CN104446105A - Polycarboxylic super plasticizer - Google Patents
Polycarboxylic super plasticizer Download PDFInfo
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- CN104446105A CN104446105A CN201410610310.5A CN201410610310A CN104446105A CN 104446105 A CN104446105 A CN 104446105A CN 201410610310 A CN201410610310 A CN 201410610310A CN 104446105 A CN104446105 A CN 104446105A
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Abstract
The invention discloses a polycarboxylic super plasticizer which is formed by copolymerizing alkyl unsaturated polyether A which accounts for 60-95% of the total weight of a monomer, an unsaturated carboxylic monomer which accounts for 5-30% of the total weight of the monomer, N-vinyl pyrrolidone which accounts for 0.5-5.0% of the total weight of the monomer and a polymerizable monomer C which accounts for 0-20% of the total weight of the monomer in an aqueous liquid at 40-100 DEG C in the presence of an initiator and a chain transfer agent. According to the polycarboxylic super plasticizer disclosed by the invention, in the presence of pyrrolidone lactam ring, the contact among cement particles is reduced, so that good dispersibility and dispersing stability are provided for concrete.
Description
Technical field
The invention belongs to technical field of concrete additives, relate to mortar and the reinforcement of concrete superplasticizer, more particularly relate to a kind of polycarboxylic acid super-plasticizer.
Background technology
Along with the development of modern concrete technology, the application of high performance concrete in engineering construction is more and more extensive, polycarboxylic acid super-plasticizer is as the chemical admixture of current latest generation, for concrete provides good mobility and flowing retentivity, become and prepare the indispensable component of high performance concrete.Existing polycarboxylic acid super-plasticizer mainly adopts acrylic acid or the like, acrylic amide minor comonomer and the copolymerization of unsaturated alkyl polyethers to obtain, acrylic acid or the like, acrylic amide minor comonomer are sterically hindered less, easy polymerization, but because individual space steric hindrance is less, also the space resistance between cement granules and particle be can reduce after being adsorbed on cement particle surface, dispersiveness and the dispersion retentivity of polycarboxylic acid super-plasticizer are unfavorable for.
Summary of the invention
For the problems referred to above, the invention provides a kind of polycarboxylic acid super-plasticizer, it is that under initiator and chain-transfer agent existent condition, copolymerization obtains by the NVP of unsaturated carboxylic acid monomer B, 0.5%-5.0% of alkyl unsaturated polyether A, 5%-30% part accounting for monomer total mass 60%-95% part and the polymerisable monomer C of 0%-20% in 40 ° of-100 ° of aqueous solution;
Wherein: the compound of monomer A represented by general formula (A):
In general formula (A): n is 0,1,2,3; M is the arbitrary integer of 1-120; R
1represent hydrogen or methyl; R
2o is oxyalkylene group of 2-8 carbon atom and composition thereof, and R3 is hydrogen, the alkyl of a 1-6 carbon atom or its mixture;
Unsaturated carboxylic acid monomer B is: the one of vinylformic acid, methacrylic acid, butenoic acid, methylene-succinic acid, itaconic anhydride, toxilic acid, maleic anhydride, fumaric acid, two or more mixture;
Polymerisable monomer C is: methyl acrylate, ethyl propenoate, butyl acrylate, Hydroxyethyl acrylate, Propylene glycol monoacrylate, dimethylaminoethyl acrylate, vinylformic acid lignocaine ethyl ester, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, butyl methacrylate, hydroxyethyl methylacrylate, Rocryl 410, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, vinyl cyanide, sodium allyl sulfonate, methallylsulfonic acid sodium, sodium p styrene sulfonate, acrylamide, 2-acrylamide-2 methyl propane sulfonic acid or its salt, propylene sulphur ethyl ester, methacrylic sulphur ethyl ester, n-methylolacrylamide, one or more mixing in vinyl acetate.
Described polycarboxylic acid super-plasticizer, its initiator comprises thermal decomposition initiating and redox initiator.Thermal decomposition initiating comprises one or more mixing of ammonium persulphate, Potassium Persulphate, Sodium Persulfate, hydrogen peroxide or tertbutyl peroxide; Redox initiator adopts thermal decomposition initiating and reductive agent jointly to form, wherein thermal decomposition initiating is one or more mixing of ammonium persulphate, Potassium Persulphate, Sodium Persulfate, hydrogen peroxide or tertbutyl peroxide, and reductive agent is one or more mixing in sodium bisulfite, Potassium hydrogen sulfite, Sodium Pyrosulfite, Hypophosporous Acid, 50, sodium hypophosphite, potassium hypophosphite, rongalite, xitix and sodium ascorbate.
Described polycarboxylic acid super-plasticizer, the thermal decomposition initiating consumption joined in reaction system is the 0.1%-10.0% of monomer total mass, and the reductive agent consumption joined in reaction system is the 0%-8% of monomer total mass.
Described polycarboxylic acid super-plasticizer, chain-transfer agent used is one or more mixing in Virahol, mercaptoethanol, Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid and Dodecyl Mercaptan, and chain-transfer agent consumption accounts for the 0.2%-8.0% of monomer total mass.
Described polycarboxylic acid super-plasticizer, its unsaturated alkyl polyethers A can be one or more mixing in isobutene alcohol polyoxyethylene ether HPEG, prenol polyoxyethylene ether TPEG.
Described polycarboxylic acid super-plasticizer is that copolymerization obtains in the aqueous solution of 40 °-100 °, and the copolyreaction time is 2-10 hour, after copolyreaction terminates, can select as required regulate the pH value of product or do not regulate.If selection adjust ph, neutralization reagent used is sodium hydroxide, potassium hydroxide, calcium hydroxide, amine or organic amine and their aqueous solution.
Its weight-average molecular weight of described polycarboxylic acid super-plasticizer is 10000-200000.
Owing to introducing NVP monomer in the present invention, on its molecular chain, the existence of pyrrolidone lactam nucleus increases the sterically hindered of polycarboxylic acid super-plasticizer molecule, thus the contact reduced between cement granules, for concrete provides good dispersiveness and dispersion retentivity, and can significantly improve concrete serviceability.
concrete case study on implementation
By following case study on implementation, the present invention is described further, but any restriction is not produced to the present invention.
Use listed abbreviation in an embodiment below:
A1
:the average oxyethyl group adduct number 54 of isobutene alcohol polyoxyethylene ether HPEG()
A2: prenol polyoxyethylene ether TPEG(average oxyethyl group adduct number 23)
A3: prenol polyoxyethylene ether TPEG(average oxyethyl group adduct number 90)
B1: vinylformic acid
B2: maleic anhydride
C1:2-acrylamide-2 methyl propane sulfonic acid
C2: acrylamide
Case study on implementation 1
Be configured with agitator, thermometer, Dropping feeder 1000ml four-hole boiling flask in add 432g A1,310.5g water, stir be warming up to 60 DEG C.Add the hydrogen peroxide of 2.50g 30% concentration, start to drip 50.0g initiator solution (by 1.50g sodium ascorbate, 2.5g 3-thiohydracrylic acid is dissolved in 46g water and obtains), then the NVP aqueous solution (be dissolved in 44.0g water by 4.0g NVP and obtain) of 80.0g monomer solution (be dissolved in 28.2g water by 51.8g B1 monomer and obtain) and 48.0g is dripped respectively, initiator time for adding controls at 210 minutes, monomer solution and NVP aqueous solution time for adding control at 180 minutes, temperature of reaction controls at 58 ~ 62 DEG C.After dropping terminates, at 58 ~ 62 DEG C, be incubated 60 minutes, make polyreaction complete.After insulation terminates, be cooled to less than 50 DEG C and add the 77.0g 30%NaOH aqueous solution, obtain polycarboxylic acid super-plasticizer PCE-1 of the present invention, its solid content is 50.4%, and weight-average molecular weight is 46000.
Case study on implementation 2
Be configured with agitator, thermometer, Dropping feeder 1000ml four-hole boiling flask in add 408g A1,298g water, stir be warming up to 60 DEG C.Add the hydrogen peroxide of 3.0g 30% concentration, start to drip 50g initiator solution (by 1.50g sodium ascorbate, 2.8g 3-thiohydracrylic acid is dissolved in 45.7g water and obtains), then 120.0g monomer solution is dripped respectively (by 42.8g B1 monomer, 35.2g C1 monomer is dissolved in 42g water and obtains) and the NVP aqueous solution (be dissolved in 30.5g water by 9.5g NVP and obtain) of 40.0g, initiator time for adding controls at 210 minutes, monomer solution and NVP aqueous solution time for adding control at 180 minutes, temperature of reaction controls at 58 ~ 62 DEG C.After dropping terminates, at 58 ~ 62 DEG C, be incubated 60 minutes, make polyreaction complete.After insulation terminates, be cooled to less than 50 DEG C and add the 81.0g 30%NaOH aqueous solution, obtain polycarboxylic acid super-plasticizer PCE-2 of the present invention, its solid content is 51.2%, and weight-average molecular weight is 54000.
Case study on implementation 3
Be configured with agitator, thermometer, Dropping feeder 1000ml four-hole boiling flask in add 396g A2,16g B2,325g water, stir be warming up to 65 DEG C.Add the hydrogen peroxide of 3.0g 30% concentration, start to drip 50g initiator solution (by 1.50g sodium ascorbate, 2.5g 3-thiohydracrylic acid is dissolved in 46g water and obtains), then the NVP aqueous solution (be dissolved in 39g water by 11g NVP and obtain) of 90.0g monomer solution (be dissolved in 54.4g water by 35.6g B1 monomer and obtain) and 50.0g is dripped respectively, initiator time for adding controls at 240 minutes, monomer solution and NVP aqueous solution time for adding control at 210 minutes, temperature of reaction controls at 63 ~ 67 DEG C.After dropping terminates, at 63 ~ 67 DEG C, be incubated 60 minutes, make polyreaction complete.After insulation terminates, be cooled to less than 50 DEG C and add the 70.0g 30%NaOH aqueous solution, obtain polycarboxylic acid super-plasticizer PCE-3 of the present invention, its solid content is 47.5%, and weight-average molecular weight is 41000.
Case study on implementation 4
Be configured with agitator, thermometer, Dropping feeder 1000ml four-hole boiling flask in add 400g A3,302g water, stir be warming up to 60 DEG C.Add the hydrogen peroxide of 3.0g 30% concentration, start to drip 50g initiator solution (by 1.50g sodium ascorbate, 3.8g 3-thiohydracrylic acid is dissolved in 44.7g water and obtains), then 120.0g monomer solution is dripped respectively (by 61.2g B1 monomer, 14.2g C2 monomer is dissolved in 44.6g water and obtains) and the NVP aqueous solution (be dissolved in 34.5g water by 5.5g NVP and obtain) of 40.0g, initiator time for adding controls at 240 minutes, monomer solution and NVP aqueous solution time for adding control at 210 minutes, temperature of reaction controls at 58 ~ 62 DEG C.After dropping terminates, at 58 ~ 62 DEG C, be incubated 60 minutes, make polyreaction complete.After insulation terminates, be cooled to less than 50 DEG C and add the 85.0g 30%NaOH aqueous solution, obtain polycarboxylic acid super-plasticizer PCE-4 of the present invention, its solid content is 49.9%, and weight-average molecular weight is 68000.
Application examples
According to the test request of high-performance water reducing agent in GB8076-2008 " concrete admixture " standard, the sample of 1-4 synthesis in case study on implementation and certain commercially available polycarboxylic acid super-plasticizer (code name PCE) have been carried out performance comparison, and experimental result is in table 1.
Table 1 polycarboxylic acid super-plasticizer the performance test results
As can be seen from the test result of table 1, compared with commercially available polycarboxylic acid super-plasticizer, polycarboxylate water-reducer of the present invention still has high water-reducing rate and slump retention ability under lower volume, shows good dispersiveness and dispersion retentivity.
Claims (8)
1. a polycarboxylic acid super-plasticizer, it is characterized in that it is that copolymerization obtains under initiator and chain-transfer agent existent condition by the NVP of unsaturated carboxylic acid monomer B, 0.5%-5.0% of alkyl unsaturated polyether A, 5%-30% part accounting for monomer total mass 60%-95% part and the polymerisable monomer C of 0%-20% in 40 ° of-100 ° of aqueous solution;
Wherein: the compound of monomer A represented by general formula (A):
In general formula (A): n is 0,1,2,3; M is the arbitrary integer of 1-120; R
1represent hydrogen or methyl; R
2o is oxyalkylene group of 2-8 carbon atom and composition thereof, and R3 is hydrogen, the alkyl of a 1-6 carbon atom or its mixture;
Unsaturated carboxylic acid monomer B is: the one of vinylformic acid, methacrylic acid, butenoic acid, methylene-succinic acid, itaconic anhydride, toxilic acid, maleic anhydride, fumaric acid, two or more mixture;
Polymerisable monomer C is: methyl acrylate, ethyl propenoate, butyl acrylate, Hydroxyethyl acrylate, Propylene glycol monoacrylate, dimethylaminoethyl acrylate, vinylformic acid lignocaine ethyl ester, methyl methacrylate, methyl esters ethyl propenoate, butyl methacrylate, hydroxyethyl methylacrylate, Rocryl 410, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, vinyl cyanide, sodium allyl sulfonate, methallylsulfonic acid sodium, sodium p styrene sulfonate, acrylamide, 2-acrylamide-2 methyl propane sulfonic acid or its salt, propylene sulphur ethyl ester, methacrylic sulphur ethyl ester, n-methylolacrylamide, one or more mixing in vinyl acetate.
2. polycarboxylic acid super-plasticizer according to claim 1, is characterized in that described initiator comprises thermal decomposition initiating and redox initiator.
3. thermal decomposition initiating is one or more mixing of ammonium persulphate, Potassium Persulphate, Sodium Persulfate, hydrogen peroxide or tertbutyl peroxide; Redox initiator adopts thermal decomposition initiating and reductive agent jointly to form, wherein thermal decomposition initiating is one or more mixing of ammonium persulphate, Potassium Persulphate, Sodium Persulfate, hydrogen peroxide or tertbutyl peroxide, and reductive agent is one or more mixing in sodium bisulfite, Potassium hydrogen sulfite, Sodium Pyrosulfite, Hypophosporous Acid, 50, sodium hypophosphite, potassium hypophosphite, rongalite, xitix and sodium ascorbate.
4. polycarboxylic acid super-plasticizer according to claim 1, is characterized in that the thermal decomposition initiating consumption joined in reaction system is the 0.1%-10.0% of monomer total mass, and the reductive agent consumption joined in reaction system is the 0%-8% of monomer total mass.
5. polycarboxylic acid super-plasticizer according to claim 1, its feature is one or more mixing in Virahol, mercaptoethanol, Thiovanic acid, 2 mercaptopropionic acid, 3-thiohydracrylic acid and Dodecyl Mercaptan at chain-transfer agent used, and chain-transfer agent consumption accounts for the 0.2%-8.0% of monomer total mass.
6. polycarboxylic acid super-plasticizer according to claim 1, is characterized in that described unsaturated alkyl polyethers A is one or more mixing in isobutene alcohol polyoxyethylene ether HPEG, prenol polyoxyethylene ether TPEG.
7. the polycarboxylic acid super-plasticizer according to claim 1-5 Arbitrary Term, it is characterized in that it is that copolymerization obtains in the aqueous solution of 40 °-100 °, the copolyreaction time is 2-10 hour.
8. the polycarboxylic acid super-plasticizer according to claim 1-6 Arbitrary Term, is characterized in that its weight-average molecular weight is 10000-200000.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829792A (en) * | 2015-05-12 | 2015-08-12 | 西南科技大学 | Method for preparing polyether modified polycarboxylic acid grinding aid |
| CN105036596A (en) * | 2015-08-04 | 2015-11-11 | 科之杰新材料集团有限公司 | Low-temperature synthesis polycarboxylate superplasticizer and preparation method thereof |
| CN105367721A (en) * | 2015-11-30 | 2016-03-02 | 江苏苏博特新材料股份有限公司 | Method for preparing viscosity-reduction-type polycarboxylic acid superplasticizer and application of viscosity-reduction-type polycarboxylic acid superplasticizer |
| CN105712650A (en) * | 2015-12-11 | 2016-06-29 | 江苏苏博特新材料股份有限公司 | Method for preparing high-adaptability polycarboxylate water-reducing agent |
| CN105732911A (en) * | 2016-01-15 | 2016-07-06 | 江苏苏博特新材料股份有限公司 | Preparation method and application of viscosity-reducing polycarboxylate superplasticizer |
| CN105754034A (en) * | 2016-03-09 | 2016-07-13 | 合众（佛山）化工有限公司 | N-Methylolacrylamide modified polycarboxylate ceramic water reducer and normal-temperature preparation method and application thereof |
| CN106496433A (en) * | 2016-10-11 | 2017-03-15 | 常州市鼎升环保科技有限公司 | A kind of preparation method of polycarboxylic acid super-plasticizer |
| CN106608950A (en) * | 2016-12-22 | 2017-05-03 | 江苏奥克化学有限公司 | Lactam polycarboxylic water reducing agent and preparation method thereof |
| CN110655625A (en) * | 2019-10-30 | 2020-01-07 | 广东红墙新材料股份有限公司 | Multifunctional polycarboxylate superplasticizer containing gradient polymer side chains and preparation method thereof |
| CN111607040A (en) * | 2020-06-24 | 2020-09-01 | 南宁新泰瑞科建材股份有限公司 | Super-slow release type polycarboxylic slump retaining agent and preparation method thereof |
| CN113603840A (en) * | 2021-09-06 | 2021-11-05 | 抚顺东科精细化工有限公司 | Preparation method of antirust slow-release polycarboxylic acid superplasticizer |
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| CN101914187A (en) * | 2010-08-19 | 2010-12-15 | 上海三瑞高分子材料有限公司 | Polycarboxylic acid super-plasticizer |
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Patent Citations (2)
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| CN101333092A (en) * | 2007-06-25 | 2008-12-31 | 深圳市海川实业股份有限公司 | Cement concrete superplasticizer and method for preparing same |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829792A (en) * | 2015-05-12 | 2015-08-12 | 西南科技大学 | Method for preparing polyether modified polycarboxylic acid grinding aid |
| CN104829792B (en) * | 2015-05-12 | 2018-04-13 | 西南科技大学 | A kind of preparation method of polyether-modified polycarboxylic acids grinding aid |
| CN105036596A (en) * | 2015-08-04 | 2015-11-11 | 科之杰新材料集团有限公司 | Low-temperature synthesis polycarboxylate superplasticizer and preparation method thereof |
| CN105036596B (en) * | 2015-08-04 | 2017-03-22 | 科之杰新材料集团有限公司 | Low-temperature synthesis polycarboxylate superplasticizer and preparation method thereof |
| CN105367721A (en) * | 2015-11-30 | 2016-03-02 | 江苏苏博特新材料股份有限公司 | Method for preparing viscosity-reduction-type polycarboxylic acid superplasticizer and application of viscosity-reduction-type polycarboxylic acid superplasticizer |
| CN105367721B (en) * | 2015-11-30 | 2018-02-23 | 江苏苏博特新材料股份有限公司 | The preparation method and application of viscosity reduction type polycarboxylic acid super-plasticizer |
| CN105712650A (en) * | 2015-12-11 | 2016-06-29 | 江苏苏博特新材料股份有限公司 | Method for preparing high-adaptability polycarboxylate water-reducing agent |
| CN105732911B (en) * | 2016-01-15 | 2018-02-23 | 江苏苏博特新材料股份有限公司 | The preparation method and application of viscosity reduction type polycarboxylate water-reducer |
| CN105732911A (en) * | 2016-01-15 | 2016-07-06 | 江苏苏博特新材料股份有限公司 | Preparation method and application of viscosity-reducing polycarboxylate superplasticizer |
| CN105754034B (en) * | 2016-03-09 | 2018-06-29 | 合众（佛山）化工有限公司 | N hydroxymethyl acrylamide modified polycarboxylic acid ceramic water reducing agent and its normal temperature preparation method and application |
| CN105754034A (en) * | 2016-03-09 | 2016-07-13 | 合众（佛山）化工有限公司 | N-Methylolacrylamide modified polycarboxylate ceramic water reducer and normal-temperature preparation method and application thereof |
| CN106496433A (en) * | 2016-10-11 | 2017-03-15 | 常州市鼎升环保科技有限公司 | A kind of preparation method of polycarboxylic acid super-plasticizer |
| CN106608950A (en) * | 2016-12-22 | 2017-05-03 | 江苏奥克化学有限公司 | Lactam polycarboxylic water reducing agent and preparation method thereof |
| CN110655625A (en) * | 2019-10-30 | 2020-01-07 | 广东红墙新材料股份有限公司 | Multifunctional polycarboxylate superplasticizer containing gradient polymer side chains and preparation method thereof |
| CN110655625B (en) * | 2019-10-30 | 2022-01-07 | 广东红墙新材料股份有限公司 | Multifunctional polycarboxylate superplasticizer containing gradient polymer side chains and preparation method thereof |
| CN111607040A (en) * | 2020-06-24 | 2020-09-01 | 南宁新泰瑞科建材股份有限公司 | Super-slow release type polycarboxylic slump retaining agent and preparation method thereof |
| CN111607040B (en) * | 2020-06-24 | 2022-11-04 | 南宁新泰瑞科建材股份有限公司 | Super-slow release type polycarboxylic slump retaining agent and preparation method thereof |
| CN113603840A (en) * | 2021-09-06 | 2021-11-05 | 抚顺东科精细化工有限公司 | Preparation method of antirust slow-release polycarboxylic acid superplasticizer |
| CN113603840B (en) * | 2021-09-06 | 2023-09-19 | 抚顺东科精细化工有限公司 | Preparation method of rust-proof slow-release polycarboxylic acid superplasticizer |
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