CN105461866A - Viscosity-reducing type polycarboxylic-acid water-reducing agent and preparation method thereof - Google Patents
Viscosity-reducing type polycarboxylic-acid water-reducing agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a water-reducing agent, specifically to a viscosity-reducing type polycarboxylic-acid water-reducing agent and a preparation method thereof. The agent is prepared through the following steps: subjecting 7% to 16% of an unsaturated acid or unsaturated-acid derivative monomer a, 80% to 92% of a prenyl alcohol polyoxyethylene ether monomer b with a relative molecular mass M of 600 to 5000, and 6% to 13% of a gylcol ester monomer c to copolymerization reaction in an aqueous solution at 10 DEG C to 60 DEG C under the actions of an oxidation-reduction system and a chain transfer agent, and adjusting a PH value to 6.8 with a PH-value regulator so as to obtain a copolymerization reactant, wherein the total weight of the monomer a, the monomer b and the monomer c is 1. The viscosity-reducing type polycarboxylic-acid water-reducing agent provided by the invention can effectively reduce slurry viscosity of concrete with low water-binder ratio and high strength, and has long-time effects on maintaining slump and fluidity of concrete without the need of compounding use with a highly-slump-retaining type polycarboxylic-acid water-reducing agent.
Description
[technical field]
The present invention relates to a kind of water reducer, particularly relate to a kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof.
[background technology]
Along with the development in city, building site day is becoming tight, and for improving the rate of utilization in soil, will more and more adopt high level or high-rise building in the urban construction in future.
In order to ensure high level or high-rise building amount, increasing its internal space simultaneously, all adopting when building high-strength concrete to construct.And this type of builds often complex structure, cloth muscle is intensive, therefore requires high to fresh concrete, not only needs good workability, and need good flowing property and self-compacting ability.The domestic existing polycarboxylate water-reducer preparation high-strength concrete of the current employing mainly component such as composite thickening, viscosity reduction, but only deal with problems extremely limited by composite means, and effect is also undesirable, fresh concrete due to viscosity large fluidity can be poor, also take off end phenomenon with segregation simultaneously, so that cannot smooth construction; Although adopt external import polycarboxylate water-reducer to reach ideal effect, it is expensive, adds cost, more importantly its technical know-how, is unfavorable for the development of China's technology.
Patent publication No be CN102936112A patent describes a kind of polycarboxylate water-reducer being applicable to High-strength self-compaction concrete and preparation method thereof.This water reducer is mainly with the copolymerization and obtaining in 60 ~ 80 DEG C of aqueous solution of isopentene group Soxylat A 25-7, binary unsaturated carboxylic acid and derivative thereof, unitary unsaturated carboxylic acid and derivative thereof.Its innovation is to introduce the 4th monomer, and hydroxyl and sulfonic reaction promoter make the product of synthesis have higher dispersing property.As the polycarboxylate water-reducer for high-strength concrete, although this product can reduce concrete viscosity, but the slump and degree of mobilization hold facility limited, need with high collapse protection type polycarboxylate water-reducer compound use, so just have impact on its viscosity reducing effect and cost is also higher; Need the temperature being heated to 60 ~ 80 DEG C during this products production simultaneously, be unfavorable for energy-saving and emission-reduction.
Patent publication No is that a kind of tune that patent describes of CN103553413A glues type polycarboxylate water-reducer and preparation method thereof.This water reducer is mainly with unsaturated acrylic monomer, unsaturated polyoxy vinyl monomer with adjust allonge body (being mainly unsaturated alkyl ester, fluorinated ester, alkyl acrylamide or its mixture) copolymerization and obtaining in the aqueous solution of 70 ~ 90 DEG C.This water reducer significantly reduces the plastic viscosity of cement paste, but needs high temperature equally in process of production, and energy consumption is larger; Most importantly adjust allonge body to be first dissolved in water phase surfactant mixture, then participate in polyreaction, but in the end in product these tensio-active agents cannot remove.High performance water reducing agent of polyocarboxy acid belongs to air-entraining water-reducing agent originally, and tensio-active agent all has air-entraining function in varying degrees, and the product therefore obtained by the method probably causes high-strength concrete air content bigger than normal when applying, and its intensity cannot be ensured.
Patent publication No be CN102643042A patent describes a kind of cross-linking type polycarboxylate water-reducer.This water reducer is with the copolymerization and obtaining in the aqueous solution of 60 ~ 62 DEG C of methyl allyl alcohol polyoxyethylene ether, polyethylene glycol dimethacrylate, methylpropene sodium sulfonate and vinylformic acid.This water reducer, mainly using polyethylene glycol dimethacrylate as linking agent, utilizes its ester bond under alkaline environment, be hydrolyzed the effect that the principle discharging poly carboxylic acid molecule plays slump retention.But when being applied to the high-strength concrete of low water binder ratio, its effect is similar with the polycarboxylate water-reducer taking polyethylene glycol monomethyl ethermethacrylic acid esters as side chain, and cannot well be hydrolyzed, and keeps the slump and degree of mobilization; Simultaneously because the slump retention ability of methacrylic Soxylat A 25-7 is also limited, therefore this product also really cannot be satisfied the demand and be had the high-strength concrete requirement of superior fluidity energy; And because raw material double bond is active and initiator system, temperature required also higher during polyreaction, cannot low-temperature energy-saving be realized.
[summary of the invention]
High for solving energy consumption in the production of existing viscosity reduction type polycarboxylate water-reducer, result of use is undesirable, and product stability is difficult to the technical problem ensured, the invention provides a kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof.
The scheme of technical solution problem of the present invention is to provide a kind of viscosity reduction type polycarboxylate water-reducer, it is by the derivatives monomer a of 7% ~ 16% unsaturated acid or unsaturated acid, 80% ~ 92% relative molecular mass M is the isopentenol polyoxyethylene ether monomer b of 600 ~ 5000, with 6% ~ 13% glycol ester monomer c under the effect of redox system and chain-transfer agent, copolyreaction is there is in 10 DEG C ~ 60 DEG C aqueous solution, and obtain copolymer reactant after regulating PH to 6.8 with pH value conditioning agent, wherein, the weight sum of a, b, c monomer is 1;
The general formula of described monomer a is as follows:
Wherein: R1 is-H ,-COOH or-COOCH
3one or more in three kinds of groups, R2 is-H or-CH
3;
The chemical structural formula of monomer b is as follows:
Wherein: n is the average addition mole number of oxyethane chain link, and its value is 10 ~ 120.
The general formula of monomer c is as follows:
Wherein: R3, R4 are all selected from-HC=CH
2or
Preferably, the relative molecular mass M of described monomer b is 1200-2000.
Preferably, in the general formula of described monomer b, n is 10-80.
Preferably, in the general formula of described monomer b, n is 25 ~ 45.
Preferably, in described redox system, oxygenant comprises persulfate ion, hydrogen peroxide, reductive agent comprises sulfurous acid hydrogen radical ion, vitamins C, rongalite, ferrous sulfate ion, wherein oxygenant join that reaction mixture accounts for added monomer total mass 0.4% ~ 1.8%, reductive agent join that reaction mixture accounts for added monomer total mass 0.1% ~ 1.0%.
Preferably, described redox system be Sodium Persulfate and sodium bisulfite, ammonium persulphate and sodium bisulfite, ammonium persulphate and vitamins C, hydrogen peroxide and vitamins C, hydrogen peroxide and rongalite, hydrogen peroxide and ferrous ammonium sulphate any one or its combine.
Preferably, described chain-transfer agent is the mixture of a kind of or its above-mentioned substance in Thiovanic acid, mercaptoethanol, methylpropene sodium sulfonate or n-dodecyl mercaptan; The whole transfer agents added in reaction mixture account for 0.2% ~ 1.3% of added monomer total mass.
Preferably, described pH value conditioning agent is flap or the aqueous solution of sodium hydroxide or potassium hydroxide.
Another technical scheme that the present invention solves the problem is to provide a kind of preparation method possessing the viscosity reduction type polycarboxylate water-reducer of above-mentioned feature, it is characterized in that: comprise the following steps: in the glass reactor being configured with agitator, thermometer, Dropping feeder, add deionized water, isopentenol polyoxyethylene ether monomer b and glycol ester monomer c, heat while stirring, system temperature is kept to maintain 10 DEG C-60 DEG C, after material dissolution, drop into oxygenant; Then keep this temperature and in 3 ~ 3.5h, evenly drip the mixing solutions of reductive agent, chain-transfer agent and monomer a simultaneously; Drip rear insulation reaction 1h, then thin up is 40% to solid content, then to be neutralized to pH value with pH value conditioning agent be 6.8.
Compared with prior art, viscosity reduction type polycarboxylate water-reducer of the present invention can effectively reduce the slurry viscosity of low water binder ratio strong concrete, makes it meet construction requirement.And need not just have with high collapse protection type polycarboxylate water-reducer compound use the effect that the concrete slump and degree of mobilization are kept for a long time, reach the object of concrete long-distance transportation.In addition, viscosity reduction type polycarboxylate water-reducer of the present invention can synthesize under low temperature or normal temperature state, energy efficient, economic environmental protection.
[embodiment]
In order to make object of the present invention, technical scheme and advantage are clearly understood, below in conjunction with embodiment, are further elaborated to the present invention.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
In the embodiment of the present invention, if do not have other explanation, mentioned concentration is the abbreviation of mass percent concentration.Viscosity reduction type polycarboxylate water-reducer synthesized is in all embodiments designated as A, and in comparative example, existing water reducer is designated as B.
Embodiment 1
In the glass reactor being configured with agitator, thermometer, Dropping feeder, add the isopentenol polyoxyethylene ether monomer that 160g deionized water, 48.34g glycol diacrylate and 320.5g molecular weight M are 1800, heat while stirring, whole system temperature is kept to maintain 20 DEG C, treat material dissolution, drop into 1.92g30% hydrogen peroxide; Then keep this temperature and evenly drip the solution mixed with 80g deionized water by 0.61g vitamins C, 1.91g Thiovanic acid and the solution mixed with 120g deionized water by 31.2g vinylformic acid simultaneously in 3 ~ 3.5h; Drip rear maintenance 20 DEG C and continue reaction 1h, then thin up is 40% to solid content, then to be neutralized to pH value with pH value conditioning agent be 6.8, namely obtains product, is designated as A-1.
Described pH value conditioning agent is alkaline matter, includes but not limited to: the flap of sodium hydroxide, potassium hydroxide or the aqueous solution.In the present embodiment, pH value conditioning agent adopts sodium hydroxide solution.
Embodiment 2
In the glass reactor being configured with agitator, thermometer, Dropping feeder, add 155g deionized water, 12.11g toxilic acid, 51.21g EDIA maleic acid ester, 138.4g molecular weight M be 1200 isopentenol polyoxyethylene ether monomer and 173g molecular weight M be 1800 isopentenol polyoxyethylene ether monomer, warming while stirring, temperature drops into 2.82g sodium bisulfite after rising to 40 DEG C; Then keep this temperature and evenly drip the solution mixed with 105g deionized water by 6.45g ammonium persulphate and the solution mixed with 125g deionized water by 25.26g vinylformic acid, 4.70g methylpropene sodium sulfonate simultaneously in 3 ~ 3.5h; Drip rear maintenance 40 DEG C and continue reaction 1h, then thin up is 40% to solid content, then to be neutralized to pH value with pH value conditioning agent be 6.8, namely obtains product, is designated as A-2.
In the present embodiment, pH value conditioning agent adopts potassium hydroxide solution.
Embodiment 3
In the glass reactor being configured with agitator, thermometer, Dropping feeder, add the isopentenol polyoxyethylene ether monomer that 160g deionized water, 50.23g ethylene glycol dimethacrylate and 314g molecular weight M are 2000, warming while stirring, temperature rises to 50 DEG C, rear input 2.32g30% hydrogen peroxide; Then keep this temperature and evenly drip the solution mixed with 105g deionized water by 0.65g vitamins C, 0.40g ferrous ammonium sulphate, 1.47g mercaptoethanol and the solution mixed with 130g deionized water by 21.45g vinylformic acid, 14.39g methacrylic acid simultaneously in 3 ~ 3.5h; Drip rear maintenance 50 DEG C and continue reaction 1h, then thin up is 40% to solid content, then to be neutralized to pH value with pH value conditioning agent be 6.8, namely obtains product, is designated as A-3.
In the present embodiment, pH value conditioning agent adopts sodium hydroxide solution.
Embodiment 4
In the glass reactor being configured with agitator, thermometer, Dropping feeder, add the isopentenol polyoxyethylene ether monomer that 156g deionized water, 27.75g toxilic acid, 47.08g glycol diacrylate and 312.2g molecular weight M are 1800, heat while stirring, whole system temperature is kept to maintain 25 DEG C, treat material dissolution, drop into 2.30g30% hydrogen peroxide; Then keep this temperature and evenly drip the solution mixed with 80g deionized water by 0.62g vitamins C, 1.90g Thiovanic acid and the solution mixed with 87g deionized water by 13.00g vinylformic acid simultaneously in 3 ~ 3.5h; Drip rear maintenance 25 DEG C and continue reaction 1h, then thin up is 40% to solid content, then to be neutralized to pH value with pH value conditioning agent be 6.8, namely obtains product, is designated as A-4.
In the present embodiment, pH value conditioning agent adopts sodium hydroxide solution.
In above-described embodiment 1 to embodiment 4, temperature of reaction can be controlled in arbitrary temperature between 10 DEG C-60 DEG C, is preferably 20 DEG C, 25 DEG C, 40 DEG C, 50 DEG C, and vinylformic acid, toxilic acid, methacrylic acid are unsaturated acid monomer a, and its general formula can be expressed as:
Wherein: R1 is-H ,-COOH or-COOCH
3one or more in three kinds of groups, R2 is-H or-CH
3; Therefore in other embodiments, it can also be methyl-maleic acid, can also be the derivative of unsaturated acid as monomethyl maleate, can also be the mixing of above-mentioned substance.
Isopentenol polyoxyethylene ether is monomer b, and its relative molecular mass M is 600-5000, and be preferably 400-3650, more excellent is 1200-2000, and its polymerization degree is 10-120, and be preferably 10-80, more excellent is 25-45.Its general formula can be expressed as:
Wherein n is the polymerization degree.
Glycol diacrylate, ethylene glycol dimethacrylate or EDIA maleic acid ester are glycol ester monomer c, and its general formula can be expressed as:
Wherein: R3, R4 are all selected from-HC=CH
2or
Therefore, in other embodiments, it can also be the mixing of ethylene glycol bisthioglycolate maleic acid ester or above-mentioned substance.
In the total mass of derivatives monomer a, the isopentenol polyoxyethylene ether monomer b of unsaturated acid or unsaturated acid, glycol ester monomer c for 1, the derivatives monomer a of unsaturated acid or unsaturated acid accounts for 7%-16%, isopentenol polyoxyethylene ether monomer b accounts for 80%-92%, and glycol ester monomer c accounts for 6%-13%.
Thiovanic acid, mercaptoethanol are the chain-transfer agent of reaction, in other embodiments, chain-transfer agent can also be the mixing of methylpropene sodium sulfonate, n-dodecyl mercaptan or above-mentioned substance, and the whole transfer agents added in reaction mixture account for 0.2% ~ 1.3% of added monomer total mass.
In embodiment 1 in hydrogen peroxide and vitamins C, embodiment 2 in ammonium persulphate and sodium bisulfite, embodiment 3 in hydrogen peroxide and ferrous ammonium sulphate, embodiment 4 hydrogen peroxide and vitamins C form the redox system in respective embodiment, in described redox system, oxygenant includes but not limited to persulfate ion, hydrogen peroxide, and reductive agent includes but not limited to sulfurous acid hydrogen radical ion, vitamins C, rongalite, ferrous sulfate ion.Wherein oxygenant join that reaction mixture accounts for added monomer total mass 0.4% ~ 1.8%, reductive agent join that reaction mixture accounts for added monomer total mass 0.1% ~ 1.0%.
Comparative example 1
In the glass reactor being configured with agitator, thermometer, Dropping feeder, add the isopentenol polyoxyethylene ether monomer that 180g deionized water and 360g molecular weight M are 2000, warming while stirring, temperature rises to 50 DEG C, rear input 2.66g30% hydrogen peroxide; Then keep this temperature and evenly drip the solution mixed with 120g deionized water by 0.74g vitamins C, 0.46g ferrous ammonium sulphate, 1.68g mercaptoethanol and the solution mixed with 100g deionized water by 24.6g vinylformic acid, 16.5g methacrylic acid simultaneously in 3 ~ 3.5h; Drip rear maintenance 50 DEG C and continue reaction 1h, then thin up is 40% to solid content, then to be neutralized to pH value with sodium hydroxide be 6.8, namely obtains product, is set to B-1.
Comparative example 2
The polycarboxylate water-reducer B-2 synthesized for polymeric monomer with isopentene polyoxyethylenated alcohol that comparative example 2 is sold for market.
Implementation result compares:
By polycarboxylate water-reducer A-1, A-2, A-3, A-4 of obtaining by the inventive method, the poly carboxylic acid series water reducer (B-1, B-2) simultaneously relatively had now, carries out cement paste test and C80 concrete test.Wherein cement paste test surveys with reference to GB/T8077-2012 " Methods for testing uniformity of concrete admixture " standard its initial paste flowing degree, 1h paste flowing degree, 2h paste flowing degree also measure cement paste viscosity with reference to GB/T10274-2008 " Viscosity Measurement Methods "; Concrete test is with reference to the slump, the divergence after the first slump of GB8076-2008 " concrete admixture " canonical measure low water binder ratio high-strength concrete, divergence degree and 2h, and measure its slump bucket refluence time, and the relevant regulations of reference GB/T50081-2002 " standard for test methods of mechanical properties of ordinary concrete " measures the ultimate compression strength of maturing.Test cement is starfish little wild field P.O42.5R cement, and C80 concrete mix is in table 1, and cement paste test-results and concrete test result are respectively in table 2 and table 3.
Table 1C80 concrete mix
| C | FA | K | Si | S | G | W | Ad |
| 360 | 80 | 80 | 40 | 630 | 1120 | 140 | 12.32 |
Table 2 cement paste test-results
Table 3 concrete test result
From table 2, the viscosity reduction type polycarboxylate water-reducer obtained by the present invention, effectively can reduce the viscosity of cement slurry, and paste flowing degree retention is good; Also can find out that the high-strength concrete slump that the viscosity reduction type polycarboxylate water-reducer obtained by application the present invention makes, expansion ratio retention are good from table 3, and the time that flows backwards is short, good flowing properties, can meet engineering demand.
Compared with prior art, viscosity reduction type polycarboxylate water-reducer of the present invention can effectively reduce the slurry viscosity of low water binder ratio high-strength concrete, makes it meet construction requirement.And need not just have with high collapse protection type polycarboxylate water-reducer compound use the effect that the concrete slump and degree of mobilization are kept for a long time, reach the object of concrete long-distance transportation.In addition, viscosity reduction type polycarboxylate water-reducer of the present invention can synthesize under low temperature or normal temperature state, energy efficient, economic environmental protection.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within principle of the present invention, equivalent replacement and improvement etc. all should comprise within protection scope of the present invention.
Claims (9)
1. a viscosity reduction type polycarboxylate water-reducer, it is characterized in that: it is by the derivatives monomer a of 7% ~ 16% unsaturated acid or unsaturated acid, 80% ~ 92% relative molecular mass M is the isopentenol polyoxyethylene ether monomer b of 600 ~ 5000, with 6% ~ 13% glycol ester monomer c under the effect of redox system and chain-transfer agent, copolyreaction is there is in 10 DEG C ~ 60 DEG C aqueous solution, and obtain copolymer reactant after regulating PH to 6.8 with pH value conditioning agent, wherein, the weight sum of a, b, c monomer is 1;
The general formula of described monomer a is as follows:
Wherein: R1 is-H ,-COOH or-COOCH
3one or more in three kinds of groups, R2 is-H or-CH
3;
The chemical structural formula of monomer b is as follows:
Wherein: n is the average addition mole number of oxyethane chain link, and its value is 10 ~ 120.
The general formula of monomer c is as follows:
Wherein: R3, R4 are all selected from-HC=CH
2or
2. viscosity reduction type polycarboxylate water-reducer as claimed in claim 1, is characterized in that: the relative molecular mass M of described monomer b is 1200-2000.
3. viscosity reduction type polycarboxylate water-reducer as claimed in claim 1, is characterized in that: in the general formula of described monomer b, n is 10-80.
4. viscosity reduction type polycarboxylate water-reducer as claimed in claim 3, is characterized in that: in the general formula of described monomer b, n is 25 ~ 45.
5. viscosity reduction type polycarboxylate water-reducer as claimed in claim 1, it is characterized in that: in described redox system, oxygenant comprises persulfate ion, hydrogen peroxide, reductive agent comprises sulfurous acid hydrogen radical ion, vitamins C, rongalite, ferrous sulfate ion, wherein oxygenant join that reaction mixture accounts for added monomer total mass 0.4% ~ 1.8%, reductive agent join that reaction mixture accounts for added monomer total mass 0.1% ~ 1.0%.
6. viscosity reduction type polycarboxylate water-reducer as claimed in claim 1, is characterized in that: described redox system is any one or multiple combination of Sodium Persulfate and sodium bisulfite, ammonium persulphate and sodium bisulfite, ammonium persulphate and vitamins C, hydrogen peroxide and vitamins C, hydrogen peroxide and rongalite, hydrogen peroxide and ferrous ammonium sulphate.
7. viscosity reduction type polycarboxylate water-reducer as claimed in claim 1, is characterized in that: described chain-transfer agent is the mixture of a kind of or its above-mentioned substance in Thiovanic acid, mercaptoethanol, methylpropene sodium sulfonate or n-dodecyl mercaptan; The whole chain-transfer agents added in reaction mixture account for 0.2% ~ 1.3% of added monomer total mass.
8. viscosity reduction type polycarboxylate water-reducer as claimed in claim 1, is characterized in that: described pH value conditioning agent is flap or the aqueous solution of sodium hydroxide or potassium hydroxide.
9. the preparation method of the viscosity reduction type polycarboxylate water-reducer as described in any one of claim 1-8, it is characterized in that: comprise the following steps: in the glass reactor being configured with agitator, thermometer, Dropping feeder, add deionized water, isopentenol polyoxyethylene ether monomer b and glycol ester monomer c, heat while stirring, system temperature is kept to maintain 10 DEG C-60 DEG C, after material dissolution, drop into oxygenant; Then keep this temperature and in 3 ~ 3.5h, evenly drip the mixing solutions of reductive agent, chain-transfer agent and monomer a simultaneously; Drip rear insulation reaction 1h, then thin up is 40% to solid content, then to be neutralized to pH value with pH value conditioning agent be 6.8.
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| CN106967200A (en) * | 2017-03-31 | 2017-07-21 | 刘翠芬 | It is a kind of to have poly carboxylic acid series water reducer that guarantor is collapsed with viscosity-reducing performance and preparation method thereof concurrently |
| CN109053974A (en) * | 2018-07-23 | 2018-12-21 | 中铁四局集团有限公司 | Preparation method of viscosity-reducing polycarboxylate superplasticizer |
| CN109721722A (en) * | 2018-12-25 | 2019-05-07 | 广东红墙新材料股份有限公司 | A kind of viscosity reduction type polycarboxylate water-reducer and its preparation method and application containing double down viscous functional group |
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| CN113968692A (en) * | 2021-12-03 | 2022-01-25 | 湖南先锋建材有限公司 | High-strength concrete viscosity-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN114057956A (en) * | 2021-12-07 | 2022-02-18 | 中建西部建设新材料科技有限公司 | Water-reducing slump-retaining comprehensive polycarboxylic acid water reducer and preparation method thereof |
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| CN114057956A (en) * | 2021-12-07 | 2022-02-18 | 中建西部建设新材料科技有限公司 | Water-reducing slump-retaining comprehensive polycarboxylic acid water reducer and preparation method thereof |
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