CN108585594A - A kind of high and easy retentivity polycarboxylate water-reducer of 1800 molecular weight polyethers and preparation method - Google Patents
A kind of high and easy retentivity polycarboxylate water-reducer of 1800 molecular weight polyethers and preparation method Download PDFInfo
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- CN108585594A CN108585594A CN201810518905.6A CN201810518905A CN108585594A CN 108585594 A CN108585594 A CN 108585594A CN 201810518905 A CN201810518905 A CN 201810518905A CN 108585594 A CN108585594 A CN 108585594A
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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
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/32—Polyethers, e.g. alkylphenol polyglycolether
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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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
-
- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
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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
- C08F228/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a bond to sulfur or by a heterocyclic ring containing sulfur
- C08F228/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a bond to sulfur or by a heterocyclic ring containing sulfur by a bond to sulfur
-
- 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
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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
-
- 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
-
- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
Abstract
The present invention provides a kind of high and easy retentivity polycarboxylate water-reducer of 1800 molecular weight polyethers and preparation methods.The parts by weight of component of each component is in the polycarboxylate water-reducer：1800 molecular weight polyether polymeric monomers：325 340 parts, hydrogen peroxide：1 2.1 parts, unsaturated sulfonic acid salt：25 parts, acrylic acid：35 45 parts, amide groups minor comonomer：37 parts, reducing agent：0.35 0.55 parts, flexible chain monomer：4 10 parts, chain-transferring agent：0.3 0.7 parts, neutralizer：6 10 parts, surplus is water, and 1000 parts of gross mass, final product quality score is 40% after preparation, and sour ether ratio is within the scope of 2.9 3.7.The method carries out as follows：1, it feeds for the first time；2, add hydrogen peroxide；3, solution A, solution B is added；4, prepared by finished product.The present invention, as raw material, obtains partially short side chain lengths using the polyether monomer of 1800 molecular weight, compensates for the problem of short-side chain brings steric hindrance effect that can be weakened, backbone length design is slightly longer, builds the molecular configuration of long main chain, short-side chain.
Description
Technical field：
The present invention relates to construction materials and polycarboxylate water-reducer technical field, are related specifically to a kind of 1800 molecular weight polyethers use
High and easy retentivity polycarboxylate water-reducer and preparation method.
Background technology：
With the development of modern building technology, high performance concrete also obtains significant progress, pushes directly on polycarboxylic acids and subtracts
The progress of aqua technology also has higher requirement the functionality of water-reducing agent.In application process, such as water consumption it is more,
In the case that the ratio of mud is larger, some polycarboxylate water-reducers are more sensitive to water, and the micro adjustment of itself volume can bring about work
Make the big ups and downs of performance, generate isolation excreting water phenomenon, especially situation is more aobvious when using the fine sand material of large specific surface area
It writes.
The water retention property of water-reducing agent is beneficial to concrete workability and function of slump protection, and common collapse protection type water-reducing agent and guarantor are collapsed
Agent, which mostly uses, introduces the groups such as ester group, and gradually hydrolysis release carboxyl is adsorbed onto cement particle surface, obtains diminishing dispersion effect.Just
For the molecular configuration and the mechanism of action of water-reducing agent, initial water reducing ability is mutually restricted with function of slump protection, and the initial ability that subtracts is strong,
Function of slump protection can be weaker；Function of slump protection is good, and initial water-reducing rate is not also high.
Patent CN103254420A discloses a kind of low molecular polyether water-reducing agent and its preparation method and application, the hair
It is bright to be reacted with raw materials such as alkyl oxyalkylene, p-hydroxybenzoate, maleic anhydrides, obtain low molecular weight diminishing
Agent.The low molecular weight water-reducing agent of the invention can be directly used as polycarboxylate water-reducer, also can be multiple with other type polycarboxylate water-reducers
Match, it can also be with other vinyl monomer copolymerizations at high molecular weight polycarboxylate water-reducer.
Patent CN107056994A discloses a kind of preparation method of Mobyneb polycarboxylate water-reducer, and this method is with isoamyl
Alkenyl polyoxyethylene ether, fumaric acid, oxidant, 7 mass parts of acrylic acid, hydroxy-ethyl acrylate, acrylamido methylpropane sulfonic acid, third
Acrylamide and water are made into solution A；Reducing agent, chain-transferring agent are made into B solution；Solution A is added dropwise successively in gained homogeneous solution
And B solution；Aging 1 hour at 40 DEG C supplements remaining water, stirs 0.5 hour, obtain Mobyneb polycarboxylate water-reducer；It should
Invent the Mobyneb polycarboxylate water-reducer prepared it is adaptable it is wide, protect function admirable of collapsing, concrete strength can be improved
Feature.
Patent CN106146759A discloses a kind of high-performance polycarboxylic acids water reducing agent and preparation method thereof, by following quality hundred
The each component of ratio is divided to be prepared：Polycarboxylic acid water reducer macromer 15%-20%；Initiator 1-2%；Chain-transferring agent 3-5%；Methyl-prop
Olefin(e) acid 10-13%；- 2 methyl propane sulfonic acid sodium 5-8% of 2- acrylamides；Sodium hydroxide 2-3%；Water 50-70%.The polycarboxylate water-reducer
Environmentally protective, water-reducing rate is high, good dispersion, and in concrete in use, playing higher plasticizing effect under low-dosage, mobility is protected
Holding property is good, notable to concrete enhancing effect.
Patent CN106632890A discloses a kind of collapse protective poly-carboxylic acid water reducing agent preparation method, especially by unsaturated first
Base cyclobutenyl polyethylene glycol ethers monomer, unsaturated carboxylic acid class monomer, sealing end phosphate and unsaturated acids hydroxy ester are in initiator
After being copolymerized under the action of molecular weight regulator, adds in alkaline solution and obtained after pH value to 6-7.The invention
Collapse protective poly-carboxylic acid water reducing agent have the advantages that low-dosage, high diminishing, high-thin arch dam and cement adaptability are good, and production cycle
Short, low energy consumption, and production cost is low, has very high application value.
Invention content：
The purpose of the present invention is to provide a kind of high and easy retentivity polycarboxylate water-reducer of 1800 molecular weight polyethers and preparation sides
Method.
The design philosophy of the present invention is the polyether macromonomer using 1800 molecular weight, introduces hydrophilic sulfonic group, amide groups
Monomer obtains good hydrophilic water holding capacity；The monomer with flexible chain is introduced, main chain flexibility is enhanced, improves package ability.
By targeted design, acquisition backbone length is longer, flexible preferable, the good height of water retention property and easy retentivity polycarboxylic acids diminishing
Agent.
The present invention, as raw material, obtains partially short side chain lengths, while to make up using the polyether monomer of 1800 molecular weight
The problem of short-side chain brings steric hindrance effect that can be weakened, backbone length design comparison is long, builds point of long main chain, short-side chain
Sub- configuration.Hydrophilic radical is introduced, control water is retained；And flexible chain enhancing main chain flexibility is introduced, and package ability is improved, it is final to obtain
It is good to package ability, the form compact and stable height of cement particle surface hydration shell and easy retentivity polycarboxylate water-reducer.
To achieve the above object, the technical scheme is that:
A kind of 1800 molecular weight polyethers height and easy retentivity polycarboxylate water-reducer, it is characterised in that：The polycarboxylic acids diminishing
The parts by weight component of each component is in agent：
1800 molecular weight polyether polymeric monomers：325-340 parts, hydrogen peroxide：1-2.1 parts,
Unsaturated sulfonic acid salt：2-5 parts, acrylic acid：35-45 parts,
Amide groups minor comonomer：3-7 parts, reducing agent：0.35-0.55 parts,
Flexible chain monomer：4-10 parts, chain-transferring agent：0.3-0.7 parts,
Neutralizer：6-10 parts, surplus is water, and 1000 parts of gross mass, final product quality score is 40% after preparation, and sour ether ratio is in 2.9-
Within the scope of 3.7.
In the polycarboxylate water-reducer 1800 molecular weight polyether polymeric monomers by molecular weight 1800 allyl polyethenoxy
Ether (APEG), methyl allyl alcohol polyoxyethylene ether (HPEG), isoamyl alcohol polyoxyethylene ether (TPEG), poly glycol monomethyl ether
(MPEG) one or more of compositions.
Flexible chain monomer is by bis- (4- amino-benzene oxygens) ethane of 1,2-, bis- (the 4- ammonia of 1,3- in the polycarboxylate water-reducer
Phenoxyl) propane, bis- (4- amino-benzene oxygens) butane of Isosorbide-5-Nitrae-, cyclobutane tetracarboxylic dianhydride, 4,4 one diaminodiphenyl ethers,
One or more of compositions of two amido detergent alkylates, two amido octadecyl benzene.
Reducing agent is sodium dithionite, sodium formaldehyde sulphoxylate, ascorbic acid, Asia in the polycarboxylate water-reducer
One or more of compositions of niter cake, sodium pyrosulfite, sodium hypophosphite, Dextrose Monohydrate, maltodextrin.
Unsaturated sulfonic acid salt is sodium vinyl sulfonate, acrylic sodium sulfonate, metering system in the polycarboxylate water-reducer
Sodium sulfonate, sodium styrene sulfonate, 2- methallylsulfonic acids ammonium, 2- cyanoethanes sodium sulfonate, Sodium Allyl Sulfonate one kind or
Several compositions.
Amide groups minor comonomer is 2- acrylamide-2-methyl propane sulfonics, acrylamide, first in the polycarboxylate water-reducer
Base acrylamide, N- methyl -2- acrylamides, N- methyl-1s-ethenesulfonamide, N hydroxymethyl acrylamide, N- isopropyl first
Base acrylamide, N- tertiary butyls methacrylamide, N- cyclohexyl methyls allylamine, 3- acrylamides -3 Methylbutanoic acid, N- are (different
Butoxymethyl) acrylamide, N, N- dimethylformamides, N- methylacryloyl glycine one or more of compositions.
The polycarboxylate water-reducer Chain transfer agent be thioacetic acid, mercaptopropionic acid, mercaptoethanol, mercaprol one
Kind or several compositions.
In the polycarboxylate water-reducer neutralizer be sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate,
One or more of compositions of sodium methoxide, sodium ethoxide, ethanol amine, diethanol amine, triethanolamine, triisopropanolamine.
It is 27.5% industrial grade hydrogen peroxide that hydrogen peroxide, which is mass percent, in the polycarboxylate water-reducer.
A kind of high preparation method with easy retentivity polycarboxylate water-reducer of 1800 molecular weight polyether, it is characterised in that：Institute
Method is stated to carry out as follows：
1, it feeds for the first time：1800 molecular weight polyether polymeric monomer of 325-340 parts and 180-220 parts of water are added in reaction kettle,
Agitating and heating waits for its dissolving；
2, add hydrogen peroxide：Reactor temperature is measured, control reactor temperature is at 30-40 DEG C, after temperature is stablized, disposably
1-2.1 parts of hydrogen peroxide are added；
3, solution A, solution B is added：It waits for after five minutes, starts that solution B, solution A is added dropwise successively, after solution B is added, in 10 minutes
Start that solution A is added dropwise, solution A time for adding is 2-4 hours, and solution B time for adding is 2.5-4.5 hours；Solution B is by 0.35-
0.55 part of reducing agent, 0.3-0.7 parts of chain-transferring agents and 80-100 parts of water are uniformly mixed, solution A by 35-45 parts of acrylic acid,
2-5 portions of unsaturated sulfonic acid salt, 3-7 parts of amide groups minor comonomers, 4-10 parts of flexible chain monomers and 50-70 parts of water are uniformly mixed；
4, prepared by finished product：It after completion of dropwise addition, keeps temperature constant, cures 1-3 hours, when reaction solution temperature is less than 30 DEG C,
6-10 parts of neutralizers are slowly added to, moisturizing is protected to the 1800 molecular weight polyethers height that 1000 parts are 40% to get mass fraction with easy
Holding property polycarboxylate water-reducer.
Compared with prior art, the positive effect of the present invention is:
1, the present invention obtains partially short side chain lengths, while short to make up using the polyether monomer of 1800 molecular weight as raw material
The problem of side chain brings steric hindrance effect that can be weakened, backbone length design is slightly longer, builds the molecule structure of long main chain, short-side chain
Type；
2, for the present invention in the case where side chain is shorter, side chain density is higher just to meet Molecular Geometries, and set by the present invention
The sour ether ratio of meter is in 2.9-3.7 or so, and side chain density is higher, can promote to form fine and close hydration shell, which can stablize
In the presence of improving the maintenance properties of concrete；
3, present invention introduces the groups such as sulfonic group, amide groups, not only strengthen anchoring ability, but also enhance hydrophilic ability, increase
Add the stability of hydration shell, interferes water film to cement granules internal penetration, delay hydration process to a certain extent, make coagulation
Soil has preferable state-retention capabilities；
4, longer in main chain, diminishing agent molecule faces the problem of flexibility deficiency, i.e. main chain rigidity is larger, can not wrap
Cement granules are wrapped, it is poor macroscopically to show as concrete wrapping property.For this situation, present invention introduces main chains to have flexibility
Polymerized monomer, so that diminishing agent molecule is obtained preferable flexibility, obtain good package performance.
Specific embodiment
Clear, complete description further is carried out to technical scheme of the present invention with reference to embodiment.
Embodiment 1：
1, it feeds for the first time：325 parts of HPEG1800 polymeric monomers and 180 parts of water are added in reaction kettle, agitating and heating waits for that its is molten
Solution；
2, add hydrogen peroxide：Reactor temperature is measured, control reactor temperature is at 30 DEG C, disposable to add after temperature is stablized
Enter 1 part of hydrogen peroxide；
3, solution A, solution B is added：It waits for after five minutes, starts that solution B, solution A is added dropwise successively, after solution B is added, in 10 minutes
Start that solution A is added dropwise, solution A time for adding is 2 hours, and solution B time for adding is 2.5 hours；Solution B is sub- by 0.35 part of company two
Sodium sulphate, 0.7 part of thioacetic acid and 100 parts of water are uniformly mixed, and solution A is by 45 parts of acrylic acid, 4 parts of sodium vinyl sulfonates, 6
Part 2- acrylamide-2-methyl propane sulfonics, 10 parts of cyclobutane tetracarboxylic dianhydrides and 50 parts of water are uniformly mixed；
4, prepared by finished product：It after completion of dropwise addition, keeps temperature constant, cures 1 hour, when reaction solution temperature is less than 30 DEG C, delay
Slow 7 parts of mass ratioes of addition are 1:2 sodium methoxide and the composition of ethanol amine, moisturizing are 40% to get mass fraction to 1000 parts
1800 molecular weight polyethers height and easy retentivity polycarboxylate water-reducer
Embodiment 2
1, it feeds for the first time：333 parts of APEG1800 polymeric monomers and 190 parts of water are added in reaction kettle, agitating and heating waits for that its is molten
Solution；
2, add hydrogen peroxide：Reactor temperature is measured, control reactor temperature is at 32 DEG C, disposable to add after temperature is stablized
Enter 1.1 parts of hydrogen peroxide；
3, solution A, solution B is added：It waits for after five minutes, starts that solution B, solution A is added dropwise successively, after solution B is added, in 10 minutes
Start that solution A is added dropwise, solution A time for adding is 2.2 hours, and solution B time for adding is 2.7 hours；Solution B is by 0.38 part of quality
Than being 1:2 sodium formaldehyde sulphoxylate and the composition of ascorbic acid, 0.55 part of mercaptopropionic acid and 85 parts of water uniformly mixing and
At solution A is by 43 parts of acrylic acid, 5 parts of acrylic sodium sulfonates, 4 parts of N- methyl -2- acrylamides, 4 parts of mass ratioes 1:The 1,2- of 1
Bis- (4- amino-benzene oxygens) ethane and the composition of cyclobutane tetracarboxylic dianhydride, 55 parts of water are uniformly mixed；
4, prepared by finished product：It after completion of dropwise addition, keeps temperature constant, cures 1.3 hours, when reaction solution temperature is less than 30 DEG C,
It is slowly added to sodium bicarbonate, moisturizing is 40% 1800 molecular weight polyethers height and easy retentivity to get mass fraction to 1000 parts
Polycarboxylate water-reducer.
Embodiment 3
1, it feeds for the first time：330 parts of TPEG1800 polymeric monomers and 185 parts of water are added in reaction kettle, agitating and heating waits for that its is molten
Solution；
2, add hydrogen peroxide：Reactor temperature is measured, control reactor temperature is at 35 DEG C, disposable to add after temperature is stablized
Enter 1.27 parts of hydrogen peroxide；
3, solution A, solution B is added：It waits for after five minutes, starts that solution B, solution A is added dropwise successively, after solution B is added, in 10 minutes
Start that solution A is added dropwise, solution A time for adding is 2.5 hours, and solution B time for adding is 3 hours；Solution B is closed by 0.4 part of formaldehyde
Sodium bisulphite, 0.62 part of mass ratio are 1:2 thioacetic acid and the composition of mercaptopropionic acid, 95 parts of water are uniformly mixed,
Solution A is by 41 parts of acrylic acid, 4.5 parts of methylpropene sodium sulfonates, 2- methallylsulfonic acids ammonium, Sodium Allyl Sulfonate, 7 parts of N- hydroxyls
Methacrylamide, 9 parts of mass ratioes 1:The combination of 11,3- bis- (4- amino-benzene oxygens) propane and cyclobutane tetracarboxylic dianhydride
Object, 56 parts of water are uniformly mixed；
4, prepared by finished product：It after completion of dropwise addition, keeps temperature constant, cures 1.5 hours, when reaction solution temperature is less than 30 DEG C,
7.5 parts of sodium hydroxides are slowly added to, moisturizing is high and easy for 40% 1800 molecular weight polyethers to get mass fraction to 1000 parts
Retentivity polycarboxylate water-reducer.
Embodiment 4
1, it feeds for the first time：337 parts of MPEG1800 polymeric monomers and 200 parts of water are added in reaction kettle, agitating and heating waits for that its is molten
Solution；
2, add hydrogen peroxide：Reactor temperature is measured, control reactor temperature is at 36 DEG C, disposable to add after temperature is stablized
Enter 1.63 parts of hydrogen peroxide；
3, solution A, solution B is added：It waits for after five minutes, starts that solution B, solution A is added dropwise successively, after solution B is added, in 10 minutes
Start that solution A is added dropwise, solution A time for adding is 3.3 hours, and solution B time for adding is 3.8 hours；Solution B is anti-bad by 0.45 part
Hematic acid, 0.35 part of mercaptoethanol and 88 parts of water are uniformly mixed, and solution A is by 44 parts of acrylic acid, 3.5 parts of mass ratioes 1:1 2-
Methallylsulfonic acid ammonium and the composition of Sodium Allyl Sulfonate, 3.2 parts of N- tertiary butyls methacrylamides, 5 parts of mass ratioes 1:1
Bis- (4- amino-benzene oxygens) butane of Isosorbide-5-Nitrae-and composition, the 65 parts of water of cyclobutane tetracarboxylic dianhydride are uniformly mixed；
4, prepared by finished product：It after completion of dropwise addition, keeps temperature constant, cures 2 hours, when reaction solution temperature is less than 30 DEG C, delay
Slowly 6.5 parts of sodium ethoxides of addition, 1800 molecular weight polyethers height and easily holding of the moisturizing to 1000 parts to get mass fraction for 40%
Property polycarboxylate water-reducer.
Embodiment 5
1, it feeds for the first time：332 parts of HPEG1800 polymeric monomers and 210 parts of water are added in reaction kettle, agitating and heating waits for that its is molten
Solution；
2, add hydrogen peroxide：Reactor temperature is measured, control reactor temperature is at 38 DEG C, disposable to add after temperature is stablized
Enter 1.82 parts of hydrogen peroxide；
3, solution A, solution B is added：It waits for after five minutes, starts that solution B, solution A is added dropwise successively, after solution B is added, in 10 minutes
Start that solution A is added dropwise, solution A time for adding is 3.5 hours, and solution B time for adding is 4 hours；After completion of dropwise addition, temperature is kept
It is constant, cure 2.5 hours, when reaction solution temperature be less than 30 DEG C when, be slowly added to 10 parts of diethanol amine, moisturizing to 1000 parts,
It is 40% 1800 molecular weight polyethers height and easy retentivity polycarboxylate water-reducer up to mass fraction.
4, prepared by finished product：It after completion of dropwise addition, keeps temperature constant, cures 2.5 hours, wait for that reaction solution temperature is less than 30 DEG C
When, be slowly added to 10 parts of diethanol amine, moisturizing to 1000 parts to get mass fraction be 40% 1800 molecular weight polyethers it is high with
Easy retentivity polycarboxylate water-reducer.
Embodiment 6
1, it feeds for the first time：340 parts of TPEG1800 polymeric monomers and 220 parts of water are added in reaction kettle, agitating and heating waits for that its is molten
Solution；
2, add hydrogen peroxide：Reactor temperature is measured, control reactor temperature is at 40 DEG C, disposable to add after temperature is stablized
Enter 2.1 parts of hydrogen peroxide；
3, solution A, solution B is added：It waits for after five minutes, starts that solution B, solution A is added dropwise successively, after solution B is added, in 10 minutes
Start that solution A is added dropwise, solution A time for adding is 4 hours, and solution B time for adding is 4.5 hours；Solution B is by 0.5 part phosphorous
Sour sodium, 0.3 part of thioacetic acid and 95 parts of water are uniformly mixed, and solution A is by 40 parts of acrylic acid, 2 parts of 2- methallylsulfonic acids
Ammonium, 3 parts of N- (isobutoxymethyl) acrylamides, 8 parts of mass ratioes 2:1 cyclobutane tetracarboxylic dianhydride and two amido dodecyls
The composition of benzene, 70 parts of water are uniformly mixed；
4, prepared by finished product：It after completion of dropwise addition, keeps temperature constant, cures 3 hours, when reaction solution temperature is less than 30 DEG C, delay
Slowly 6 parts of triisopropanolamines of addition, 1800 molecular weight polyethers height and easily guarantor of the moisturizing to 1000 parts to get mass fraction for 40%
Holding property polycarboxylate water-reducer.
Example detection result：
Respectively the high and easy retentivity polycarboxylate water-reducer of 1800 molecular weight polyethers of test above-described embodiment 1,2,3,4,5,6 and
Common cement paste initial fluidity and 1h mobility of the polycarboxylate water-reducer under comparable sodium, and in concrete initially
The slump/divergence and through when the slump/divergence.Experiment cement used is new 42.5 ordinary portland cement of China, with reference to GB/8076-
2008《Concrete admixture》Testing standard.
Different Water-reducing Admixtures To Cements net slurry flow effects（New 42.5 ordinary portland cement of China）
| Water-reducing agent type | Initial fluidity mm | 1h mobility mm |
| Ordinary water-reducing agent | 230 | 210 |
| Embodiment 1 | 230 | 210 |
| Embodiment 2 | 220 | 200 |
| Embodiment 3 | 235 | 225 |
| Embodiment 4 | 225 | 210 |
| Embodiment 5 | 220 | 200 |
| Embodiment 6 | 240 | 220 |
Different water-reducing agents are to the influence containing ash, the big concrete flowability of mud amount（New 42.5 ordinary portland cement of China）
| Water-reducing agent type | Initial slump/divergence mm | Through when the slump/divergence mm | Bleeding rate % |
| Ordinary water-reducing agent | 210/500 | 130/380 | 3.1 |
| Embodiment 1 | 200/500 | 175/480 | 1.8 |
| Embodiment 2 | 220/510 | 185/470 | 1.6 |
| Embodiment 3 | 205/490 | 175/460 | 1.7 |
| Embodiment 4 | 215/500 | 180/480 | 1.7 |
| Embodiment 5 | 220/510 | 170/470 | 1.8 |
| Embodiment 6 | 200/510 | 160/465 | 1.7 |
According to above-mentioned cement paste initial fluidity, 1h mobility and concrete initial fluidity and through when mobility compare,
The high and easy retentivity polycarboxylate water-reducer embodiment 1,2,3,4,5,6 of 1800 molecular weight polyethers is being tested with ordinary water-reducing agent
When, initial fluidity, 1h mobility are essentially identical compared with ordinary water-reducing agent.In the experimental data of the big concrete flowability of clay content
In, ordinary water-reducing agent is substantially suitable with initial slump/divergence of embodiment 1,2,3,4,5,6, but ordinary water-reducing agent is added
Concrete occur serious isolation excreting water phenomenon after a certain time, and the concrete of embodiment 1,2,3,4,5,6 remains unchanged
There is preferable slump divergence, and bleeding rate is very low.In conclusion 1800 molecular weight polyether is high and easy retentivity is poly-
Carboxylic acid water reducer can better adapt to variation of the concrete containing ash, mud amount, show good workability.
All features disclosed in this specification or disclosed all formulas, volume and step, in addition to mutually exclusive spy
Other than sign and/or formula, volume, it can combine in any way.This specification（Including claim, abstract）Disclosed in
Any feature can be replaced by other alternative features that are equivalent or have similar purpose unless specifically stated.It is i.e. unless special
It does not describe, each feature is an example in a series of equivalent or similar characteristics.
Described above is only the non-limiting embodiment of invention, a large amount of embodiment can also be derived, for this field
Those of ordinary skill for, not departing from the invention design and under the premise of do not make creative work, can also do
Go out the embodiment of several modifications and improvements, these are all within the scope of protection of the present invention.
Claims (10)
1. a kind of 1800 molecular weight polyethers height and easy retentivity polycarboxylate water-reducer, it is characterised in that：The polycarboxylic acids subtracts
The parts by weight component of each component is in aqua：
1800 molecular weight polyether polymeric monomers：325-340 parts, hydrogen peroxide：1-2.1 parts,
Unsaturated sulfonic acid salt：2-5 parts, acrylic acid：35-45 parts,
Amide groups minor comonomer：3-7 parts, reducing agent：0.35-0.55 parts,
Flexible chain monomer：4-10 parts, chain-transferring agent：0.3-0.7 parts,
Neutralizer：6-10 parts, surplus is water, and 1000 parts of gross mass, final product quality score is 40% after preparation, and sour ether ratio is in 2.9-
Within the scope of 3.7.
2. 1800 molecular weight polyether height according to claim 1 and easy retentivity polycarboxylate water-reducer, it is characterised in that：
In the polycarboxylate water-reducer 1800 molecular weight polyether polymeric monomers by molecular weight 1800 allyl polyethenoxy ether (APEG)
, methyl allyl alcohol polyoxyethylene ether (HPEG), isoamyl alcohol polyoxyethylene ether (TPEG), poly glycol monomethyl ether (MPEG) one
Kind or several compositions.
3. 1800 molecular weight polyether height according to claim 1 and easy retentivity polycarboxylate water-reducer, it is characterised in that：
Flexible chain monomer is by bis- (4- amino-benzene oxygens) ethane of 1,2-, bis- (the 4- aminobenzene oxygen of 1,3- in the polycarboxylate water-reducer
Base) propane, bis- (4- amino-benzene oxygens) butane of Isosorbide-5-Nitrae-, cyclobutane tetracarboxylic dianhydride, 4,4 one diaminodiphenyl ethers, two amidos
One or more of compositions of detergent alkylate, two amido octadecyl benzene.
4. 1800 molecular weight polyether height according to claim 1 and easy retentivity polycarboxylate water-reducer, it is characterised in that：
Reducing agent is sodium dithionite, sodium formaldehyde sulphoxylate, ascorbic acid, bisulfite in the polycarboxylate water-reducer
One or more of compositions of sodium, sodium pyrosulfite, sodium hypophosphite, Dextrose Monohydrate, maltodextrin.
5. 1800 molecular weight polyether height according to claim 1 and easy retentivity polycarboxylate water-reducer, it is characterised in that：
Unsaturated sulfonic acid salt is sodium vinyl sulfonate, acrylic sodium sulfonate, methylpropene sodium sulfonate, benzene in the polycarboxylate water-reducer
One or more of compositions of vinyl sulfonic acid sodium, 2- methallylsulfonic acids ammonium, 2- cyanoethanes sodium sulfonate, Sodium Allyl Sulfonate.
6. 1800 molecular weight polyether height according to claim 1 and easy retentivity polycarboxylate water-reducer, it is characterised in that：
Amide groups minor comonomer is 2- acrylamide-2-methyl propane sulfonics, acrylamide, methacryl in the polycarboxylate water-reducer
Amine, N- methyl -2- acrylamides, N- methyl-1s-ethenesulfonamide, N hydroxymethyl acrylamide, N- isopropyl methyl acryloyls
Amine, N- tertiary butyls methacrylamide, N- cyclohexyl methyls allylamine, 3- acrylamides -3 Methylbutanoic acid, N- (isobutoxy first
Base) acrylamide, N, N- dimethylformamides, N- methylacryloyl glycine one or more of compositions.
7. 1800 molecular weight polyether height according to claim 1 and easy retentivity polycarboxylate water-reducer, it is characterised in that：
The polycarboxylate water-reducer Chain transfer agent is thioacetic acid, the one or more of mercaptopropionic acid, mercaptoethanol, mercaprol
Composition.
8. 1800 molecular weight polyether height according to claim 1 and easy retentivity polycarboxylate water-reducer, it is characterised in that：
In the polycarboxylate water-reducer neutralizer be sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium methoxide,
One or more of compositions of sodium ethoxide, ethanol amine, diethanol amine, triethanolamine, triisopropanolamine.
9. 1800 molecular weight polyether height according to claim 1 and easy retentivity polycarboxylate water-reducer, it is characterised in that：
It is 27.5% industrial grade hydrogen peroxide that hydrogen peroxide, which is mass percent, in the polycarboxylate water-reducer.
10. a kind of high preparation side with easy retentivity polycarboxylate water-reducer of 1800 molecular weight polyether as described in claim 1
Method, it is characterised in that：The method carries out as follows：
（1）, for the first time feed：1800 molecular weight polyether polymeric monomer of 325-340 parts and 180-220 parts of water are added to reaction kettle
In, agitating and heating waits for its dissolving；
（2）Plus hydrogen peroxide：Reactor temperature is measured, control reactor temperature is at 30-40 DEG C, after temperature is stablized, once
Property be added 1-2.1 parts of hydrogen peroxide；
（3）, be added solution A, solution B：It waits for after five minutes, starts that solution B, solution A is added dropwise successively, after solution B is added, 10 minutes
Inside start that solution A is added dropwise, solution A time for adding is 2-4 hours, and solution B time for adding is 2.5-4.5 hours；Solution B by
0.35-0.55 parts of reducing agents, 0.3-0.7 parts of chain-transferring agents and 80-100 parts of water are uniformly mixed, and solution A is by 35-45 parts third
Olefin(e) acid, 2-5 portions of unsaturated sulfonic acid salt, 3-7 parts of amide groups minor comonomers, 4-10 parts of flexible chain monomers and 50-70 parts of water uniformly mix
It forms；
（4）, finished product prepare：It after completion of dropwise addition, keeps temperature constant, cures 1-3 hours, wait for that reaction solution temperature is less than 30 DEG C
When, be slowly added to 6-10 parts of neutralizers, moisturizing to 1000 parts to get mass fraction be 40% 1800 molecular weight polyethers it is high with
Easy retentivity polycarboxylate water-reducer.
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