CN103011669A - Early-strength polycarboxylate superplasticizer and preparation method thereof - Google Patents
Early-strength polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an early-strength polycarboxylate superplasticizer, which is prepared through aqueous solution polymerization on 75-90% of monomer A, 0.5-2.0% of monomer B, 0.8-3.2% of monomer C, 5-20% of monomer D and 1-3.5% of monomer E under action of an oxidation-reduction system. A preparation method comprises the following steps: 1) putting the monomer A, the monomer B and the monomer E into a reaction kettle, heating to 30 DEG C, stirring to uniformly dissolve into water, heating to 50 DEG C and adding an oxidant; 2) respectively dripping a mixed aqueous solution of the monomer C and the monomer D and a mixed aqueous solution of a reductant and a chain transfer agent, dripping off within 2-4 hours at the same time, maintaining the temperature at 50 DEG C, and further stirring for 1 hour; and 3) cooling to room temperature, adding water and liquid alkali, and regulating pH to 5-6.5 and the solid content to about 40%. The early-strength polycarboxylate superplasticizer has significant early strength enhancing performance, and the middle strength and the later strength thereof are stably improved; and the preparation method is easy to operate, short in production cycle and low in cost.
Description
Technical field
The invention belongs to the technical field of concrete additives in the material of construction, be specifically related to a kind of early strength type polycarboxylic acid series high-performance dehydragent, particularly the preparation method of this kind water reducer.
Background technology
The water reducers such as poly carboxylic acid series water reducer with traditional naphthalene is, melamine series are compared owing to having the advantages such as volume is low, water-reducing rate is high, cement adaptability is good, become gradually research and widely used water reducer of new generation.Along with rise, the especially planning implementation of state-owned railroads Line for Passenger Transportation net engineering of the Large Infrastructure Projects such as China's nuclear power, water conservancy, bridge, tunnel, to the market requirement sustainable growth of poly carboxylic acid series water reducer.Common poly carboxylic acid series water reducer has certain delayed coagulation at present, the early strength slower development, concrete 1d ultimate compression strength only can reach 20 ~ 30% of design strength, especially in the situation that low temperature or use large volume mineral admixture, early strength is lower, has greatly limited its range of application.
In order to improve concrete early strength, accelerate the template turnover, accelerating construction progress, present general employing reduces water-binder ratio, improves cement mark or the technological approaches such as cement consumption and interpolation hardening accelerator.When adopting inorganic salt or organic hardening accelerator and poly carboxylic acid series water reducer to carry out physical compounding, the phenomenons such as layering, flatulence, package stability be poor occuring easily not only, and can reduce the water-reducing property of poly carboxylic acid series water reducer.Vitriol in the inorganic salt can improve alkali content greatly, cause potential alkali-aggregate reaction harm, and vitriol has negative impact to late strength of concrete; Villaumite is limited to use owing to easily causing steel bar corrosion; Potent fruit morning when alcamines hardening accelerator list is mixed in the organism is not too obvious, and is expensive and volume is wayward.
Summary of the invention
The present invention is directed to the in early days deficiency of intensity aspect of existing poly carboxylic acid series water reducer, by master, side-chain radical equimolecular structure design, introduce new polymerization single polymerization monomer, provide that a kind of water-reducing rate is high, time of coagulation is short, early by force effective, stable performance, the simple early strength type polycarboxylic acid series high-performance dehydragent of preparation technology and preparation technology thereof.During especially for precast concrete, can significantly improve early age strength of concrete, thereby reduction precast concrete production energy consumption is enhanced productivity in the ahead of time demoulding.
The present invention relates to a kind of early strength type polycarboxylic acid series high-performance dehydragent, this water reducer is to carry out aqueous solution polymerization by following monomer under the oxidation-reduction system effect to form:
1) monomer A is the methacrylic Soxylat A 25-7, and molecular weight is that 3000 ~ 5000(is M
W=3000 ~ 5000), monomer A accounts for 75 ~ 90% of total reactant solid weight;
2) monomers B is lauryl alcohol, and monomers B accounts for 0.5 ~ 2.0% of total reactant solid weight;
3) structural formula of monomer C is as follows:
Wherein, R
1, R
2, R
3, R
4Independently represent H or hydroxyethyl or hydroxypropyl respectively, but R
1, R
2, R
3, R
4Can not be H simultaneously; Monomer C accounts for 0.8 ~ 3.2% of total reactant solid weight;
4) monomer D is acrylic or methacrylic acid, and monomer D accounts for 5 ~ 20% of total reactant solid weight;
5) monomer E is the unsaturated sulfonic acid salt monomer, comprises one or more the mixture in allylsulfonate, methallylsulfonic acid salt, the styrene sulfonate etc., and monomer E accounts for 1 ~ 3.5% of total reactant solid weight.
The preparation method of described early strength type polycarboxylic acid series high-performance dehydragent may further comprise the steps:
1) monomer A, monomers B and monomer E are dropped into reactor, be warming up to 30 ℃ and stir so that it all is dissolved in the water, be warming up to 50 ℃ and add oxygenant;
2) drip respectively the mixed aqueous solution of monomer C and monomer D and the mixed aqueous solution of reductive agent and chain-transfer agent, in 2 ~ 4h, drip off simultaneously, remain on 50 ℃ after adding and continue to stir 1h;
3) be down to room temperature and add entry and liquid caustic soda, regulating the pH value is 5 ~ 6.5, and solid content is about 40%.
Described oxygenant is hydrogen peroxide or tertbutyl peroxide, and its consumption is 0.5 ~ 2.2% of reaction monomers gross weight, and described reductive agent is xitix, and its consumption is 0.1 ~ 0.6% of reaction monomers gross weight.
Described chain-transfer agent is mercaptoethanol, Thiovanic acid or 3-thiohydracrylic acid, and consumption is 0.3 ~ 1.5% of reaction monomers gross weight.
Described monomer C is selected from the mixture of one or more arbitrary proportions in dihydroxy ethyl quadrol, dihydroxypropyl quadrol, tetrahydroxyethyl-ethylene diamine or the tetrahydroxypropyl ethylenediamine.
Beneficial effect of the present invention: the present invention has that water-reducing rate is high, time of coagulation is short, concrete 's air-containing is low, the early strength advantages of higher, when being used for precast concrete, can significantly improve early age strength of concrete, thus the ahead of time demoulding, enhance productivity, reduce the precast concrete production energy consumption.
Embodiment
Below describe embodiments of the present invention in detail with specific embodiment, how the utilisation technology means solve technical problem to the present invention whereby, and the implementation procedure of reaching technique effect can fully understand and implements according to this.
Embodiment 1.
In reactor, add 310 parts of methacrylic Soxylat A 25-7 (M
W=3000), 4.8 parts of lauryl alcohols and 8 parts of methylpropene sodium sulfonates, and add 220 parts of water, be warming up to 30 ℃ and stir so that it all is dissolved in the water, be warming up to 50 ℃ and add 5.2 parts of tertiary butyl hydrogen peroxide and stir; Drip simultaneously the mixed aqueous solution that is made into by 7.8 parts of dihydroxy ethyl quadrols, 48 parts of methacrylic acids and 120 parts of water and by 1.2 parts of xitix, 3.2 parts of 3-thiohydracrylic acids and 100 parts of mixed aqueous solutions that water is made into, dropwise in the 3.5h; Remain on 50 ℃ after adding and continue to stir 1h; Be down to add 42 parts of liquid caustic soda after the room temperature and add 120 parts in water and stir and get final product.
Embodiment 2.
In reactor, add 344 parts of methacrylic Soxylat A 25-7 (M
W=5000), 3 parts of lauryl alcohols and 6.2 parts of sodium allyl sulfonates, and add 220 parts of water, be warming up to 30 ℃ and stir so that it all is dissolved in the water, be warming up to 50 ℃ and add 4.5 parts of hydrogen peroxide and stir; Drip simultaneously the mixed aqueous solution that is made into by 6.4 parts of tetrahydroxyethyl-ethylene diamines, 23 parts of vinylformic acid and 120 parts of water and by 1.8 parts of xitix, 2.4 parts of Thiovanic acids and 100 parts of mixed aqueous solutions that water is made into, dropwise in the 3.5h; Remain on 50 ℃ after adding and continue to stir 1h; Be down to add 32 parts of liquid caustic soda after the room temperature and add 140 parts in water and stir and get final product.
Embodiment 3.
In reactor, add 330 parts of methacrylic Soxylat A 25-7 (M
W=5000), 6 parts of lauryl alcohols and 6 parts of sodium allyl sulfonates, and add 220 parts of water, be warming up to 30 ℃ and stir so that it all is dissolved in the water, be warming up to 50 ℃ and add 4.4 parts of hydrogen peroxide and stir; Drip simultaneously the mixed aqueous solution that is made into by 7 parts of dihydroxypropyl quadrols, 28 parts of vinylformic acid and 120 parts of water and by 2.2 parts of xitix, 3 parts of mercaptoethanols and 100 parts of mixed aqueous solutions that water is made into, dropwise in the 3.5h; Remain on 50 ℃ after adding and continue to stir 1h; Be down to add 45 parts of liquid caustic soda after the room temperature and add 125 parts in water and stir and get final product.
Embodiment 4.
In reactor, add 320 parts of methacrylic Soxylat A 25-7 (M
W=4000), 4.5 parts of lauryl alcohols and 8.6 parts of phenylallene sodium sulfonates, and add 220 parts of water, be warming up to 30 ℃ and stir so that it all is dissolved in the water, be warming up to 50 ℃ and add 5.5 parts of tertiary butyl hydrogen peroxide and stir; Drip simultaneously the mixed aqueous solution that is made into by 5 parts of tetrahydroxyethyl-ethylene diamines, 38 parts of methacrylic acids and 120 parts of water and by 2 parts of xitix, 4.6 parts of 3-thiohydracrylic acids and 100 parts of mixed aqueous solutions that water is made into, dropwise in the 3.5h; Remain on 50 ℃ after adding and continue to stir 1h; Be down to add 40 parts of liquid caustic soda after the room temperature and add 130 parts in water and stir and get final product.
Comparative Examples 1.
In reactor, add 342 parts of methacrylic Soxylat A 25-7 (M
W=3000), 220 parts of water, constantly stir so that it all is dissolved in the water, be warming up to 60 ℃ and add 3.2 parts of ferric sulfate and stir; Drip simultaneously the mixed aqueous solution that is made into by 0.7 part of Thiovanic acid, 1.2 parts of xitix and 120 parts of water and by 38 parts of vinylformic acid and 100 parts of mixed aqueous solutions that water is made into, dropwise in the 3.5h, remain on 60 ℃ after adding and continue to stir 1h; Be down to add 50 parts of liquid caustic soda after the room temperature and add 125 parts in water and stir and get final product.
Comparative Examples 2.
In reactor, add 330 parts of methacrylic Soxylat A 25-7 (M
W=2400), 6 parts of methylpropene sodium sulfonates and 220 parts of water, be warming up to 60 ℃ and stir so that it all is dissolved in the water, add 4.2 parts of hydrogen peroxide and stir; Drip simultaneously the mixed aqueous solution that is made into by 42 parts of vinylformic acid and 100 parts of water and by 2.2 parts of xitix, 3.6 parts of mercaptoethanols and 120 parts of mixed aqueous solutions that water is made into, dropwise in the 3.5h; Remain on 60 ℃ after adding and continue to stir 1h; Be down to add 132 parts in water after the room temperature and add 40 parts of liquid caustic soda and stir and get final product.
Application Example 1.
With reference to standard GB/T 8076-2008 " concrete admixture " relevant regulations, estimate concrete water-reducing rate, time of coagulation and the different age strength of mixing early strength type polycarboxylic acid series high-performance dehydragent of the present invention.Peaceful sheep P.II 52.5 cement of gold are adopted in test, fineness modulus is 2.7 medium sand, the rubble of 5 ~ 20mm continuous grading, concrete mix is C:S:G=360:842:1028, it is 210mm ± 10mm that the adjustment water consumption makes the initial slump of fresh concrete, and the volume of water reducer is that the 0.2%(folding of cement weight is solid).Test-results sees the following form 1.
Table 1 is mixed concrete performance of the present invention
By table 1 result as seen, early strength type polycarboxylic acid series high-performance dehydragent of the present invention has the advantages that water-reducing rate is high, concrete 's air-containing is low, time of coagulation is short, mix concrete 1d ultimate compression strength of the present invention and be improved significantly, and 28d ultimate compression strength is had no adverse effects.
Application Example 2.
Compared early strength type polycarboxylic acid series high-performance dehydragent of the present invention, comparative example poly carboxylic acid series water reducer and commercially available poly carboxylic acid series water reducer PCA(standard type) and the PCE(early-strength type) application performance in the non-evaporating curing concrete pile tube of C80.Peaceful sheep P.II 52.5 cement of gold are adopted in test, and fineness modulus is 2.7 medium sand, and the rubble of 5 ~ 20mm continuous grading, concrete mix are C:S:G:W=530:554:1231:135; The concrete pouring system is: the quiet 2h that stops after the moulding, and band mould atmospheric steam curing 6h, 3h is down to room temperature, the results are shown in Table 2.
The non-evaporating curing concrete early strength of table 2 C80
By table 2 result as seen, adopt concrete of the present invention exempting to press the strength grade that can satisfy C80 in the steaming situation, epistasis morning of early strength type polycarboxylic acid series high-performance dehydragent of the present invention can obviously be better than Comparative Examples and commercially available common poly carboxylic acid series water reducer, also be better than commercially available early strength type polycarboxylic acid series high-performance dehydragent, thereby can improve throughput, reduction production energy consumption.
Early strength type polycarboxylic acid series high-performance dehydragent of the present invention has outstanding water-reducing property, especially has to strengthen the property by force significant morning, and middle and later periods intensity stabilization growth, be conducive to accelerate the template turnover, accelerating construction progress.Preparation process of the present invention has the advantages such as simple to operate, with short production cycle, with low cost in addition, is fit to suitability for industrialized production.
Although the present invention is described by embodiment, embodiment limits the present invention.Those skilled in the art can make various distortion and improvement in the scope of spirit of the present invention, for example adjustment of component proportions or time range, and the effect after this adjustment is predictable, so it is equally within protection scope of the present invention.Ratio in the application form is the ratio between the monomer, and the monomer of namely considering emphatically accounts for the ratio of total reactant solid, and that water is just regulated solid content is used.Therefore protection scope of the present invention should be as the criterion by the protection domain that technical characterictic was defined identical with the application's claim or that be equal to.
Claims (5)
1. an early strength type polycarboxylic acid series high-performance dehydragent is characterized in that, this water reducer is to carry out aqueous solution polymerization by following monomer under the oxidation-reduction system effect to form:
1) monomer A is the methacrylic Soxylat A 25-7, and molecular weight is 3000 ~ 5000, and monomer A accounts for 75 ~ 90% of total reactant solid weight;
2) monomers B is lauryl alcohol, and monomers B accounts for 0.5 ~ 2.0% of total reactant solid weight;
3) structural formula of monomer C is as follows:
Wherein, R
1, R
2, R
3, R
4Independently represent H, hydroxyethyl or hydroxypropyl respectively, but R
1, R
2, R
3, R
4Can not be H simultaneously; Monomer C accounts for 0.8 ~ 3.2% of total reactant solid weight;
4) monomer D is acrylic or methacrylic acid, and monomer D accounts for 5 ~ 20% of total reactant weight;
5) monomer E is the unsaturated sulfonic acid salt monomer, comprises one or more the mixture in allylsulfonate, methallylsulfonic acid salt, the styrene sulfonate etc., and monomer E accounts for 1 ~ 3.5% of total reactant solid weight.
2. early strength type polycarboxylic acid series high-performance dehydragent according to claim 1, it is characterized in that: described monomer C is selected from the mixture of one or more arbitrary proportions in dihydroxy ethyl quadrol, dihydroxypropyl quadrol, tetrahydroxyethyl-ethylene diamine or the tetrahydroxypropyl ethylenediamine.
3. the preparation method of a claim 1 or 2 described early strength type polycarboxylic acid series high-performance dehydragents is characterized in that: may further comprise the steps:
1) monomer A, monomers B and monomer E are dropped into reactor, be warming up to 30 ℃ and stir so that it all is dissolved in the water, be warming up to 50 ℃ and add oxygenant;
2) drip respectively the mixed aqueous solution of monomer C and monomer D and the mixed aqueous solution of reductive agent and chain-transfer agent, in 2 ~ 4h, drip off simultaneously, remain on 50 ℃ after adding and continue to stir 1h;
3) be down to room temperature and add entry and liquid caustic soda, regulating the pH value is 5 ~ 6.5, and solid content is about 40%.
4. early strength type polycarboxylic acid series high-performance dehydragent preparation method according to claim 3, it is characterized in that: described oxygenant is hydrogen peroxide or tertbutyl peroxide, its consumption is 0.5 ~ 2.2% of reaction monomers gross weight; Described reductive agent is xitix, and its consumption is 0.1 ~ 0.6% of reaction monomers gross weight.
5. early strength type polycarboxylic acid series high-performance dehydragent preparation method according to claim 3, it is characterized in that: described chain-transfer agent is mercaptoethanol, Thiovanic acid or 3-thiohydracrylic acid, and consumption is 0.3 ~ 1.5% of reaction monomers gross weight.
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| CN104261720A (en) * | 2014-09-22 | 2015-01-07 | 厦门天润锦龙建材有限公司 | Ether polycarboxylate superplasticizer and preparation method thereof |
| CN104861122A (en) * | 2015-04-22 | 2015-08-26 | 厦门路桥翔通建材科技有限公司 | Heat-source-free early strength polycarboxylate water reducer and preparation method thereof |
| CN105218757A (en) * | 2015-09-17 | 2016-01-06 | 深圳市迈地砼外加剂有限公司 | There is Early-strength polycarboxylate superplasticizer of protecting function of collapsing and preparation method thereof |
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| CN105271903A (en) * | 2015-10-22 | 2016-01-27 | 岳阳东方雨虹防水技术有限责任公司 | Polycarboxylate superplasticizer with super high early strength and preparation method of polycarboxylate superplasticizer |
| CN105461914A (en) * | 2014-08-15 | 2016-04-06 | 辽宁奥克化学股份有限公司 | Methyl allyl polyoxyethylene ether and preparation method and application thereof |
| CN105731863A (en) * | 2014-12-09 | 2016-07-06 | 上海东大化学有限公司 | Viscosity-lowering type polycarboxylic acid water reducing agent and preparation and use methods therefor |
| CN106007452A (en) * | 2016-05-17 | 2016-10-12 | 福建建工建材科技开发有限公司 | Preparation method of early strength type high-performance polycarboxylic acid water reducing agent |
| CN109337022A (en) * | 2018-08-25 | 2019-02-15 | 太和县鑫泰高科新型建筑材料有限公司 | A kind of high performance water reducing agent of polyocarboxy acid |
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| CN105461914A (en) * | 2014-08-15 | 2016-04-06 | 辽宁奥克化学股份有限公司 | Methyl allyl polyoxyethylene ether and preparation method and application thereof |
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| CN105731863B (en) * | 2014-12-09 | 2018-01-30 | 上海东大化学有限公司 | Glutinous type poly carboxylic acid series water reducer of one kind drop and preparation method thereof and application method |
| CN105731863A (en) * | 2014-12-09 | 2016-07-06 | 上海东大化学有限公司 | Viscosity-lowering type polycarboxylic acid water reducing agent and preparation and use methods therefor |
| CN104861122A (en) * | 2015-04-22 | 2015-08-26 | 厦门路桥翔通建材科技有限公司 | Heat-source-free early strength polycarboxylate water reducer and preparation method thereof |
| CN105218757A (en) * | 2015-09-17 | 2016-01-06 | 深圳市迈地砼外加剂有限公司 | There is Early-strength polycarboxylate superplasticizer of protecting function of collapsing and preparation method thereof |
| CN105218757B (en) * | 2015-09-17 | 2020-07-14 | 深圳市迈地砼外加剂有限公司 | Early-strength polycarboxylate superplasticizer with slump retaining function and preparation method thereof |
| CN105271903A (en) * | 2015-10-22 | 2016-01-27 | 岳阳东方雨虹防水技术有限责任公司 | Polycarboxylate superplasticizer with super high early strength and preparation method of polycarboxylate superplasticizer |
| CN105271903B (en) * | 2015-10-22 | 2017-08-25 | 岳阳东方雨虹防水技术有限责任公司 | A kind of ultra high early strength poly-carboxylic water reducer and preparation method thereof |
| CN105273180A (en) * | 2015-11-03 | 2016-01-27 | 上海台界化工有限公司 | Synthesis method of unsaturated polyoxyethylene ether derivative and product of unsaturated polyoxyethylene ether derivative |
| CN105273180B (en) * | 2015-11-03 | 2018-03-13 | 上海台界化工有限公司 | A kind of synthetic method of unsaturated polyoxyethylene ether derivant and products thereof |
| CN106007452A (en) * | 2016-05-17 | 2016-10-12 | 福建建工建材科技开发有限公司 | Preparation method of early strength type high-performance polycarboxylic acid water reducing agent |
| CN106007452B (en) * | 2016-05-17 | 2018-05-04 | 福建建工建材科技开发有限公司 | A kind of preparation method of early strength polycarboxylic acid high performance dehydragent |
| CN109337022A (en) * | 2018-08-25 | 2019-02-15 | 太和县鑫泰高科新型建筑材料有限公司 | A kind of high performance water reducing agent of polyocarboxy acid |
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