutralizer
It should be made；
The bottom material is composed of the following raw materials by weight: 340.0 parts of isoamyl alcohol polyoxyethylene ether, 3.0 parts of maleic anhydride, and secondary Asia
3.0 parts of sodium phosphate, 2.4 parts of hydrogen peroxide, 200.0 parts of water；
The A liquid is composed of the following raw materials by weight: 0.5 part of ascorbic acid, 1.8 parts of mercaptopropionic acid, 120.0 parts of water；
The B liquid is composed of the following raw materials by weight: 15.0 parts of acrylic acid, 25.0 parts of methyl acrylate, and two propylene of polyethylene glycol
3.0 parts of acid esters, 5.0 parts of acrylamide, 6.0 parts of 2-hydroxyethyl methacrylate phosphate, 80.0 parts of water；
The neutralizer is composed of the following raw materials by weight: 3.0 parts of sodium hydroxide, 200.0 parts of water.
The preparation method of anti-mud slow release slump retaining polycarboxylate water reducer, the specific steps are as follows:
(1) prepare bottom material: weigh the isoamyl alcohol polyoxyethylene ethers of above-mentioned parts by weight, maleic anhydride, sodium hypophosphite and go from
Sub- water is added in reaction kettle, stirs under room temperature, is completely dissolved raw material, obtains reaction bottom material；
(2) it prepares dropping liquid A: the ascorbic acid of above-mentioned parts by weight and mercaptopropionic acid being added in deionized water, stirs evenly, obtains
To dropping liquid A；
(3) dropping liquid B is prepared: by the acrylic acid of above-mentioned parts by weight, methyl acrylate, polyethyleneglycol diacrylate, acryloyl
Amine and 2-hydroxyethyl methacrylate phosphate (HEMAP) are added in deionized water, stir evenly, obtain dropping liquid B；
(4) hydrogen peroxide of above-mentioned parts by weight is added in bottom material, stirs 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 3.5h, B liquid time for adding are 3.0h, drip subsequent continuation of insurance temperature 1.0h；
(5) after the reaction was completed, it is 5-7 that the sodium hydroxide and deionized water that above-mentioned parts by weight are added, which adjust pH value of solution, is obtained containing solid
The anti-mud slow release slump retaining polycarboxylate water reducer that amount is 40%.
In the present embodiment, isoamyl alcohol polyoxyethylene ether molecular weight is 2400 dalton, polyethyleneglycol diacrylate
Molecular weight is 400 dalton, and hydrogen peroxide mass concentration is 27.5%, 2-hydroxyethyl methacrylate phosphoric acid ester molecular structure are as follows:
。
Embodiment 2
A kind of anti-mud slow release slump retaining polycarboxylate water reducer by copolyreaction and is neutralized anti-by bottom material, A liquid, B liquid and neutralizer
It should be made；
The bottom material is composed of the following raw materials by weight: 360.0 parts of isoamyl alcohol polyoxyethylene ether, 5.0 parts of itaconic anhydride, and secondary Asia
4.0 parts of sodium phosphate, 4.0 parts of ammonium persulfate, 200 parts of water；
The A liquid is composed of the following raw materials by weight: 0.7 part of ascorbic acid, 1.5 parts of thioacetic acid, 120 parts of water；
The B liquid is composed of the following raw materials by weight: 18.0 parts of acrylic acid, 26.0 parts of hydroxy-ethyl acrylate, and polyethylene glycol diformazan
4.0 parts of base acrylate, 7.0 parts of 2- acrylamide-2-methyl propane sulfonic, 8.0 parts of 1- hydroxyl ethyl ester methacrylate phosphate,
80 parts of water；
The neutralizer is composed of the following raw materials by weight: 3.0 parts of potassium hydroxide, 240.0 parts of water.
The preparation method of anti-mud slow release slump retaining polycarboxylate water reducer, the specific steps are as follows:
(1) isoamyl alcohol polyoxyethylene ether, itaconic anhydride, sodium hypophosphite and the deionization of above-mentioned parts by weight bottom material processed: are weighed
Water is added in reaction kettle, stirs under room temperature, is completely dissolved raw material, obtains reaction bottom material；
(2) it prepares dropping liquid A: the ascorbic acid of above-mentioned parts by weight and thioacetic acid being added in deionized water, stirs evenly, obtains
To dropping liquid A；
(3) prepare dropping liquid B: by the acrylic acid of above-mentioned parts by weight, hydroxy-ethyl acrylate, polyethylene glycol dimethacrylate,
2- acrylamide-2-methyl propane sulfonic and 1- hydroxyl ethyl ester methacrylate phosphate are added in deionized water, stir evenly, obtain
To dropping liquid B；
(4) ammonium persulfate of above-mentioned parts by weight is added in bottom material, stirs 5-10 minutes, is then at the uniform velocity dripped into reaction kettle respectively
Add A liquid, B liquid, control A liquid time for adding 4.0h, B liquid time for adding is 3.5h, drips subsequent continuation of insurance temperature 1.0h；
(5) after the reaction was completed, it is 5-7 that the potassium hydroxide and deionized water that above-mentioned parts by weight are added, which adjust pH value of solution, is obtained containing solid
The anti-mud slow release slump retaining polycarboxylate water reducer that amount is 40%.
In the present embodiment, isoamyl alcohol polyoxyethylene ether molecular weight is 3000 dalton, polyethylene glycol dimethyl allene
Acid ester molecules amount is 400 dalton, 1- hydroxyl ethyl ester methacrylate phosphate molecular structural formula are as follows:
Embodiment 3
A kind of anti-mud slow release slump retaining polycarboxylate water reducer by copolyreaction and is neutralized anti-by bottom material, A liquid, B liquid and neutralizer
It should be made；
The bottom material is composed of the following raw materials by weight: 350.0 parts of methyl allyl alcohol polyoxyethylene ether, 6.0 parts of maleic anhydride, secondary
4.0 parts of sodium phosphite, 3.0 parts of hydrogen peroxide, 200.0 parts of water；
The A liquid is composed of the following raw materials by weight: 1.0 parts of sodium formaldehyde sulfoxylate, 2.0 parts of mercaptopropionic acid, 120.0 parts of water；
The B liquid is composed of the following raw materials by weight: 24.0 parts of methacrylic acid, 22.0 parts of hydroxypropyl acrylate, and polyethylene glycol
6.0 parts of diacrylate, 8.0 parts of acrylamide, 9.0 parts of 2-hydroxyethyl methacrylate phosphate, 80.0 parts of water；
The neutralizer is composed of the following raw materials by weight: 4.0 parts of sodium hydroxide, 240.0 parts of water.
The preparation method of anti-mud slow release slump retaining polycarboxylate water reducer, the specific steps are as follows:
(1) it prepares bottom material: weighing methyl allyl polyoxyethylene ether, maleic anhydride, sodium hypophosphite, the dioxygen of above-mentioned parts by weight
Water and deionized water are added in reaction kettle, stir under room temperature, are completely dissolved raw material, obtain reaction bottom material；
(2) it prepares dropping liquid A: the sodium formaldehyde sulfoxylate of above-mentioned parts by weight and mercaptopropionic acid being added in deionized water, stirs evenly, obtains
Dropping liquid A；
(3) prepare dropping liquid B: by the methacrylic acid of above-mentioned parts by weight, hydroxypropyl acrylate, polyethyleneglycol diacrylate,
Acrylamide and 2-hydroxyethyl methacrylate phosphate are added in deionized water, stir evenly, obtain dropping liquid B；
(4) hydrogen peroxide of above-mentioned parts by weight is added in bottom material, stirs (5-10) minute, is then at the uniform velocity dripped into reaction kettle respectively
Add A liquid, B liquid, control A liquid time for adding 3.5h, B liquid time for adding is 3.0h, drips subsequent continuation of insurance temperature 1.5h；
(5) after the reaction was completed, it is 5-7 that the sodium hydroxide and deionized water that above-mentioned parts by weight are added, which adjust pH value of solution, is obtained containing solid
The anti-mud slow release slump retaining polycarboxylate water reducer that amount is 40%.
In the present embodiment, methyl allyl polyoxyethylene ether molecular weight is 2400 dalton, glycol diacrylate
Molecular weight is 600 dalton, and hydrogen peroxide mass concentration is 27.5%, 2-hydroxyethyl methacrylate phosphoric acid ester molecular structure are as follows:
。
Embodiment 4
A kind of anti-mud slow release slump retaining polycarboxylate water reducer by copolyreaction and is neutralized anti-by bottom material, A liquid, B liquid and neutralizer
It should be made；
The bottom material is composed of the following raw materials by weight: 370.0 parts of isoamyl alcohol polyoxyethylene ether, 4.0 parts of maleic anhydride, and secondary Asia
5.0 parts of sodium phosphate, 5.0 parts of ammonium persulfate, 200.0 parts of water；
The A liquid is composed of the following raw materials by weight: 0.6 part of sodium sulfite, 1.6 parts of thioacetic acid, 120.0 parts of water；
The B liquid is composed of the following raw materials by weight: 20.0 parts of methacrylic acid, 20.0 parts of hydroxyethyl methacrylate, and poly- second
5.0 parts of glycol maleic acid diester, 6.0 parts of sulphur of 2- acrylamide -2- methyl-prop, 1- hydroxyl ethyl ester methacrylate phosphate 7.0
Part, 80.0 parts of water；
The neutralizer is composed of the following raw materials by weight: 4.0 parts of sodium hydroxide, 250.0 parts of water.
The preparation method of anti-mud slow release slump retaining polycarboxylate water reducer, the specific steps are as follows:
(1) prepare bottom material: weigh the isoamyl alcohol polyoxyethylene ethers of above-mentioned parts by weight, maleic anhydride, sodium hypophosphite and go from
Sub- water is added in reaction kettle, stirs under room temperature, is completely dissolved raw material, obtains reaction bottom material；
(2) it prepares dropping liquid A: the sodium sulfite of above-mentioned parts by weight and thioacetic acid being added in deionized water, stirs evenly, obtains
To dropping liquid A；
(3) dropping liquid B is prepared: the methacrylic acid of above-mentioned parts by weight, hydroxyethyl methacrylate, polyethylene glycol maleic acid is double
Ester, 2- acrylamide-2-methyl propane sulfonic and 1- hydroxyl ethyl ester methacrylate phosphate are added in deionized water, and stirring is equal
It is even, obtain dropping liquid B；
(4) ammonium persulfates of above-mentioned parts by weight is added in bottom material, stirs (5-10) minute, then respectively into reaction kettle at the uniform velocity
A liquid, B liquid is added dropwise, control A liquid time for adding 4.0h, B liquid time for adding is 3.0h, drips subsequent continuation of insurance temperature 1.0h；
(5) after the reaction was completed, it is 5-7 that the sodium hydroxide and deionized water that above-mentioned parts by weight are added, which adjust pH value of solution, is obtained containing solid
The anti-mud slow release slump retaining polycarboxylate water reducer that amount is 40%.
In the present embodiment, isoamyl alcohol polyoxyethylene ether molecular weight is 3000 dalton, polyethylene glycol maleic acid diester
Molecular weight is 400 dalton, 1- hydroxyl ethyl ester methacrylate phosphate molecular structural formula are as follows:
Embodiment 5
A kind of anti-mud slow release slump retaining polycarboxylate water reducer by copolyreaction and is neutralized anti-by bottom material, A liquid, B liquid and neutralizer
It should be made；
The bottom material is composed of the following raw materials by weight: 355.0 parts of methyl allyl polyoxyethylene ether, 6.0 parts of itaconic anhydride, secondary
6.0 parts of sodium phosphite, 3.0 parts of hydrogen peroxide, 200.0 parts of water；
The A liquid is composed of the following raw materials by weight: 0.8 part of ascorbic acid, 2.4 parts of mercaptopropionic acid, 120.0 parts of water；
The B liquid is composed of the following raw materials by weight: 28.0 parts of acrylic acid, 30.0 parts of hydroxy propyl methacrylate, and polyethylene glycol
6.0 parts of diacrylate, 10.0 parts of acrylamide, 12.0 parts of 1- hydroxyl ethyl ester methacrylate phosphate, 80.0 parts of water；
The neutralizer is composed of the following raw materials by weight: 5.0 parts of ammonium hydroxide, 280.0 parts of water.
The preparation method of anti-mud slow release slump retaining polycarboxylate water reducer, the specific steps are as follows:
(1) it prepares bottom material: weighing the methyl allyl polyoxyethylene ethers of above-mentioned parts by weight, itaconic anhydride, sodium hypophosphite and go
Ionized water is added in reaction kettle, stirs under room temperature, is completely dissolved raw material, obtains reaction bottom material；
(2) it prepares dropping liquid A: the ascorbic acid of above-mentioned parts by weight and mercaptopropionic acid being added in deionized water, stirs evenly, obtains
To dropping liquid A；
(3) prepare dropping liquid B: by the acrylic acid of above-mentioned parts by weight, hydroxy propyl methacrylate, polyethyleneglycol diacrylate,
Acrylamide and 1- hydroxyl ethyl ester methacrylate phosphate (UPE) are added in deionized water, stir evenly, obtain dropping liquid B；
(4) hydrogen peroxide of above-mentioned parts by weight is added in bottom material, stirs 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 3.5h, B liquid time for adding are 3.0h, drip subsequent continuation of insurance temperature 1.5h；
(5) after the reaction was completed, it is 5-7 that the ammonium hydroxide and deionized water that above-mentioned parts by weight are added, which adjust pH value of solution, and obtaining solid content is
40% anti-mud slow release slump retaining polycarboxylate water reducer.
In the present embodiment, methyl allyl polyoxyethylene ether molecular weight is 2400 dalton, polyethylene glycol diacrylate
Ester molecule amount is 400 dalton, and hydrogen peroxide mass concentration is 27.5%, 1- hydroxyl ethyl ester methacrylate phosphate molecular structure
Formula are as follows:
Embodiment 6
A kind of anti-mud slow release slump retaining polycarboxylate water reducer by copolyreaction and is neutralized anti-by bottom material, A liquid, B liquid and neutralizer
It should be made；
The bottom material is composed of the following raw materials by weight: 380.0 parts of methyl allyl polyoxyethylene ether, 8.0 parts of itaconic anhydride, secondary
6.0 parts of sodium phosphite, 2.5 parts of potassium peroxydisulfate, 200.0 parts of water；
The A liquid is composed of the following raw materials by weight: 1.2 parts of ascorbic acid, 3 parts of mercaptopropionic acid, 120.0 parts of water；
The B liquid is composed of the following raw materials by weight: 30.0 parts of fumaric acid, 40.0 parts of hydroxy propyl methacrylate, and polyethylene glycol
8.0 parts of diacrylate, 12.0 parts of acrylamide, 15.0 parts of 1- hydroxyl ethyl ester methacrylate phosphate, 80.0 parts of water；
The neutralizer is composed of the following raw materials by weight: 6.0 parts of potassium hydroxide, 300.0 parts of water.
The preparation method of anti-mud slow release slump retaining polycarboxylate water reducer, the specific steps are as follows:
(1) it prepares bottom material: weighing the methyl allyl polyoxyethylene ethers of above-mentioned parts by weight, itaconic anhydride, sodium hypophosphite and go
Ionized water is added in reaction kettle, stirs under room temperature, is completely dissolved raw material, obtains reaction bottom material；
(2) it prepares dropping liquid A: the ascorbic acid of above-mentioned parts by weight and mercaptopropionic acid being added in deionized water, stirs evenly, obtains
To dropping liquid A；
(3) prepare dropping liquid B: by the fumaric acid of above-mentioned parts by weight, hydroxy propyl methacrylate, polyethyleneglycol diacrylate,
Acrylamide and 1- hydroxyl ethyl ester methacrylate phosphate (UPE) are added in deionized water, stir evenly, obtain dropping liquid B；
(4) potassium peroxydisulfate of above-mentioned parts by weight is added in bottom material, stirs 5-10 minutes, is then at the uniform velocity dripped into reaction kettle respectively
Add A liquid, B liquid, control A liquid time for adding 3.5h, B liquid time for adding is 3.0h, drips subsequent continuation of insurance temperature 2h；
(5) after the reaction was completed, it is 5-7 that the potassium hydroxide and deionized water that above-mentioned parts by weight are added, which adjust pH value of solution, is obtained containing solid
The anti-mud slow release slump retaining polycarboxylate water reducer that amount is 40%.
In the present embodiment, methyl allyl polyoxyethylene ether molecular weight is 2400 dalton, polyethylene glycol diacrylate
Ester molecule amount is 400 dalton, 1- hydroxyl ethyl ester methacrylate phosphate molecular structural formula are as follows:
。
It is 30000-80000 in the molecular weight of anti-mud slow release slump retaining polycarboxylate water reducer prepared in the above embodiments,
Molecular structural formula are as follows:
6 kinds of anti-mud slow release slump retaining polycarboxylate water reducer samples that embodiment 1-6 is synthesized carry out net slurry and concrete examination respectively
It tests, and compares test with current several commercially available water-reducing agent sample P CE-1, PCE-2, PCE-3.Wherein PCE-1 is conventional
Plain edition polycarboxylate water-reducer, PCE-2 are common collapse protective poly-carboxylic acid water reducing agent, and PCE-3 is anti-mud collapse protective poly-carboxylic acid diminishing
Agent.
1) paste flowing degree is tested
Net slurry tests reference standard GB/T 8077-2012 " Methods for testing uniformity of concrete admixture ", and cement consumption is
300g, water consumption 78g, cement are 42.5 cement of Yumen PO, while being mud in sandstone in simulation concrete to water-reducing agent
Absorption mixes 1.0% sodium bentonite in cement.Test data is shown in Table 1:
1 cement paste Experimental Comparison of table
As it can be seen from table 16 embodiments of the invention, flowing degree of net paste of cement has in the later period significantly to be increased, and
It is able to maintain higher paste flowing degree within some time, the slowly releasing effect of water-reducing agent is obvious, compares the poly- carboxylic of common collapse protection type
Sour water-reducing agent, polycarboxylate water-reducer of the invention, which has more preferably to be sustained, protects ability of collapsing；Simultaneously as can be seen that poly- carboxylic of the invention
Sour water-reducing agent has better anti-mud effect, is especially embodied in the holding capacity to mobility, and paste flowing degree loses speed
Much smaller than commercially available anti-mud collapse protective poly-carboxylic acid water reducing agent.
Pass through optimization polyether macromonomer and function monomer and the intermolecular crosslinking degree of minor comonomer ratio, water-reducing agent and diminishing
Agent molecule amount can make water-reducing agent comprehensive performance reach best.
2) concrete slump is tested
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, and folk prescription is matched
Composition and division in a proportion are as follows: cement 270kg, flyash 70kg, sand 830kg, stone 1060kg, water 160kg, it is 0.2% that water-reducing agent, which rolls over solid volume,.
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, clay content
It is 5%；Stone is (5-25) mm continuous grading rubble.Test data is shown in Table 2.
The comparison of 2 concrete test of table
As can be seen from Table 2,6 embodiments of the invention subtract with common polycarboxylate water-reducer (PCE-1), common collapse protective poly-carboxylic acid
Aqua (PCE-2) and anti-mud collapse protective poly-carboxylic acid water reducing agent (PCE-3) carry out concrete compbined test, compare concrete 's air-containing
It was found that product of the present invention and comparative sample air content difference are unobvious, illustrate that product of the present invention will not cause concrete 's air-containing
Adverse effect；Concrete slump discovery is compared, product of the invention, which is directed to, has higher tolerance, concrete containing silt particle
Slump free of losses in two hours, and the slump of 3 comparative samples has a degree of loss, illustrates that product of the invention has
Significant anti-mud protects effect of collapsing；Compression strength discovery is compared, the concrete crushing strength using product configuration of the invention is higher than
The concrete crushing strength that comparative sample is prepared, illustrates that anti-mud slow release slump retaining polycarboxylate water reducer of the invention can reduce in sandstone
Influence of the clay content to concrete crushing strength.Therefore, product of the present invention not only shows more the concrete prepared containing silt particle
Good anti-mud effect and ability of collapsing is protected, and there are also certain reinforcing effects to concrete strength, it will not be to concrete 's air-containing
Cause adverse effect, excellent combination property.
The preparation of anti-mud slow release slump retaining polycarboxylate water reducer of the present invention should be executed in strict accordance with above-mentioned preparation process,
The more stable raw material of quality should be chosen as far as possible simultaneously, guarantees the stabilization of product quality, reduced present in practical implementation
Problem.
The solid volume of the folding of anti-mud slow release slump retaining polycarboxylate water reducer of the present invention is generally cementitious material gross mass
0.05%-0.25% can not only be used for the exclusive use of collapse protection type water-reducing agent according to the needs that workability of concrete is kept, can also be with
Other water-reducing agents (such as polycarboxylate water-reducer, ligno-sulfate based plasticizer) and small powder (such as retarder, air entraining agent, defoaming agent
Deng) compounding after use, good performance Overlay can be played.
Only presently preferred embodiments of the present invention is explained in detail above, but the present invention is not limited to above-described embodiment,
Within the knowledge of a person skilled in the art, it can also make without departing from the purpose of the present invention each
Kind variation, various change should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of anti-mud slow release slump retaining polycarboxylate water reducer, it is characterised in that: passed through altogether by bottom material, A liquid, B liquid and neutralizer
Poly- reaction and neutralization reaction are made；
The bottom material is composed of the following raw materials by weight: 340-380 parts of polyether macromonomer, 3-8 parts of dibasic acid anhydride, and phosphate 3-6
Part, 2-5 parts of oxidant, 200 parts of water；
The A liquid is composed of the following raw materials 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 is composed of the following raw materials by weight: 15-30 parts of unsaturated carboxylic acid, 20-40 parts of esters of unsaturated carboxylic acids, and crosslinking agent
3-8 parts, 5-12 parts of amides monomer, 5-15 parts of unsaturated phosphate ester；
The neutralizer is composed of the following raw materials by weight: 3-6 parts of neutralizer, 200-300 parts of water.
2. a kind of anti-mud slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that: the anti-mud is slow
The molecular weight for releasing collapse protective poly-carboxylic acid water reducing agent is 30000-80000.
3. a kind of anti-mud slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that: the anti-mud is slow
Release the molecular structural formula of collapse protective poly-carboxylic acid water reducing agent are as follows:
。
4. a kind of anti-mud slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that: the polyethers is big
Monomer is isoamyl alcohol polyoxyethylene ether or methyl allyl alcohol polyoxyethylene ether, and molecular weight is 2400-3000 dalton；Described two
First acid anhydrides is maleic anhydride or itaconic anhydride；The phosphate is sodium hypophosphite；The oxidant is that mass concentration is 27.5%
Hydrogen peroxide, ammonium persulfate, in potassium peroxydisulfate and one or more mixtures.
5. a kind of anti-mud slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that: the reducing agent
For one of ascorbic acid, sodium formaldehyde sulfoxylate and sodium sulfite or a variety of mixtures；The chain-transferring agent is mercaptopropionic acid or sulfydryl
Acetic acid.
6. a kind of anti-mud slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that: the insatiable hunger carboxylic
Acid is one of acrylic acid, methacrylic acid, fumaric acid or a variety of mixtures；The esters of unsaturated carboxylic acids is acrylic acid first
One of ester, hydroxy-ethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxy propyl methacrylate are a variety of
Mixture；The crosslinking agent is polyethyleneglycol diacrylate, polyethylene glycol dimethacrylate, polyethylene glycol maleic acid pair
One of ester, molecular weight are 400-600 dalton；The amides monomer is acrylamide, 2- acrylamide -2- methyl
Propane sulfonic acid；The unsaturated phosphate ester is 2-hydroxyethyl methacrylate phosphate or 1- hydroxyl ethyl ester methacrylate phosphoric acid
Ester.
7. a kind of anti-mud slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that: the neutralizer
For one of sodium hydroxide, potassium hydroxide and ammonium hydroxide or a variety of mixtures.
8. a kind of anti-mud slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that: the water is to go
The industry water of ionized water or conductivity less than 20 μ S/cm.
9. a kind of preparation method of anti-mud slow release slump retaining polycarboxylate water reducer, comprising the following steps:
S1. it prepares bottom material: polyether macromonomer, dibasic acid anhydride, phosphate and deionized water being added in reaction kettle, stirred under room temperature
It mixes, 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, is added dropwise
Liquid A；
S3. dropping liquid B is prepared: by load weighted unsaturated carboxylic acid, esters of unsaturated carboxylic acids, crosslinking agent, amides monomer and insatiable hunger
It is added in deionized water with phosphate, stirs evenly, obtain dropping liquid B；
S4. load weighted oxidant is added in bottom material, stirs (5-10) min, A is then at the uniform velocity added dropwise into reaction kettle respectively
Liquid, B liquid, control A liquid time for adding (3.5-4.0) h, B liquid time for adding are (3.0-3.5) h, drip subsequent continuation of insurance temperature
(1.0-2.0)h；
S5. after the reaction was completed, neutralizer is added and deionized water adjusts pH value of solution as 5-7, it is slow to obtain the anti-mud that solid content is 40%
Release collapse protective poly-carboxylic acid water reducing agent.
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