CN103739790A - Slow-release collapse-preventing type polycarboxylic water reducing agent and preparation method thereof - Google Patents
Slow-release collapse-preventing type polycarboxylic water reducing agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses slow-release collapse-preventing type polycarboxylic water reducing agent and a preparation method thereof, and belongs to the field of preparation of the water reducing agent. The slow-release collapse-preventing type polycarboxylic water reducing agent consists of methyl allyl polyoxyethylene ether, acrylic acid, methyl acrylic polyethylene glycol monoester, imide, initiator, vitamin C, chain transfer agent and deionized water. The preparation method comprises the following steps of: preparing macromonomer methyl allyl polyoxyethylene ether, acrylic acid, methyl acrylic polyethylene glycol monoester, imide and vitamin C; under the action of the polymerization initiator and the chain transfer agent, dissolving the methyl allyl polyoxyethylene ether into deionized water, rising temperature to 40 DEG C for dissolving, adding the initiator, then respectively dripping water solution A prepared by dissolving the chain transfer agent, the acrylic acid, the methyl acrylic polyethylene glycol monoester and the imide in the deionized water and V.C water solution B, and after the dripping is finished, carrying out insulation, cooling and neutralization to obtain a finished product. The slow-release collapse-preventing type polycarboxylic water reducing agent disclosed by the invention has the advantages that the loss and the evaporation of water in concrete due to long-time transportation and higher temperature are effectively prevented, and the difficulty of excessively-fast slump loss of the concrete in engineering is solved.
Description
Technical field
The present invention relates to a kind of poly carboxylic acid series water reducer, or rather, relate to a kind of slowly-releasing slump-retaining polycarboxylic acid type water reducing agent and preparation method thereof.
Background technology
Along with the quickening of national urbanization process and the development of large-scale basis facility, concrete and cement increase day by day as the usage quantity of artificial works important materials.In order to realize Society and to meet the demands such as continuous some that occur are large-scale, the construction of mega-construction project, intensity, commerical ready-mixed concrete is had higher requirement.In order to keep the serviceability that concrete is good, meet the needs of various engineerings, need in fresh concrete, add the water reducer of difference in functionality.In the water reducer of various series, poly carboxylic acid series water reducer is as the third generation high-performance water reducing agent growing up after the s-generation high efficiency water reducing agents such as the first-generation ordinary water-reducing agents such as wooden calcium and naphthalene system, has that volume is low, water-reducing rate is high, a mixture workability and serviceability retentivity is good, compare the series of advantages such as Plastic Shrinkage of Concrete impact is little, environmentally safe with naphthalene system and be used widely.
But, poly carboxylic acid series water reducer synthetic method is various at present, quality differs, in addition concrete raw material quality fluctuation is large, performance variation is fast, caused such water reducer problem incompatible with starting material in actual applications, especially shown as that fresh concrete Slump Time losing of Large is too fast, bleeding segregation phenomenon is serious.This causes engineering to construct, and has not only wasted human and material resources, returns engineering construction and concrete engineering quality control brings a lot of inconvenience.For this reason, in the urgent need to developing a kind of high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent, to improve the performance of polycarboxylate water-reducer product, the kind of widening concrete admixture meets the requirement of different engineerings.
Mixing water reducer concrete slump loss has the reason of two aspects, is to be on the one hand physical cause because the physical dispersion of cement declines electrokinetic potential, be on the other hand due to the initial stage hydration reaction of cement to make water reducer consumption be chemical principle because of.And major cause is to have accelerated the initial stage hydration process of cement adding of water reducer, and adsorption reduces the effective concentration of water reducer in liquid phase very soon, and the electrokinetic potential of system constantly declines.By the method that solves water reducer slump-loss, mainly contain several at present: (1) compound slow setting component; (2) repeatedly repeatedly add water reducer; (3) addition after water reducer; (4) sustained release method; (5) composite reactive polymer multipolymer.And during normally used method, composite slow setting component in water reducer, but the long requirement that can not meet engineering construction time of coagulation sometimes.Therefore the structure that needs to change poly carboxylic acid extends the time of itself and concrete effect and increases the hold facility of its slump.
Summary of the invention
1, the technical problem that invention will solve
The present invention is directed to fresh concrete slump-loss large, and most water reducer is indeterminable technical problem again, the invention provides a kind of slowly-releasing slump-retaining polycarboxylic acid type water reducing agent and preparation method thereof, acquisition reduces fresh concrete slump-loss, strengthen the adaptability of polycarboxylate water-reducer and various cement, and extend itself and with the concrete beneficial effect of action time.
2, technical scheme
The present invention addresses the above problem adopted technical scheme:
A preparation method for slowly-releasing slump-retaining polycarboxylic acid type water reducing agent, comprises the following steps:
(1) prepare desired raw material, wherein: large monomer methacrylic Soxylat A 25-7 (molecular weight 1200～2950) accounts for 30%～65% of monomer total mass, vinylformic acid accounts for 10%～20% of monomer total mass, Methacrylate Polyglycol Monoester accounts for 5%～15% of monomer total mass, imide accounts for 10%～15% of monomer total mass, initiator accounts for 0.01%～0.1% of monomer total mass, and V.C ((vitamins C, hereinafter to be referred as V.C)) accounts for 0.1%～0.5% of monomer total mass; Chain-transfer agent consumption accounts for 0.01%～0.2% of monomer total mass, and 38%～45%(solution total mass that deionized water accounts for solution total mass is the total mass that adds the mixture of all substances in flask); The wherein quality of methacrylic Soxylat A 25-7, vinylformic acid, Methacrylate Polyglycol Monoester, 4 kinds of monomers of imide and be monomer total mass;
(2) according to the ratio in step (1), large monomer methacrylic Soxylat A 25-7 is dropped in the four-hole boiling flask with agitator and thermometer, being dissolved in deionized water, to make massfraction be 55%～65% solution, is warming up to 40 ℃ of dissolvings, adds initiator until temperature-stable during at 40 ℃;
(3), by vinylformic acid, Methacrylate Polyglycol Monoester and imide, mix and be dissolved in that in deionized water, to make massfraction be 56%～62% water solution A;
(4) chain-transfer agent and V.C are dissolved in deionized water, make massfraction and be 0.02%～0.04% aqueous solution B;
(5), when solution temperature rises to 50 ℃～65 ℃ in step (2) flask, in flask, start to drip the water solution A and the aqueous solution B that in step (3) and (4), make, time for adding approximately 1～2 hour;
(6) after dropwising, 50 ℃～65 ℃ insulations 2-3 hour, cool to 40 ℃, add liquid caustic soda to be neutralized to pH6-8, obtain slowly-releasing slump-retaining polycarboxylic acid type water reducing agent.
In the present invention, described raw material, wherein: large monomer methacrylic Soxylat A 25-7 (molecular weight 1200～2950) accounts for 30%～65% of monomer total mass, vinylformic acid accounts for 10%～20% of monomer total mass, Methacrylate Polyglycol Monoester accounts for 5%～15% of monomer total mass, imide accounts for 10%～15% of monomer total mass, and V.C accounts for 0.1%～0.5% of monomer total mass; Chain-transfer agent consumption accounts for 0.01%～0.2% of monomer total mass, deionized water accounts for 38%～45% of solution total mass, wherein the quality of methacrylic Soxylat A 25-7, vinylformic acid, Methacrylate Polyglycol Monoester and 4 kinds of monomers of imide and be monomer total mass.
In the present invention, it is one or more in 1200,2000,2400 or 2950 that the molecular weight of described large monomer methacrylic Soxylat A 25-7 is preferably.
In the present invention, described imide is that to utilize polyalcohol amine and maleic anhydride be raw material, under the effect of catalyzer 4-diformyl pyridine and hydroquinone of polymerization retarder, is warming up to 80～120 ℃, then constant temperature is lowered the temperature after 2～4 hours and obtained.Wherein the mol ratio of maleic anhydride and polyalcohol amine is 2～4:1, and catalyzer accounts for 0.1%～0.5% of raw material total mass, and stopper accounts for 0.01%～0.1% of raw material total mass.
In the present invention, described imide is hydrolyzed and discharges the polyalcohol amine that has adsorbing carboxylic acid group and have early strength function in concrete alkaline environment.
In the present invention, described initiator is that massfraction is 35% hydrogen peroxide.
In the present invention, described chain-transfer agent is thiohydracrylic acid.
3, beneficial effect
The present invention is by adopting technique scheme, obtained the poly carboxylic acid series water reducer that a kind of slump retaining is good, have slow-release function, mix concrete, can extend the time of itself and concrete effect and increase the slump hold facility of fresh concrete, compared with other technologies, can obtain following beneficial effect:
1, to use methacrylic Soxylat A 25-7 be that large monomer and vinylformic acid are for minor comonomer is as polycarboxylate water-reducer component in the present invention, this large monomer has the high feature of high, the two key retention rate of reactive behavior, can carry out good copolymerization with acrylic acid or the like minor comonomer, synthetic water reducer has that water-reducing rate is large, function of slump protection good, the feature (large monomer be polymkeric substance that molecular weight larger, minor comonomer be the material of molecular weight) good with various cement adaptabilities.
2, Methacrylate Polyglycol Monoester and imide are as polycarboxylate water-reducer component, there is the effect of the following aspects: the PEO side chain of (1) Methacrylate Polyglycol Monoester provides stronger sterically hindered, can significantly improve the dispersed of water reducer and disperse retentivity; (2) imide that imide provides also can improve dispersiveness and the stability of water reducer, and imide can be hydrolyzed and discharges the polyalcohol amine that has adsorbing carboxylic acid group and have early strength function in concrete alkaline environment; (3) take imide and polyoxyethylene glycol as the polycarboxylate water-reducer of side chain, have both sexes structure, the poly carboxylic acid of both sexes structure has unique dispersive ability, and performance is quite superior; (4) monoesters base and imide can get up a part of carboxyl " protection " on poly carboxylic acid main chain; in concrete alkaline environment condition, issue raw hydrolysis reaction; discharge the hydrolysate containing carboxylic acid group; constantly there is carboxylic acid group to be adsorbed on cement particle surface; can continue to keep the dispersiveness of cement granules; effectively keep concrete mobility, thereby reach slowly-releasing, protected the object of collapsing.
3, preparation method of the present invention adopts water solution polymerization process, and temperature of reaction is low, and the required reaction times is shorter, and reaction unit is simple to operation, pollution-free.
Embodiment
A preparation method for slow-release type polycarboxylate water reducer, is characterized in that comprising the following steps:
(1) prepare desired raw material, wherein: large monomer methacrylic Soxylat A 25-7 (molecular weight 1200～2950) accounts for 30%～65% of monomer total mass, vinylformic acid accounts for 10%～20% of monomer total mass, Methacrylate Polyglycol Monoester accounts for 5%～15% of monomer total mass, imide accounts for 10%～15% of monomer total mass, initiator accounts for 0.01%～0.1% of monomer total mass, and V.C accounts for 0.1%～0.5% of monomer total mass; Chain-transfer agent consumption accounts for 0.01%～0.2% of monomer total mass, and deionized water accounts for 38%～45% of solution total mass; The wherein quality of methacrylic Soxylat A 25-7, vinylformic acid, Methacrylate Polyglycol Monoester, 4 kinds of monomers of imide and be monomer total mass;
(2) according to the ratio in step (1), large monomer methacrylic Soxylat A 25-7 is dropped in the four-hole boiling flask with agitator and thermometer, being dissolved in deionized water, to make massfraction be 55%～65% solution, is warming up to 40 ℃ of dissolvings, adds initiator until temperature-stable during at 40 ℃;
(3), by vinylformic acid, Methacrylate Polyglycol Monoester, imide, mix and be dissolved in that in deionized water, to make massfraction be 56%～62% water solution A;
(4) chain-transfer agent and V.C are dissolved in deionized water, make massfraction and be 0.02%～0.04% aqueous solution B;
(5), when solution temperature rises to 50 ℃～65 ℃ in step (2) flask, in flask, start to drip the water solution A and the aqueous solution B that in step (3) and (4), make, time for adding approximately 1～2 hour;
(6) after dropwising, 50 ℃～65 ℃ insulations 2-3 hour, cool to 40 ℃, add liquid caustic soda to be neutralized to pH6-8, obtain high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent.
For illustrating further content of the present invention, spy enumerates following examples.Embodiment provides in the mode of explanation, but is never only confined to content of the present invention.The test of the concrete performance examination of three embodiment is all under equal conditions carried out below, and its test conditions is:
Gelling material adopts ordinary Portland cement, and fine aggregate adopts medium sand, and coarse aggregate adopts rubble (5-25mm, continuous size fraction) mixing C30 concrete, and admixture dosage is the solid volume of folding.
Embodiment 1
A preparation method for slowly-releasing slump-retaining polycarboxylic acid type water reducing agent, comprises the following steps:
(1) being equipped with in the four-hole boiling flask of agitator and thermometer, add methacrylic Soxylat A 25-7 (molecular weight 1200) 125.5g and deionized water 117.6g, warming while stirring to 40 ℃ dissolving; Until temperature-stable, during at 40 ℃, add the hydrogen peroxide of 2.42g mass percent concentration 35%.
(2) take respectively, vinylformic acid 58.8g, Methacrylate Polyglycol Monoester 42.2g, imide 56.5g, is dissolved in 68g deionized water, makes water solution A.
(3) take thiohydracrylic acid 0.18g, V.C0.4g, is dissolved in 27.4g deionized water, makes aqueous solution B.
(4) when solution temperature rises to 50 ℃ in step (1) flask, in flask, start to drip the water solution A and the aqueous solution B that in step (2) and (3), make, time for adding is about respectively 1.5 and 2 hours.
(5) after dropwising, 50 ℃ of insulations 2 hours, cool to 40 ℃, add liquid caustic soda to be neutralized to pH6, obtain high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent.
Before step 1, also comprise and prepare required reaction raw materials.
Described imide, it,, take polyalcohol amine and maleic anhydride as raw material, under the effect of catalyzer 4-diformyl pyridine and hydroquinone of polymerization retarder, is warming up to 80～120 ℃, then constant temperature is lowered the temperature after 2～4 hours and obtained; Wherein the mol ratio of maleic anhydride and polyalcohol amine is 2～4:1, and catalyzer accounts for 0.1%～0.5% of raw material total mass, and stopper accounts for 0.01%～0.1% of raw material total mass.
In concrete, add 0.2% this product that accounts for gelling material gross weight, water-reducing rate is 28.6%, and concrete mix 1h slump rheological parameters' change with time amount is 15mm, 1d compressive strength rate is 190%, 3d compressive strength rate is that 172%, 7d compressive strength rate is that 160%, 28d compressive strength rate is 143%.
Embodiment 2
A preparation method for slowly-releasing slump-retaining polycarboxylic acid type water reducing agent, comprises the following steps:
(1) being equipped with in the four-hole boiling flask of agitator and thermometer, add methacrylic Soxylat A 25-7 (molecular weight 2400) 182.5g and deionized water 99.9g, warming while stirring to 40 ℃ dissolving; Until temperature-stable, during at 40 ℃, add the hydrogen peroxide of 1.66g35%.
(2) take respectively vinylformic acid 60.8g, Methacrylate Polyglycol Monoester 23.5g, a kind of self-control imide 36.2g, is dissolved in 80.3g deionized water, makes water solution A.
(3) take thiohydracrylic acid 0.08g, V.C0.36g, is dissolved in 16.8g deionized water, makes aqueous solution B.
(4) when solution temperature rises to 60 ℃ in step (1) flask, in flask, start to drip the water solution A and the water liquid B that in step (2) and (3), make, time for adding is about respectively 1.5 and 2 hours.
(5) after dropwising, 60 ℃ of insulations 2.5 hours, cool to 40 ℃, add liquid caustic soda to be neutralized to pH7, obtain high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent.
Other steps are with embodiment 1.
In concrete, add 0.2% this product that accounts for gelling material gross weight, water-reducing rate is 33.8%, and concrete mix 1h slump rheological parameters' change with time amount is 10mm, 1d compressive strength rate is 195%, 3d compressive strength rate is that 178%, 7d compressive strength rate is that 165%, 28d compressive strength rate is 150%.
Embodiment 3
A preparation method for high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent, comprises the following steps:
(1) being equipped with in the four-hole boiling flask of agitator and thermometer, add methacrylic Soxylat A 25-7 (molecular weight 2950) 158.2g and deionized water 117.6g, warming while stirring to 40 ℃ dissolving; Until temperature-stable, during at 40 ℃, add the hydrogen peroxide of 1.97g35%.
(2) take respectively vinylformic acid 50.1g, Methacrylate Polyglycol Monoester 31.7g, imide 42.0g, is dissolved in 72.8g deionized water, makes water solution A.
(3) take thiohydracrylic acid 0.13g, V.C0.4g, is dissolved in 25.1g deionized water, makes aqueous solution B.
(4) when solution temperature rises to 60 ℃ in step (1) flask, in flask, start to drip the water solution A and the aqueous solution B that in step (2) and (3), make, time for adding is about respectively 1.5 and 2 hours.
(5) after dropwising, 60 ℃ of insulations 3 hours, cool to 40 ℃, add liquid caustic soda to be neutralized to pH8, obtain high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent.
Other steps are with embodiment 1.
In concrete, add 0.3% this product that accounts for gelling material gross weight, water-reducing rate is 32.7%, and concrete mix 1h slump rheological parameters' change with time amount is 15mm, 1d compressive strength rate is 192%, 3d compressive strength rate is that 175%, 7d compressive strength rate is that 157%, 28d compressive strength rate is 146%.
Embodiment 4
A preparation method for high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent, comprises the following steps:
(1) being equipped with in the four-hole boiling flask of agitator and thermometer, add methacrylic Soxylat A 25-7 (molecular weight 2400,2950) 190.2g and deionized water 100.8g, warming while stirring to 40 ℃ dissolving; Until temperature-stable, during at 40 ℃, add the hydrogen peroxide of 2.31g35%.
(2) take respectively vinylformic acid 47.6g, Methacrylate Polyglycol Monoester 23.8g, a kind of self-control imide 33.3g, is dissolved in 82.4g deionized water, makes water solution A.
(3) take thiohydracrylic acid 0.07g, V.C0.32g, is dissolved in 19.2g deionized water, makes aqueous solution B.
(4) when solution temperature rises to 65 ℃ in step (1) flask, in flask, start to drip the water solution A and the aqueous solution B that in step (2) and (3), make, time for adding is about respectively 1.5 and 2 hours.
(5) after dropwising, 65 ℃ of insulations 2 hours, cool to 40 ℃, add liquid caustic soda to be neutralized to pH8, obtain high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent.
Other steps are with embodiment 1.
In concrete, add 0.2% this product that accounts for gelling material gross weight, water-reducing rate is 30.0%, and concrete mix 1h slump rheological parameters' change with time amount is 10mm, 1d compressive strength rate is 190%, 3d compressive strength rate is that 175%, 7d compressive strength rate is that 160%, 28d compressive strength rate is 148%.
Claims (6)
1. a preparation method for slowly-releasing slump-retaining polycarboxylic acid type water reducing agent, is characterized in that comprising the following steps:
(1) prepare desired raw material, wherein: the large monomer methacrylic Soxylat A 25-7 that molecular weight is 1200～2950 accounts for 30%～65% of monomer total mass, vinylformic acid accounts for 10%～20% of monomer total mass, Methacrylate Polyglycol Monoester accounts for 5%～15% of monomer total mass, imide accounts for 10%～15% of monomer total mass, initiator accounts for 0.01%～0.1% of monomer total mass, V.C accounts for 0.1%～0.5% of monomer total mass, chain-transfer agent consumption accounts for 0.01%～0.2% of monomer total mass, and deionized water accounts for 38%～45% of solution total mass; The wherein quality of methacrylic Soxylat A 25-7, vinylformic acid, Methacrylate Polyglycol Monoester and 4 kinds of monomers of imide and be monomer total mass;
(2) according to the ratio in step (1), large monomer methacrylic Soxylat A 25-7 is dropped in the four-hole boiling flask with agitator and thermometer, being dissolved in deionized water, to make massfraction be 55%～65% solution, is warming up to 40 ℃ of dissolvings, adds initiator until temperature-stable during at 40 ℃;
(3), by vinylformic acid, Methacrylate Polyglycol Monoester, imide, mix and be dissolved in that in deionized water, to make massfraction be 56%～62% water solution A;
(4) chain-transfer agent and V.C are dissolved in deionized water, make massfraction and be 0.02%～0.04% aqueous solution B;
(5), when solution temperature rises to 50 ℃～65 ℃ in step (2) flask, in flask, start to drip the water solution A and the aqueous solution B that in step (3) and (4), make, time for adding approximately 1～2 hour;
(6) after dropwising, 50 ℃～65 ℃ insulations 2-3 hour, cool to 40 ℃, add liquid caustic soda to be neutralized to pH6-8, obtain high-efficiency sustained-release slump-retaining polycarboxylic acid type water reducing agent.
2. a slow-release type polycarboxylate water reducer, comprises large monomer methacrylic Soxylat A 25-7, vinylformic acid, Methacrylate Polyglycol Monoester, imide, initiator, V.C, chain-transfer agent and deionized water; Each constituent mass per-cent is: molecular weight is that 1200～2950 large monomer methacrylic Soxylat A 25-7s account for 30%～65% of monomer total mass, vinylformic acid accounts for 10%～20% of monomer total mass, Methacrylate Polyglycol Monoester accounts for 5%～15% of monomer total mass, imide accounts for 10%～15% of monomer total mass, and the total consumption of initiator and V.C accounts for 0.5%～4% of monomer total mass; Chain-transfer agent consumption accounts for 0.01%～0.2% of monomer total mass, the wherein quality of methacrylic Soxylat A 25-7, vinylformic acid, Methacrylate Polyglycol Monoester and 4 kinds of monomers of imide and be monomer total mass, deionized water accounts for 38%～45% of solution total mass.
3. slow-release type polycarboxylate water reducer according to claim 2, is characterized in that, described large monomer methacrylic Soxylat A 25-7 is one or more the large monomer methacrylic Soxylat A 25-7s in molecular weight 1200,2000,2400 or 2950.
4. a kind of slowly-releasing slump-retaining polycarboxylic acid type water reducing agent according to claim 2, it is characterized in that, described imide, it is take polyalcohol amine and maleic anhydride as raw material, under the effect of catalyzer 4-diformyl pyridine and hydroquinone of polymerization retarder, be warming up to 80～120 ℃, then constant temperature is lowered the temperature after 2～4 hours and to be obtained; Wherein the mol ratio of maleic anhydride and polyalcohol amine is 2～4:1, and catalyzer accounts for 0.1%～0.5% of raw material total mass, and stopper accounts for 0.01%～0.1% of raw material total mass.
5. slowly-releasing slump-retaining polycarboxylic acid type water reducing agent according to claim 1 and 2, is characterized in that, described initiator is that massfraction is 35% hydrogen peroxide solution.
6. slowly-releasing slump-retaining polycarboxylic acid type water reducing agent according to claim 1 and 2, is characterized in that, described chain-transfer agent is thiohydracrylic acid.
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