CN103539903A - Preparation method of powder polycarboxylate superplasticizer with air drafting and defoaming functions - Google Patents
Preparation method of powder polycarboxylate superplasticizer with air drafting and defoaming functions Download PDFInfo
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- CN103539903A CN103539903A CN201310447766.XA CN201310447766A CN103539903A CN 103539903 A CN103539903 A CN 103539903A CN 201310447766 A CN201310447766 A CN 201310447766A CN 103539903 A CN103539903 A CN 103539903A
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Abstract
The invention discloses a preparation method of a powder polycarboxylate superplasticizer with air drafting and defoaming functions. The method comprises an esterification technology and a polymerization technology and specifically comprises the following steps of adding methoxy polyethylene glycol, methacrylic acid, a monomer with an air drafting function, a monomer solution with a defoaming function, a catalyst and a polymerization inhibitor solution to an experimental device, so as to prepare a large monomer; adding a certain amount of drinking water to the experimental device, heating to polymerization temperature of 70-90 DEG C; successively adding the large monomer, a chain transfer agent solution and an initiator solution; neutralizing by sodium hydroxide solution with certain concentration, and adjusting the pH value to 6-8, so as to obtain the polycarboxylate superplasticizer with the air drafting and defoaming functions. The monomer with the air drafting function and the monomer with the defoaming function are grafted on the polycarboxylate superplasticizer by a chemical method, so that the situation of quality instability caused by physical mixing of the powder polycarboxylate superplasticizer is solved.
Description
Technical field
The present invention relates to the preparation method of the powder polycarboxylic acids water reducing agent that a kind of dry-mix uses, specifically a kind of preparation method with the powder polycarboxylic acids water reducing agent of bleed, their defoaming function.
Background technology
Powder polycarboxylic acids water reducing agent is applied in dry-mix, after adding water and stirring, can form a kind of fluid of high-consistency, if but water reducer amount of air entrainment is low, and mortar workability is poor, and contrary amount of air entrainment is high, and mortar strength is on the low side.Therefore,, when producing powder polycarboxylic acids water reducing agent, except water-reducing rate, also need to consider its application performance, i.e. the construction workability of dry-mix.The common solution of this problem has at present:
1) add dry powder air entrapment agent, dry powder defoamer and powder polycarboxylic acids water reducing agent to be uniformly mixed, be then packaged into product.Because the dry powder air entrapment agent of mixing outward, dry powder defoamer consumption are low, cause mixing time long and mix inhomogeneously, affect the stability of quality product;
2) add liquor defoamer, liquor air entrapment agent to go spraying dry together with liquid polycarboxylate water-reducer, be then packaged into product.Because liquor defoamer, liquor air entrapment agent and liquid polycarboxylate water-reducer exist the poor problem of consistency, cause equally unstable product quality.
Summary of the invention
The problem existing for above-mentioned prior art, the invention provides a kind of preparation method with the powder polycarboxylic acids water reducing agent of bleed, their defoaming function, pass through chemical process, on polycarboxylate water-reducer molecule, grafting has the monomer and the monomer with their defoaming function of air-entraining function, has solved physical mixed and has caused the unsettled situation of quality.
To achieve these goals, the technical solution used in the present invention is:
Comprise esterification technique and polymerization technique.Described esterification technique is: by add the monomer of poly glycol monomethyl ether 2000, methacrylic acid, air-entraining function, the monomer of their defoaming function in experimental installation, stopper tosic acid, catalyzer Resorcinol, esterification temperature is 110 ~ 130 ℃, vacuum tightness is-0.07 ~-0.09MPa, 6 ~ 8 hours reaction times, be cooled to 50 ~ 70 ℃ of dischargings, can obtain large monomer; Described polymerization technique flow process is: by add a certain amount of soft water in experimental installation, be heated to 70 ~ 90 ℃ of polymerization temperatures, successively add large monomer, chain-transfer agent Thiovanic acid solution and initiator ammonium persulfate solution, in 2 ~ 4h, drip off, insulation 1 ~ 3h, is then cooled to 40 ~ 60 ℃, with certain density sodium hydroxide solution, neutralizes, regulating pH value is between 6 ~ 8, can obtain having the polycarboxylate water-reducer of bleed, their defoaming function; Described air-entraining function monomer is polyoxyethylene glycol, and their defoaming function monomer is carbon atoms at 7 ~ 16 alkyl alcohol.
Further, described esterification technique raw material is air-entraining function monomer 2 ~ 4% by weight ratio, their defoaming function monomer 2 ~ 4%, and poly glycol monomethyl ether 2000 accounts for 65 ~ 73%, methacrylic acid accounts for 16 ~ 20%, tosic acid accounts for 1 ~ 4%, Resorcinol accounts for 3 ~ 6%.
Further, the raw material of described polymerization technique by weight ratio: soft water accounts for 54 ~ 60%, and large monomer accounts for 36 ~ 43%, and Thiovanic acid accounts for 0.1 ~ 0.8%, and ammonium persulphate accounts for 0.1 ~ 0.8%, and sodium hydroxide accounts for 2 ~ 2.5%.
Further, described polyoxyethylene glycol, molecular weight is 200 ~ 600, the carbon atoms of described alkyl alcohol is 7 ~ 16.
The invention has the beneficial effects as follows, by chemical process, on polycarboxylate water-reducer molecule, grafting has the monomer of air-entraining function and has the monomer of their defoaming function, has solved the situation that physical mixed causes unstable product quality.
Embodiment
Embodiment has more at large described the powder polycarboxylic acids water reducing agent preparation method with bleed, their defoaming function produced according to the present invention below, comprises esterification technique and polymerization technique.
embodiment 1
Esterification formula: add 4% Macrogol 200 in the there-necked flask that thermometer, oil bath pan, speed governing agitator, vacuum unit are housed, butanols 4%, 65% poly glycol monomethyl ether 2000, methacrylic acid 20%, tosic acid 1%, Resorcinol 6%, at 110 ~ 130 ℃, vacuum tightness, under-0.07 ~-0.09MPa, react 6 ~ 8 hours, then be cooled to 50 ~ 70 ℃ of dischargings, obtain required carboxylate.
Polymerization formula: thermometer is being housed, speed governing agitator, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, add 21.8% soft water, then stirring heating in water bath are to 70 ~ 90 ℃ of temperature, under this temperature, with 1 ~ 3h, evenly drip the mixed liquid (carboxylate 43% of above-mentioned preparation, 0.1% Thiovanic acid, the mixed solution that 10% soft water forms), when dripping mixed liquid, drip initiator solution (0.1% ammonium persulphate, the mixed solution that 18% soft water forms), 2 ~ 4h drips off, after dripping off, initiator solution is incubated 1 ~ 3h, then be cooled to 40 ~ 60 ℃, add sodium hydroxide solution (2% sodium hydroxide, the mixed solution that 5% soft water forms), obtain the spray-dired liquid polycarboxylate water-reducer for the treatment of of the present invention.
embodiment 2
Esterification formula: add 2% poly(oxyethylene glycol) 400 in the there-necked flask that thermometer, oil bath pan, speed governing agitator, vacuum unit are housed, octanol 2%, 73% poly glycol monomethyl ether 2000, methacrylic acid 16%, tosic acid 3%, Resorcinol 4%, at 110 ~ 130 ℃, vacuum tightness, under-0.07 ~-0.09MPa, react 6 ~ 8 hours, then be cooled to 50 ~ 70 ℃ of dischargings, obtain required carboxylate.
Polymerization formula: thermometer is being housed, speed governing agitator, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, add 21.6% soft water, then stirring heating in water bath are to 70 ~ 90 ℃ of temperature, under this temperature, with 1 ~ 3h, evenly drip the mixed liquid (carboxylate 36% of above-mentioned preparation, 0.8% Thiovanic acid, the mixed solution that 12% soft water forms), when dripping mixed liquid, drip initiator solution (0.8% ammonium persulphate, the mixed solution that 20% soft water forms), 2 ~ 4h drips off, after dripping off, initiator solution is incubated 1 ~ 3h, then be cooled to 40 ~ 60 ℃, add sodium hydroxide solution (2.5% sodium hydroxide, the mixed solution that 6.3% soft water forms), obtain the spray-dired liquid polycarboxylate water-reducer for the treatment of of the present invention.
embodiment 3
Esterification formula: add 3% Polyethylene Glycol-600 in the there-necked flask that thermometer, oil bath pan, speed governing agitator, vacuum unit are housed, dodecyl alcohol 3%, 69% poly glycol monomethyl ether 2000, methacrylic acid 19%, tosic acid 3%, Resorcinol 3%, at 110 ~ 130 ℃, vacuum tightness, under-0.07 ~-0.09MPa, react 6 ~ 8 hours, then be cooled to 50 ~ 70 ℃ of dischargings, obtain required carboxylate.
Polymerization formula: thermometer is being housed, speed governing agitator, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, add 24.6% soft water, then stirring heating in water bath are to 70 ~ 90 ℃ of temperature, under this temperature, with 1 ~ 3h, evenly drip the mixed liquid (carboxylate 37% of above-mentioned preparation, 0.5% Thiovanic acid, the mixed solution that 10% soft water forms), when dripping mixed liquid, drip initiator solution (0.4% ammonium persulphate, the mixed solution that 20% soft water forms), 2 ~ 4h drips off, after dripping off, initiator solution is incubated 1 ~ 3h, then be cooled to 40 ~ 60 ℃, add sodium hydroxide solution (2.3% sodium hydroxide, the mixed solution that 5.2% soft water forms), obtain the spray-dired liquid polycarboxylate water-reducer for the treatment of of the present invention.
reference example
Esterification formula: add 75% poly glycol monomethyl ether 2000, methacrylic acid 18%, tosic acid 3%, Resorcinol 4% in the there-necked flask that thermometer, oil bath pan, speed governing agitator, vacuum unit are housed, at 110 ~ 130 ℃, vacuum tightness, under-0.07 ~-0.09MPa, react 6 ~ 8 hours, then be cooled to 50 ~ 70 ℃ of dischargings, obtain required carboxylate.
Polymerization formula: thermometer is being housed, speed governing agitator, in the four-hole boiling flask of reflux condensing tube and Dropping feeder, add 26.6% soft water, then stirring heating in water bath are to 70 ~ 90 ℃ of temperature, under this temperature, with 1 ~ 3h, evenly drip the mixed liquid (carboxylate 37% of above-mentioned preparation, 0.30% Thiovanic acid, the mixed solution that 9% soft water forms), when dripping mixed liquid, drip initiator solution (0.1% ammonium persulphate, the mixed solution that 20% soft water forms), 2 ~ 4h drips off, after dripping off, initiator solution is incubated 1 ~ 3h, then be cooled to 40 ~ 60 ℃, add sodium hydroxide solution (2% sodium hydroxide, the mixed solution that 5% soft water forms), obtain the spray-dired liquid polycarboxylate water-reducer for the treatment of of the present invention.
applicating evaluating result
In addition, the initial flow degree of reference example is slightly better than embodiment 1, embodiment 2, embodiment 3, but two hours degree of mobilization of reference example are significantly less than embodiment 1, embodiment 2, embodiment 3, and fluidity loss is larger, and embodiment 1, embodiment 2, embodiment 3 frees of losses, and be a bit larger tham initial flow degree; Bonding strength test data are known, and reference example, due to without bleed, froth breaking group, causes mortar workability and intensity all poor.
Claims (4)
1. a preparation method with the powder polycarboxylic acids water reducing agent of bleed, their defoaming function, is characterized in that, comprises esterification technique and polymerization technique; Described esterification technique is: by add the monomer of poly glycol monomethyl ether 2000, methacrylic acid, air-entraining function, the monomer of their defoaming function in experimental installation, stopper tosic acid, catalyzer Resorcinol, esterification temperature is 110 ~ 130 ℃, vacuum tightness is--0.07 ~-0.09MPa, 6 ~ 8 hours reaction times, be cooled to 50 ~ 70 ℃ of dischargings, can obtain large monomer; Described polymerization technique flow process is: by add soft water in experimental installation, be heated to 70 ~ 90 ℃ of polymerization temperatures, successively add large monomer, chain-transfer agent Thiovanic acid solution and initiator ammonium persulfate solution, in 2 ~ 4h, drip off, insulation 1 ~ 3h, then be cooled to 40 ~ 60 ℃, with certain density sodium hydroxide solution, neutralize, regulating pH value is between 6 ~ 8; Described air-entraining function monomer is polyoxyethylene glycol, and their defoaming function monomer is carbon atoms at 7 ~ 16 alkyl alcohol.
2. a kind of preparation method with the powder polycarboxylic acids water reducing agent of bleed, their defoaming function according to claim 1, it is characterized in that, described esterification technique raw material is air-entraining function monomer 2 ~ 4% by weight ratio, their defoaming function monomer 2 ~ 4%, poly glycol monomethyl ether 2000 accounts for 65 ~ 73%, methacrylic acid accounts for 16 ~ 20%, tosic acid accounts for 1 ~ 4%, Resorcinol accounts for 3 ~ 6%.
3. a kind of preparation method with the powder polycarboxylic acids water reducing agent of bleed, their defoaming function according to claim 1, it is characterized in that, described polymerization technique raw material is by weight ratio: soft water accounts for 54 ~ 60%, large monomer accounts for 36 ~ 43%, Thiovanic acid accounts for 0.1 ~ 0.8%, ammonium persulphate accounts for 0.1 ~ 0.8%, and sodium hydroxide accounts for 2 ~ 2.5%.
4. a kind of preparation method with the powder polycarboxylic acids water reducing agent of bleed, their defoaming function according to claim 1, is characterized in that, described polyoxyethylene glycol, and molecular weight is 200 ~ 600, the carbon atoms of described alkyl alcohol is 7 ~ 16.
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Cited By (5)
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| CN104016614A (en) * | 2014-06-13 | 2014-09-03 | 石家庄市长安育才建材有限公司 | Polycarboxylate water reducer with defoaming function and preparation method of water reducer |
| CN105131200A (en) * | 2015-09-17 | 2015-12-09 | 安徽森普新型材料发展有限公司 | Preparation method of powder polycarboxylate water reducer with air-entraining and defoaming functions |
| CN106589252A (en) * | 2016-11-10 | 2017-04-26 | 厦门路桥翔通建材科技有限公司 | Low air-entraining type maleic anhydride poly carboxylic acid water reducing agent and preparation method thereof |
| CN106905493A (en) * | 2017-03-20 | 2017-06-30 | 江苏苏博特新材料股份有限公司 | A kind of froth breaking type poly-carboxylic-acid cement dispersant and preparation method thereof |
| CN112279553A (en) * | 2020-09-28 | 2021-01-29 | 浙江玖龙新材料有限公司 | Ester polycarboxylate superplasticizer formula and preparation method |
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| CN102775580A (en) * | 2012-07-27 | 2012-11-14 | 北京建筑材料科学研究总院有限公司 | Defoamer matching with polycarboxylate water reducing agent and preparation method thereof |
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Patent Citations (4)
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| US5985989A (en) * | 1997-07-09 | 1999-11-16 | Arco Chemical Technology, Lp | Method of making a water reducing additive for cement |
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Cited By (8)
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| CN104016614A (en) * | 2014-06-13 | 2014-09-03 | 石家庄市长安育才建材有限公司 | Polycarboxylate water reducer with defoaming function and preparation method of water reducer |
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| CN105131200A (en) * | 2015-09-17 | 2015-12-09 | 安徽森普新型材料发展有限公司 | Preparation method of powder polycarboxylate water reducer with air-entraining and defoaming functions |
| CN106589252A (en) * | 2016-11-10 | 2017-04-26 | 厦门路桥翔通建材科技有限公司 | Low air-entraining type maleic anhydride poly carboxylic acid water reducing agent and preparation method thereof |
| CN106589252B (en) * | 2016-11-10 | 2018-11-27 | 福建路桥翔通建材科技有限公司 | A kind of low entraining type maleic anhydride class polycarboxylate water-reducer and preparation method thereof |
| CN106905493A (en) * | 2017-03-20 | 2017-06-30 | 江苏苏博特新材料股份有限公司 | A kind of froth breaking type poly-carboxylic-acid cement dispersant and preparation method thereof |
| CN106905493B (en) * | 2017-03-20 | 2019-12-27 | 江苏苏博特新材料股份有限公司 | Defoaming polycarboxylic acid cement dispersant and preparation method thereof |
| CN112279553A (en) * | 2020-09-28 | 2021-01-29 | 浙江玖龙新材料有限公司 | Ester polycarboxylate superplasticizer formula and preparation method |
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