CN105601843A - Early-strength ethers polycarboxylic acid water reducing agent and preparation method thereof - Google Patents
Early-strength ethers polycarboxylic acid water reducing agent and preparation method thereof Download PDFInfo
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- CN105601843A CN105601843A CN201610186337.5A CN201610186337A CN105601843A CN 105601843 A CN105601843 A CN 105601843A CN 201610186337 A CN201610186337 A CN 201610186337A CN 105601843 A CN105601843 A CN 105601843A
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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
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Macromonomer-Based Addition Polymer (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to an early-strength ethers polycarboxylic acid water reducing agent and a preparation method thereof, belonging to the technical field of construction concrete additives. The preparation method of the early-strength ethers polycarboxylic acid water reducing agent comprises the steps: mixing and dissolving TPEG with a molecular weight of 6000 to 8000 and deionized water at the normal temperature, then adding a catalyst, then successively dropwise adding a solution A formed by mixing acrylic acid, sulphosalts unsaturated monomers and deionized water and a solution B formed by mixing an initiator, a chain transfer agent and deionized water to perform the water-based polymerization reaction, stirring after the dropwise addition, and finally adding an alkaline liquid to perform the neutralization to obtain the early-strength ethers polycarboxylic acid water reducing agent. A great amount of rigid benzene rings and sulfonate radicals are introduced into the molecular structure of the water reducing agent, so that the content of carboxylic groups having a delayed coagulation effect in the polycarboxylic acid molecules is greatly reduced, the early strength effect of the polycarboxylic acid water reducing agent molecules is greatly improved, a certain water reducing performance is achieved, and the application prospect is wide.
Description
Technical field
The present invention relates to a kind of ethers early-strength polycarboxylate water-reducer and preparation method thereof, belong to building concrete additive technology neckTerritory.
Background technology
Along with development and the progress of high performance water reducing agent of polyocarboxy acid synthetic technology, at commerical ready-mixed concrete, particularly prefabricated componentsActual production process in, more urgent to the demand of new function water reducer-early-strength polycarboxylate water-reducer, it can improveConcrete service behaviour, significantly improves concrete early strength, production efficiency, can reduce energy consumption simultaneously. Early strongThe polycarboxylate water-reducer of function can solve in winter construction process that early strength is low, concrete is subject to the problems such as freeze injury effectively, withTime can improve form cycling rate, reduce even remove steam curing expense from, accelerating construction progress, increases economic efficiency. CloselyNian Lai, large-scale high-quality requires engineering more and more, and concrete performance has also just been had to higher requirement, and for there being height to subtractThe poly-application by sour water reducer of early-strength of water, high early epistasis energy also can be more and more extensive. But for a long time, use MOLECULE DESIGN sideIt is more rare that formula is synthesized the research of early-strength polycarboxylate water-reducer, and this has limited polycarboxylate water-reducer greatly at common prefabricated structureApplication in part concrete and high-strength pipe pile concrete.
CN103304181A discloses a kind of early-strength poly-carboxylic high-performance diminishing being made up of following compositions in weight percentageThe poly carboxylic acid series water reducer of agent: 10-20%, the calcium chloride of 10-17%, the natrium nitrosum of 10-20%, the triethanolamine of 1-3%,Surplus is water. It is mainly by composite making simply, not from basic on the basis of common polycarboxylate water-reducerOn the molecular structure of polycarboxylate water-reducer, improving, there is the poor and adjustment of adaptability, the little problem in synergy space in its product.
CN103450408A discloses with beta-unsaturated esters, diethanol monoisopropanolamine, 2-acrylamido-methyl propane sulfonic acid and firstBase allyl polyethenoxy polyethenoxy ether is raw material, under the effect of catalyst, initator, chain-transferring agent etc., at certain barPart is through phthalein amination and polymerization process and the ethers early-strength polycarboxylate water-reducer preparing, and its preparation technology is loaded down with trivial details, reaction temperatureHeight, has relatively high expectations to production equipment, and processing safety is poor.
Therefore,, by the relation of research polycarboxylate water-reducer molecular structure and performance, synthesize and there is powerful gathering of more excellent morningCarboxylic acid water reducer, will have great importance.
Summary of the invention
The object of this invention is to provide a kind of ethers early-strength polycarboxylate water-reducer, solved the product adaptation existing in prior artProperty poor and adjustment, the little problem in synergy space, have the advantages that setting time is short, early strength is high; The present invention provides simultaneouslyIts preparation method.
The preparation method of ethers early-strength polycarboxylate water-reducer of the present invention is the methyl that is first 6000-8000 by molecular weightAllyl alcohol polyethenoxy ether and deionized water mixed dissolution at normal temperatures, then add wherein catalyst, then drip successively by thirdThe solution A that olefin(e) acid, Sulfonates unsaturated monomer, deionized water are mixed into and mixed by initator, chain-transferring agent, deionized waterSynthetic solution B is carried out polymerizable aqueous reaction, after dropwising, stirs, and finally adds alkali lye to neutralize, and obtains ethersEarly-strength polycarboxylate water-reducer.
Wherein, preferred technical scheme is as follows:
Taking the gross mass of methyl allyl alcohol polyoxyethylene ether and deionized water as 100%, methyl allyl alcohol polyoxyethylene ether accounts for45-65％。
Described catalyst is one or both in ammonium persulfate, hydrogen peroxide, and its consumption is methyl allyl alcohol polyoxyethylene ether matterThe 0.5-1wt% of amount.
In described solution A, acrylic acid consumption is the 4-7wt% of methyl allyl alcohol polyoxyethylene ether quality.
In described solution A, Sulfonates unsaturated monomer is the one or two in sodium p styrene sulfonate, methylpropene sodium sulfonateKind, its consumption is the 3-5.5wt% of methyl allyl alcohol polyoxyethylene ether quality.
In described solution B, initator is one or both in vitamin C, sodium hydrogensulfite, and its consumption is methallyl alcoholThe 2-4wt% of APEO quality.
In described solution B, chain-transferring agent is one or both in TGA, 3-mercaptopropionic acid, and its consumption is methyl allylThe 3-6wt ‰ of alcohol APEO quality.
Reaction temperature when described polymerisation is 5-30 DEG C, polymerization bottom liquid concentration 45-65%, and the reaction time is 1.5-3h.
The described alkali lye that adds is neutralized to pH value for 5-7.
The solid content of described ethers early-strength polycarboxylate water-reducer is 20-60wt%.
Beneficial effect of the present invention is as follows:
(1) the present invention, by introduce a large amount of rigidity phenyl ring and sulfonate radical in water reducer molecular structure, has significantly reduced polycarboxylic acids and has dividedIn son, there is the content of the hydroxy-acid group of slow setting effect, greatly promoted potent fruit morning of polycarboxylate water-reducer molecule, and had oneFixed water-reducing property, has a extensive future;
(2) adopt the long-chain methacrylic APEO that molecular weight is 6000-8000, potent fruit morning of its synthetic water reducerBetter;
(3) preparation method is simple, and reaction temperature is low, to production equipment require low, good operation safety.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
The preparation method of ethers early-strength polycarboxylate water-reducer is as follows:
Under normal temperature condition, in 1L glass flask, add 440g deionized water, open and stir, add 360g molecular weight to be6000 methacrylic APEO, treats abundant dissolving, and adding 1.8g concentration is the hydrogen peroxide of 27.5wt%, then successivelyDrip the solution A being mixed into by 14.4g acrylic acid, 19.8g sodium p styrene sulfonate, 40g deionized water and supported one's family by 0.72gThe solution B that element C, 1.08g TGA, 80g deionized water are mixed into, time for adding is 1.5h, after stirring 1h, adds concentrationFor the NaOH solution of 30wt% is neutralized to pH value for 5-7, then moisturizing to solid content is 40wt%, obtains ethers early-strength poly-Carboxylic acid water reducer.
Embodiment 2
The preparation method of ethers early-strength polycarboxylate water-reducer is as follows:
Under normal temperature condition, in 1L glass flask, add 193.8g deionized water, open and stir, add 360g molecular weight to be7000 methacrylic APEO, treats abundant dissolving, adds 3.6g ammonium persulfate, then drips successively by 25.2g thirdThe solution A that olefin(e) acid, 10.8g methylpropene sodium sulfonate, 40g deionized water are mixed into and by 1.44g sodium hydrogensulfite, 2.16gThe solution B that mercaptopropionic acid, 80g deionized water are mixed into, time for adding is 2h, after stirring 1h, adding concentration is 30wt%'sNaOH solution is neutralized to pH value for 5-7, and then moisturizing to solid content is 40wt%, obtains ethers early-strength polycarboxylate water-reducer.
Embodiment 3
The preparation method of ethers early-strength polycarboxylate water-reducer is as follows:
Under normal temperature condition, in 1L glass flask, add 300g deionized water, open and stir, add 360g molecular weight to be8000 methacrylic APEO, treats abundant dissolving, and adding 1g concentration is hydrogen peroxide and the 1.5g over cure of 27.5wt%Acid ammonium, then drip successively the solution A that is mixed into by 21.6g acrylic acid, 9g sodium p styrene sulfonate, 40g deionized water andThe solution B being mixed into by 1.08g vitamin C, 0.8g TGA, 1g mercaptopropionic acid, 80g deionized water, time for adding is2.5h, stir add after 0.5h concentration be the NaOH solution of 30wt% to be neutralized to pH value be 5-7, then moisturizing to solid content is40wt%, obtains ethers early-strength polycarboxylate water-reducer.
Embodiment 4
The preparation method of ethers early-strength polycarboxylate water-reducer is as follows:
Under normal temperature condition, in 1L glass flask, add 400g deionized water, open and stir, add 360g molecular weight to be6000 methacrylic APEO, treats abundant dissolving, adds 3g ammonium persulfate, then drips successively the propylene by 18gThe solution A that acid, 8g sodium p styrene sulfonate, 8.2g methylpropene sodium sulfonate, 40g deionized water are mixed into and being supported one's family by 0.6gThe solution B that element C, 1g TGA, 0.6g sodium hydrogensulfite, 0.5 mercaptopropionic acid, 80g deionized water are mixed into, when droppingBetween be 3h, stir that to add concentration after 0.5h be that the NaOH solution of 30wt% is neutralized to pH value for 5-7, then moisturizing extremely contains admittedlyAmount, for 40wt%, obtains ethers early-strength polycarboxylate water-reducer.
Adopt standard cement, the product that embodiment 1-4 is obtained and common polycarboxylate water-reducer contrast, according toGB8076-2008 " concrete admixture ", measures the each age strength of its slump and concrete. Wherein, concrete mix is:Cement 360kg/m3, sand 803kg/m3, stone 982kg/m3, the slump is controlled at 180 ± l0mm, and testing result is in table 1.
Table 1 properties of product detect index
As can be seen from Table 1, the early age strength of concrete that uses product of the present invention to prepare is higher than common polycarboxylate water-reducer,Early-strength water reducer of the present invention can significantly improve early age strength of concrete, is specially adapted to the life of prefabricated component and tubular pile concreteProduce.
Claims (10)
1. a preparation method for ethers early-strength polycarboxylate water-reducer, is characterized in that: be first 6000-8000 by molecular weightMethyl allyl alcohol polyoxyethylene ether and deionized water mixed dissolution at normal temperatures, then add wherein catalyst, then drip successivelyThe solution A being mixed into by acrylic acid, Sulfonates unsaturated monomer, deionized water and by initator, chain-transferring agent, deionizationThe solution B that water is mixed into is carried out polymerizable aqueous reaction, after dropwising, stirs, and finally adds alkali lye to neutralize, and obtainsEthers early-strength polycarboxylate water-reducer.
2. the preparation method of ethers early-strength polycarboxylate water-reducer according to claim 1, is characterized in that: with methyl alkeneThe gross mass of propyl alcohol APEO and deionized water is 100%, and methyl allyl alcohol polyoxyethylene ether accounts for 45-65%.
3. the preparation method of ethers early-strength polycarboxylate water-reducer according to claim 1, is characterized in that: catalyst isOne or both in ammonium persulfate, hydrogen peroxide, its consumption is the 0.5-1wt% of methyl allyl alcohol polyoxyethylene ether quality.
4. the preparation method of ethers early-strength polycarboxylate water-reducer according to claim 1, is characterized in that: solution AIn acrylic acid consumption be the 4-7wt% of methyl allyl alcohol polyoxyethylene ether quality.
5. the preparation method of ethers early-strength polycarboxylate water-reducer according to claim 1, is characterized in that: solution AMiddle Sulfonates unsaturated monomer is one or both in sodium p styrene sulfonate, methylpropene sodium sulfonate, and its consumption is methylThe 3-5.5wt% of allyl alcohol polyethenoxy ether quality.
6. the preparation method of ethers early-strength polycarboxylate water-reducer according to claim 1, is characterized in that: solution BMiddle initator is one or both in vitamin C, sodium hydrogensulfite, and its consumption is methyl allyl alcohol polyoxyethylene ether quality2-4wt％。
7. the preparation method of ethers early-strength polycarboxylate water-reducer according to claim 1, is characterized in that: solution BMiddle chain-transferring agent is one or both in TGA, 3-mercaptopropionic acid, and its consumption is methyl allyl alcohol polyoxyethylene ether quality3-6wt ‰.
8. the preparation method of ethers early-strength polycarboxylate water-reducer according to claim 1, is characterized in that: polymerisationTime reaction temperature be 5-30 DEG C, the reaction time is 1.5-3h; Finally add alkali lye to be neutralized to pH value for 5-7.
9. an ethers early-strength polycarboxylate water-reducer, is characterized in that: adopt the arbitrary described preparation method of claim 1-8Prepare.
10. ethers early-strength polycarboxylate water-reducer according to claim 9, is characterized in that: ethers early-strength polycarboxylic acidsThe solid content of water reducer is 20-60wt%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632892A (en) * | 2016-12-28 | 2017-05-10 | 江苏奥克化学有限公司 | Early-strength polycarboxylate water reducing agent and preparation method thereof |
| CN106866895A (en) * | 2017-03-27 | 2017-06-20 | 南宁新泰瑞科建材有限公司 | A kind of high-performance poly carboxylic acid series water reducer and preparation method thereof |
| CN107446090A (en) * | 2017-09-07 | 2017-12-08 | 江苏百瑞吉新材料有限公司 | A kind of synthetic method of Early-strength polycarboxylate superplasticizer |
| CN108101404A (en) * | 2017-12-28 | 2018-06-01 | 科之杰新材料集团有限公司 | A kind of preparation method of sustained-release polycarboxylic water reducer |
| CN110128601A (en) * | 2019-05-22 | 2019-08-16 | 上饶市天佳新型材料有限公司 | A kind of Early-strength polycarboxylate superplasticizer and preparation method thereof |
| CN111410451A (en) * | 2020-03-30 | 2020-07-14 | 深圳港创建材股份有限公司 | Raw material formula of graphene polycarboxylate superplasticizer and preparation and use methods of water reducer |
| CN111592622A (en) * | 2019-02-21 | 2020-08-28 | 天水师范学院 | Method and device for preparing early-strength polycarboxylate superplasticizer |
| CN114702628A (en) * | 2022-03-25 | 2022-07-05 | 湖南中岩建材科技有限公司 | Water reducing agent modifier and preparation method and application thereof |
| CN115849760A (en) * | 2022-12-28 | 2023-03-28 | 科之杰新材料集团有限公司 | Early-strength polycarboxylate superplasticizer and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106632892B (en) * | 2016-12-28 | 2019-11-26 | 江苏奥克化学有限公司 | A kind of Early-strength polycarboxylate superplasticizer and preparation method thereof |
| CN106632892A (en) * | 2016-12-28 | 2017-05-10 | 江苏奥克化学有限公司 | Early-strength polycarboxylate water reducing agent and preparation method thereof |
| CN106866895A (en) * | 2017-03-27 | 2017-06-20 | 南宁新泰瑞科建材有限公司 | A kind of high-performance poly carboxylic acid series water reducer and preparation method thereof |
| CN107446090A (en) * | 2017-09-07 | 2017-12-08 | 江苏百瑞吉新材料有限公司 | A kind of synthetic method of Early-strength polycarboxylate superplasticizer |
| CN108101404A (en) * | 2017-12-28 | 2018-06-01 | 科之杰新材料集团有限公司 | A kind of preparation method of sustained-release polycarboxylic water reducer |
| CN111592622B (en) * | 2019-02-21 | 2022-06-10 | 天水师范学院 | Method and device for preparing early-strength polycarboxylate superplasticizer |
| CN111592622A (en) * | 2019-02-21 | 2020-08-28 | 天水师范学院 | Method and device for preparing early-strength polycarboxylate superplasticizer |
| CN110128601A (en) * | 2019-05-22 | 2019-08-16 | 上饶市天佳新型材料有限公司 | A kind of Early-strength polycarboxylate superplasticizer and preparation method thereof |
| CN111410451A (en) * | 2020-03-30 | 2020-07-14 | 深圳港创建材股份有限公司 | Raw material formula of graphene polycarboxylate superplasticizer and preparation and use methods of water reducer |
| CN114702628A (en) * | 2022-03-25 | 2022-07-05 | 湖南中岩建材科技有限公司 | Water reducing agent modifier and preparation method and application thereof |
| CN114702628B (en) * | 2022-03-25 | 2023-12-26 | 湖南中岩建材科技有限公司 | Water reducer modifier and preparation method and application thereof |
| CN115849760A (en) * | 2022-12-28 | 2023-03-28 | 科之杰新材料集团有限公司 | Early-strength polycarboxylate superplasticizer and preparation method thereof |
| CN115849760B (en) * | 2022-12-28 | 2023-12-01 | 科之杰新材料集团有限公司 | Early-strength polycarboxylate superplasticizer and preparation method thereof |
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