CN105017491A - Early-strength polycarboxylate superplasticizer and preparation method thereof - Google Patents
Early-strength polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- CN105017491A CN105017491A CN201510522172.XA CN201510522172A CN105017491A CN 105017491 A CN105017491 A CN 105017491A CN 201510522172 A CN201510522172 A CN 201510522172A CN 105017491 A CN105017491 A CN 105017491A
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Abstract
The invention discloses an early-strength polycarboxylate superplasticizer and a preparation method thereof. The water reducer is prepared from raw materials in parts by weight as follows: 200 parts of unsaturated polyether, 10-30 parts of acrylic acid, 1-3 parts of an amide derivative, 0.1-0.5 parts of mohr's salt, 0.5-1.5 parts of a chain transfer agent, 0.2-0.8 parts of L-ascorbic acid, 0.8-4 parts of an oxidizing agent, 230 parts of deionized water and 12-20 parts of a 30% sodium hydroxide solution. The unsaturated polyether with a larger molecular weight is used, that is, a long side chain is introduced into a polycarboxylate superplasticizer molecule, quaternary amine and amide functional groups exist on a main chain, early hydration of hydration products, namely C3A and C3S, can be promoted, crystallization of Ca(OH)2 and forming of ettringite can be accelerated, the concrete setting time can be effectively shortened, the compactness of an early microstructure is improved, the early mechanical property of cement grout can be substantially improved, and the polycarboxylate superplasticizer promotes early-strength development of concrete and shows excellent early-strength performance from a macroscopic view.
Description
Technical field
The invention belongs to the technical field of material of construction, particularly relate to a kind of high-early strength type polycarboxylic acids dehydragent and preparation method thereof.
Background technology
The construction of many engineerings such as various industry and covil construction, road and rail bridge, airfield runway, [underground, hydro-structure, ocean exploitation, geothermal engineering and military affairs all be unable to do without concrete, compared with other material of construction, concrete has the features such as starting material are easy to get, applied widely, energy waste is low, long service life.
Along with the quickening of concrete works project construction, the consumption of precast concrete product also presents ever-increasing trend.Compared to normal concrete, precast concrete requires that concrete has good early strength development speed, to improve form cycling rate, or meets the strength development under cold condition.Realize early strong technological approaches by using concrete admixture and have two kinds: one is synthesizing mean, namely in the admixture molecular structure used, itself is containing Zao Qiang functional group, energy acceleration of hydration process, early strong Be very effective, fundamentally Molecular Structure Design can reach desired function, be ideal technology solution route; Another kind of composite means, namely have early powerful inorganics, organism etc. by composite, make concrete reach early potent fruit, but early potent fruit are general comparatively limited.
Common mainly contains sulfonated lignin ordinary water-reducing agent, naphthalenesulfonate formaldehyde condensation compound high efficiency water reducing agent and polycarboxylate high performance water-reducing agent by the concrete admixture of synthesis preparation.Wherein polycarboxylate high performance water-reducing agent can cut out principle of design according to polymer molecule, by free radical copolymerization, polymerizable structural unit is synthesized the water reducer of predetermined structure and performance, by adjustment monomer component and between proportionlity, choose high reaction activity monomer and initiator etc., finally obtain poly carboxylic acid main chain, the side chain containing desirable molecular structure that can meet specific demand, and make it have the polymkeric substance of certain electric density and molecular conformation molecular structure.
The research of high-early strength type polycarboxylic acids dehydragent becomes study hotspot, a lot of research institution is had to conduct a research to this at present, as CN201210554672.8, CN201310371075.6, CN201410012420.1 and CN 201510127668.7, all disclose the preparation method of high-early strength type polycarboxylic acids dehydragent, general employing oxidation-reduction body carries out aqueous solution polymerization and forms, needed various materials to drip in reaction process simultaneously, and need in a heated condition, process is not easy to control, product performance can not meet the time of coagulation of special concrete (as subway segment concrete) and early strong requirement mostly simultaneously.
Summary of the invention
The object of the invention is to overcome prior art defect, a kind of high-early strength type polycarboxylic acids dehydragent is provided.
Another object of the present invention is to the preparation method that above-mentioned high-early strength type polycarboxylic acids dehydragent is provided
Concrete technical scheme of the present invention is as follows:
A kind of high-early strength type polycarboxylic acids dehydragent, be made up of the raw material of following weight part: unsaturated polyether 200 weight part, vinylformic acid 10 ~ 30 weight part, amide derivatives 1 ~ 3 weight part, Mohr's salt 0.1 ~ 0.5 weight part, chain-transfer agent 0.5 ~ 1.5 weight part, L-AA 0.2 ~ 0.8 weight part, oxygenant 0.8 ~ 4 weight part, deionized water 230 weight part and 30% sodium hydroxide solution 12 ~ 20 weight part, wherein
The molecular formula of unsaturated polyether is CH
2=CH (CH
3) CH
2cH
2o (CH
2cH
2o)
m(CH
2cH
3cHO)
nh (methyl thiazolinyl polyoxyethylene, polyethenoxy ether, with reference to http://www.oxiranchem.com/gufen/product.php? form_id=1225 & bigkind=03 & kind=0302), wherein, m is the integer of 70 ~ 110, n is the integer of 1 ~ 10, and 70≤m+n≤120;
Quaternary ammonium salt is diallyldimethylammonium chloride, dimethyl diallyl brometo de amonio, allyl group trimethyl ammonium chloride or allyl group trimethylammonium bromide;
Amide derivatives is N hydroxymethyl acrylamide, 2-methyl propane sulfonic acid acrylamide or N,N methylene bis acrylamide.
In a preferred embodiment of the invention, described chain-transfer agent is 2 mercapto ethanol, 2-Thiovanic acid, 3-mercaprol or 3-thiohydracrylic acid.
In a preferred embodiment of the invention, described oxygenant is hydrogen peroxide, t-butyl hydroperoxide, hydrogen phosphide cumene or di-isopropylbenzene hydroperoxide.
A preparation method for above-mentioned high-early strength type polycarboxylic acids dehydragent, comprises the steps:
(1) unsaturated polyether, 5 ~ 10 parts by weight of acrylic acid, quaternary ammonium salt, amide derivatives, Mohr's salt and 200 parts by weight of deionized water are stirred;
(2) remaining vinylformic acid, chain-transfer agent, L-AA and remaining deionized water are mixed, obtain mixing solutions;
(3) controlling reacting initial temperature is 10 ~ 30 DEG C, in the material of step (1) disposable add oxygenant after, open the mixing solutions dripping step (2) wherein, dropwise in 30 ~ 45min, after dripping, continue at 35 ~ 45 DEG C of insulation reaction 30 ~ 40min;
(4) place 12 ~ 24h after material obtained for step (3) being cooled to room temperature, then add 30% sodium hydroxide solution wherein and neutralize, obtain described high-early strength type polycarboxylic acids dehydragent.
The invention has the beneficial effects as follows:
1, the unsaturated polyether that the molecular weight used in high-early strength type polycarboxylic acids dehydragent of the present invention is larger, namely introduces long side chain, and main chain has quaternary amine and amide functional group in polycarboxylate water-reducer molecule, can facilitate hydrated product C in cement slurry
3a and C
3the early hydration of S, can accelerate Ca (OH)
2crystallization and the formation of ettringite, effectively can shorten concrete coagulating time, improve the degree of compactness of early stage microtexture, significantly improve the early mechanics characteristics of cement slurry, there is promoter action to concrete early strength development, macroscopically show as superior epistasis energy morning.
2, preparation method of the present invention adopts rapid loading synthesis technique, and technological process is simple, is easy to control and realize suitability for industrialized production; And do not heat in production process, at room temperature react, energy-conserving and environment-protective.
Embodiment
Below by way of embodiment, technical scheme of the present invention is further detailed and is described.
Embodiment 1
With parts by weight, by 200 parts of CH
2=CH (CH
3) CH
2cH
2o (CH
2cH
2o)
70cH
2cH
3cHO H, 5 parts of vinylformic acid, 2 parts of diallyldimethylammonium chlorides, 2 parts of N hydroxymethyl acrylamides, 0.2 part of Mohr's salt and 200 parts of deionized waters add in reactor and stir; 20 parts of vinylformic acid, 0.9 part of 2 mercapto ethanol, 0.44 part of L-AA and 30 parts of deionized waters mix and are made into mixing solutions.Control reacting initial temperature be 12 DEG C, toward reactor is disposable add 0.25 part of hydrogen peroxide after, start to drip mixing solutions, and dropwised in 45 minutes; Continue at 35 ~ 45 DEG C of insulations 30 minutes after reaction terminates, material is transferred in storage tank, and naturally cools to room temperature; Material add place 12h in storage tank after 20 parts of mass concentrations be 30% sodium hydroxide solution carry out in and, namely obtain described high-early strength type polycarboxylic acids dehydragent.
Embodiment 2
With parts by weight, by 200 parts of CH
2=CH (CH
3) CH
2cH
2o (CH
2cH
2o)
110(CH
2cH
3cHO)
10h, 8 parts of vinylformic acid, 1 part of dimethyl diallyl brometo de amonio, 3 parts of 2-methyl propane sulfonic acid acrylamides, 0.4 part of Mohr's salt and 200 parts of deionized waters add in reactor and stir; 5 parts of vinylformic acid, 0.9 part of 2-Thiovanic acid, 0.8 part of L-AA and 30 parts of deionized waters mix and are made into mixing solutions.Control reacting initial temperature be 30 DEG C, toward reactor is disposable add 0.8 part of t-butyl hydroperoxide after, start to drip mixing solutions, and dropwised in 30 minutes; Continue at 35 ~ 45 DEG C of insulations 30 minutes after reaction terminates, material is transferred in storage tank, and naturally cools to room temperature; Material add place 18h in storage tank after 12 parts of mass concentrations be 30% sodium hydroxide solution carry out in and, namely obtain described high-early strength type polycarboxylic acids dehydragent.
Embodiment 3
With parts by weight, by 200 parts of CH
2=CH (CH
3) CH
2cH
2o (CH
2cH
2o)
90(CH
2cH
3cHO)
2h, 10 parts of vinylformic acid, 5 parts of allyl group trimethyl ammonium chlorides, 3 parts of N,N methylene bis acrylamides, 0.5 part of Mohr's salt and 200 parts of deionized waters add in reactor and stir; 12 parts of vinylformic acid, 0.5 part of 3-mercaprol, 0.2 part of L-AA and 30 parts of deionized waters mix and are made into mixing solutions.Control reacting initial temperature be 18 DEG C, toward reactor is disposable add 4 parts of hydrogen phosphide cumenes after, start to drip mixing solutions, and dropwised in 30 minutes; Continue at 35 ~ 45 DEG C of insulations 30 minutes after reaction terminates, material is transferred in storage tank, and naturally cools to room temperature; Material add place 20h in storage tank after 18 parts of mass concentrations be 30% sodium hydroxide solution carry out in and, namely obtain described high-early strength type polycarboxylic acids dehydragent.
Embodiment 4
With parts by weight, by 200 parts of CH
2=CH (CH
3) CH
2cH
2o (CH
2cH
2o)
85(CH
2cH
3cHO)
6h, 6 parts of vinylformic acid, 3 parts of allyl group trimethylammonium bromides, 1 part of 2-methyl propane sulfonic acid acrylamide, 0.1 part of Mohr's salt and 200 parts of deionized waters add in reactor and stir; 10 parts of vinylformic acid, 1.5 parts of 3-thiohydracrylic acids, 0.62 part of L-AA and 30 parts of deionized waters mix and are made into mixing solutions.Control reacting initial temperature be 23 DEG C, toward reactor is disposable add 3.2 parts of di-isopropylbenzene hydroperoxides after, start to drip mixing solutions, and dropwised in 45 minutes; Continue at 35 ~ 45 DEG C of insulations 30 minutes after reaction terminates, material is transferred in storage tank, and naturally cools to room temperature; Material add place 24h in storage tank after 14 parts of mass concentrations be 30% sodium hydroxide solution carry out in and, namely obtain described high-early strength type polycarboxylic acids dehydragent.
Embodiment 5
The product of embodiment 1 ~ 4 gained is adopted China Resources cement P.O 42.5R, and flyash is II grade of ash, and sand is the river sand of fineness modulus 2.8, and stone is particle diameter 5-20 continuous grading rubble.According to GB 8076-2008 " concrete admixture ", survey its slump, each age strength of concrete and concrete initial condensation time.Initial slump controls at 210 ± 10mm, and concrete mix is: cement 330kg/m
3, flyash 70kg/m
3, breeze 40kg/m
3, sand 700kg/m
3, stone 1130kg/m
3, admixture dosage is about 0.18% (being converted into solid part) of glue material amount.Acquired results is as shown in table 1.
Table 1 embodiment performance comparison
From table 1 test result, high-early strength type polycarboxylic acids dehydragent of the present invention has higher water-reducing property and significant short solidifying and early stage reinforced effects.Compared with blank sample, initial set and final setting time obviously shorter than blank sample, 12 hours ultimate compression strength more than the early anti pressured intension of 15MPa, 1d and 3d apparently higher than blank sample, and later strength increases stable, can be applicable to the use of the special concretes such as subway segment.
Those skilled in the art are known, when component of the present invention and parameter change in following ranges, still can obtain same as the previously described embodiments or close technique effect:
A kind of high-early strength type polycarboxylic acids dehydragent, be made up of the raw material of following weight part: unsaturated polyether 200 weight part, vinylformic acid 10 ~ 30 weight part, amide derivatives 1 ~ 3 weight part, Mohr's salt 0.1 ~ 0.5 weight part, chain-transfer agent 0.5 ~ 1.5 weight part, L-AA 0.2 ~ 0.8 weight part, oxygenant 0.8 ~ 4 weight part, deionized water 230 weight part and 30% sodium hydroxide solution 12 ~ 20 weight part, wherein
The molecular formula of unsaturated polyether is CH
2=CH (CH
3) CH
2cH
2o (CH
2cH
2o)
m(CH
2cH
3cHO)
nh, wherein, m is the integer of 70 ~ 110, and n is the integer of 1 ~ 10, and 70≤m+n≤120;
Quaternary ammonium salt is diallyldimethylammonium chloride, dimethyl diallyl brometo de amonio, allyl group trimethyl ammonium chloride or allyl group trimethylammonium bromide;
Amide derivatives is N hydroxymethyl acrylamide, 2-methyl propane sulfonic acid acrylamide or N,N methylene bis acrylamide.
Described chain-transfer agent is 2 mercapto ethanol, 2-Thiovanic acid, 3-mercaprol or 3-thiohydracrylic acid.
Described oxygenant is hydrogen peroxide, t-butyl hydroperoxide, hydrogen phosphide cumene or di-isopropylbenzene hydroperoxide.
A preparation method for above-mentioned high-early strength type polycarboxylic acids dehydragent, comprises the steps:
(1) unsaturated polyether, 5 ~ 10 parts by weight of acrylic acid, quaternary ammonium salt, amide derivatives, Mohr's salt and 200 parts by weight of deionized water are stirred;
(2) remaining vinylformic acid, chain-transfer agent, L-AA and remaining deionized water are mixed, obtain mixing solutions;
(3) controlling reacting initial temperature is 10 ~ 30 DEG C, in the material of step (1) disposable add oxygenant after, open the mixing solutions dripping step (2) wherein, dropwise in 30 ~ 45min, after dripping, continue at 35 ~ 45 DEG C of insulation reaction 30 ~ 40min;
(4) place 12 ~ 24h after material obtained for step (3) being cooled to room temperature, then add 30% sodium hydroxide solution wherein and neutralize, obtain described high-early strength type polycarboxylic acids dehydragent.
The above, be only preferred embodiment of the present invention, therefore can not limit scope of the invention process according to this, the equivalence change namely done according to the scope of the claims of the present invention and description with modify, all should still belong in scope that the present invention contains.
Claims (4)
1. a high-early strength type polycarboxylic acids dehydragent, it is characterized in that: be made up of the raw material of following weight part: unsaturated polyether 200 weight part, vinylformic acid 10 ~ 30 weight part, amide derivatives 1 ~ 3 weight part, Mohr's salt 0.1 ~ 0.5 weight part, chain-transfer agent 0.5 ~ 1.5 weight part, L-AA 0.2 ~ 0.8 weight part, oxygenant 0.8 ~ 4 weight part, deionized water 230 weight part and 30% sodium hydroxide solution 12 ~ 20 weight part, wherein
The molecular formula of unsaturated polyether is CH
2=CH (CH
3) CH
2cH
2o (CH
2cH
2o)
m(CH
2cH
3cHO)
nh, wherein, m is the integer of 70 ~ 110, and n is the integer of 1 ~ 10, and 70≤m+n≤120;
Quaternary ammonium salt is diallyldimethylammonium chloride, dimethyl diallyl brometo de amonio, allyl group trimethyl ammonium chloride or allyl group trimethylammonium bromide;
Amide derivatives is N hydroxymethyl acrylamide, 2-methyl propane sulfonic acid acrylamide or N,N methylene bis acrylamide.
2. a kind of high-early strength type polycarboxylic acids dehydragent as claimed in claim 1, is characterized in that: described chain-transfer agent is 2 mercapto ethanol, 2-Thiovanic acid, 3-mercaprol or 3-thiohydracrylic acid.
3. a kind of high-early strength type polycarboxylic acids dehydragent as claimed in claim 1, is characterized in that: described oxygenant is hydrogen peroxide, t-butyl hydroperoxide, hydrogen phosphide cumene or di-isopropylbenzene hydroperoxide.
4. a preparation method for the high-early strength type polycarboxylic acids dehydragent in claims 1 to 3 described in arbitrary claim, is characterized in that: comprise the steps:
(1) unsaturated polyether, 5 ~ 10 parts by weight of acrylic acid, quaternary ammonium salt, amide derivatives, Mohr's salt and 200 parts by weight of deionized water are stirred;
(2) remaining vinylformic acid, chain-transfer agent, L-AA and remaining deionized water are mixed, obtain mixing solutions;
(3) controlling reacting initial temperature is 10 ~ 30 DEG C, in the material of step (1) disposable add oxygenant after, open the mixing solutions dripping step (2) wherein, dropwise in 30 ~ 45min, after dripping, continue at 35 ~ 45 DEG C of insulation reaction 30 ~ 40min;
(4) place 12 ~ 24h after material obtained for step (3) being cooled to room temperature, then add 30% sodium hydroxide solution wherein and neutralize, obtain described high-early strength type polycarboxylic acids dehydragent.
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Application publication date: 20151104 |