CN102358774B - Preparation method of polycarboxylic acid high-efficiency water reducer - Google Patents
Preparation method of polycarboxylic acid high-efficiency water reducer Download PDFInfo
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- CN102358774B CN102358774B CN201110212778A CN201110212778A CN102358774B CN 102358774 B CN102358774 B CN 102358774B CN 201110212778 A CN201110212778 A CN 201110212778A CN 201110212778 A CN201110212778 A CN 201110212778A CN 102358774 B CN102358774 B CN 102358774B
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Abstract
The invention belongs to the technical field of water reducers for concrete, and specially, relates to a preparation method of a polycarboxylic acid high-efficiency water reducer. The preparation method comprises the following steps of mixing water, an unsaturated polyether and a monomer containing unsaturated double-bond and polar groups, heating the mixture to a temperature of 50 to 70 DEG C, adding an unsaturated carboxylic acid, an initiator, a polymeric chain growth agent and a terminator by one process, and carrying out heat preservation for 0.5 to 1 hour to obtain the polycarboxylic acid high-efficiency water reducer. The preparation method has the advantages of simple process, short reaction period and low energy consumption.
Description
Technical field
The invention belongs to concrete and use the water reducer technical field, particularly a kind of preparation method of high-efficiency water-reducing agent of poly-carboxylic acid.
Background technology
Water reducer is a kind of important concrete admixture, is one of staple product of building material mainstay industry.High efficiency water reducing agent has not only improved the mechanical property of high-strength concrete greatly, and simple and easy to do construction technology is provided.High-efficiency water-reducing agent of poly-carboxylic acid be continue wooden calcium be the ordinary water-reducing agent of representative and be the high efficiency water reducing agent of representative with naphthalene system after the third generation high-performance water reducing agent that grows up, be forefront, scientific and technological content is the highest, application prospect is best, over-all properties is optimum a kind of high efficiency water reducing agent in the world at present.Mostly the preparation method of high-efficiency water-reducing agent of poly-carboxylic acid is to adopt monomer under the condition that auxiliary agents such as initiator exist, to be polymerized at present.But have following defective: temperature of reaction is high more, and has the lifting process of temperature; Secondly, because reaction raw materials needs to drip in the reaction process, the dropping time is long, so reaction time is longer, and energy consumption is big.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-efficiency water-reducing agent of poly-carboxylic acid, overcome the defective that present preparing method's temperature is high, reaction time is long.
The technical scheme that the present invention adopts is following:
The preparation method of high-efficiency water-reducing agent of poly-carboxylic acid; Be warming up to 50-70 ℃ with water, unsaturated polyether with after having monomer unsaturated double-bond, the band polar group to mix earlier; Disposable then adding unsaturated carboxylic acid, initiator, polymeric chain growing agent and terminator; Insulation reaction 0.5-1h promptly gets described high-efficiency water-reducing agent of poly-carboxylic acid.
Described unsaturated polyether is the methacrylic Soxylat A 25-7.
Described have unsaturated double-bond, the band polar group monomer be methylpropene sodium sulfonate.
Described unsaturated carboxylic acid is a vinylformic acid.
Described initiator is an ammonium persulphate.
Described polymeric chain growing agent is an acrylic amide.
Described terminator is a Thiovanic acid.
The mass ratio that feeds intake of each material is: water: unsaturated polyether: monomer unsaturated double-bond, the band polar group is arranged: unsaturated carboxylic acid: initiator: polymeric chain growing agent: terminator is 550-650: 300-400: 6-10: 30-40: 2-4: 1-3: 1-3.
Concrete; The preparation process of described polycarboxylate water-reducer is: be warming up to 50-70 ℃ after earlier 600 parts water, 350 parts the methylpropene sodium sulfonate of methacrylic Soxylat A 25-7 and 8 parts being mixed; 35 parts of vinylformic acid of disposable then adding, 3 parts of ammonium persulphates, 2 parts of acrylic amides and 2 parts of Thiovanic acids; Insulation reaction 0.5-1h promptly gets described high-efficiency water-reducing agent of poly-carboxylic acid.
The present invention prepares in the method for polycarboxylate water-reducer; Monomer mixing with partial reaction earlier is warming up to 50-70 ℃, then the monomer adding of other reactions is reacted, because disposable initiator and the chain propagation agent of having added of while; Therefore; Polyreaction is carried out fast, but owing to also added simultaneously terminator, therefore avoided no terminator problem the problem includes: under the situation polyreaction too fast and cause reacting the problem that can't normally carry out.In the traditional method, for fear of reaction carry out too fast, can only adopt long-time, a small amount of mode that drips to carry out, the present invention has then overcome this difficult problem, makes shorten greatly reaction time, reaction process is simplified, and has practiced thrift energy consumption; Simultaneously, temperature of reaction maintains 50-70 ℃ basically, does not need big thermal source, has further practiced thrift energy consumption.
The present invention has following advantage with respect to prior art:
Technology of the present invention is simple, reaction time short, and energy consumption is low.
Embodiment
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
The preparation method of high-efficiency water-reducing agent of poly-carboxylic acid; Be warming up to 70 ℃ after earlier 600 parts water, 350 parts the methylpropene sodium sulfonate of methacrylic Soxylat A 25-7 and 8 parts being mixed; 35 parts of vinylformic acid of disposable then adding, 3 parts of ammonium persulphates, 2 parts of acrylic amides and 2 parts of Thiovanic acids; Insulation reaction 1h promptly gets described high-efficiency water-reducing agent of poly-carboxylic acid.
Embodiment 2
The preparation method of high-efficiency water-reducing agent of poly-carboxylic acid; Be warming up to 55 ℃ after earlier 600 parts water, 300 parts the methylpropene sodium sulfonate of methacrylic Soxylat A 25-7 and 6 parts being mixed; 30 parts of vinylformic acid of disposable then adding, 2 parts of ammonium persulphates, 1 part of acrylic amide and 1 part of Thiovanic acid; Insulation reaction 1h promptly gets described high-efficiency water-reducing agent of poly-carboxylic acid.
Embodiment 3
The preparation method of high-efficiency water-reducing agent of poly-carboxylic acid; Be warming up to 60 ℃ after earlier 650 parts water, 400 parts the methylpropene sodium sulfonate of methacrylic Soxylat A 25-7 and 10 parts being mixed; 40 parts of vinylformic acid of disposable then adding, 4 parts of ammonium persulphates, 3 parts of acrylic amides and 3 parts of Thiovanic acids; Insulation reaction 1h promptly gets described high-efficiency water-reducing agent of poly-carboxylic acid.
The high-efficiency water-reducing agent of poly-carboxylic acid that above embodiment obtains is a colourless transparent liquid.
The detected result of the high-efficiency water-reducing agent of poly-carboxylic acid that embodiment 1 obtains sees the following form 1, and detecting foundation is GB8076-2008; In the detection, agglutinate is a reference cement, and admixture dosage is 0.4% of a cement quality.
Table 1
Claims (6)
1. the preparation method of high-efficiency water-reducing agent of poly-carboxylic acid; It is characterized in that; Be warming up to 50-70 ℃ with water, unsaturated polyether with after having monomer unsaturated double-bond, the band polar group to mix earlier; Disposable then adding unsaturated carboxylic acid, initiator, polymeric chain growing agent and terminator, insulation reaction 0.5-1h promptly gets described high-efficiency water-reducing agent of poly-carboxylic acid; Described unsaturated polyether is the methacrylic Soxylat A 25-7; Described have unsaturated double-bond, the band polar group monomer be methylpropene sodium sulfonate; The mass ratio that feeds intake of each material is: water: unsaturated polyether: monomer unsaturated double-bond, the band polar group is arranged: unsaturated carboxylic acid: initiator: polymeric chain growing agent: terminator is 550-650:300-400:6-10:30-40:2-4:1-3:1-3.
2. the preparation method of high-efficiency water-reducing agent of poly-carboxylic acid as claimed in claim 1 is characterized in that, described unsaturated carboxylic acid is a vinylformic acid.
3. the preparation method of high-efficiency water-reducing agent of poly-carboxylic acid as claimed in claim 1 is characterized in that, described initiator is an ammonium persulphate.
4. the preparation method of high-efficiency water-reducing agent of poly-carboxylic acid as claimed in claim 1 is characterized in that, described polymeric chain growing agent is an acrylic amide.
5. the preparation method of high-efficiency water-reducing agent of poly-carboxylic acid as claimed in claim 1 is characterized in that, described terminator is a Thiovanic acid.
6. like the preparation method of one of claim 1-5 described high-efficiency water-reducing agent of poly-carboxylic acid; It is characterized in that; Be warming up to 50-70 ℃ after earlier 600 parts water, 350 parts the methylpropene sodium sulfonate of methacrylic Soxylat A 25-7 and 8 parts being mixed; 35 parts of vinylformic acid of disposable then adding, 3 parts of ammonium persulphates, 2 parts of acrylic amides and 2 parts of Thiovanic acids, insulation reaction 0.5-1h promptly gets described high-efficiency water-reducing agent of poly-carboxylic acid.
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| CN201110212778A CN102358774B (en) | 2011-07-28 | 2011-07-28 | Preparation method of polycarboxylic acid high-efficiency water reducer |
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| CN201110212778A CN102358774B (en) | 2011-07-28 | 2011-07-28 | Preparation method of polycarboxylic acid high-efficiency water reducer |
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| CN102358774A CN102358774A (en) | 2012-02-22 |
| CN102358774B true CN102358774B (en) | 2012-10-03 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731730A (en) * | 2012-06-21 | 2012-10-17 | 马清浩 | Hydrogen peroxide auxiliarily-initiated carboxylic acid water reducer and its preparation method |
| CN102936110B (en) * | 2012-12-10 | 2014-08-06 | 马鞍山中海新材料有限公司 | Lignosulfonate-polycarboxylic acid copolymerized composite high-performance water reducer and preparation method thereof |
| CN103172291B (en) * | 2012-12-14 | 2015-05-27 | 上海东大化学有限公司 | Polycarboxylic-acid water reducing agent synthesized at normal temperature, and preparation method and application method thereof |
| CN104496249B (en) * | 2014-12-24 | 2017-01-18 | 江西省萍乡市联友建材有限公司 | High-slump retaining and high-strength slump retaining agent and preparation method thereof |
| CN104817658A (en) * | 2015-05-21 | 2015-08-05 | 苏州市湘园特种精细化工有限公司 | Acrylic acid water reducing agent and preparation method thereof |
| CN104829791A (en) * | 2015-05-21 | 2015-08-12 | 苏州市湘园特种精细化工有限公司 | Water reducer with low slump loss and preparation method of water reducer |
| CN109053966A (en) * | 2018-05-25 | 2018-12-21 | 湖北工业大学 | 2200 molecular weight polyether polycarboxylate water-reducers of one kind and preparation method |
| CN109134780A (en) * | 2018-05-25 | 2019-01-04 | 湖北工业大学 | A kind of hard and soft cabinet-type polycarboxylate water-reducer of main chain and preparation method |
| CN111377674A (en) * | 2018-12-27 | 2020-07-07 | 东莞市易发混凝土有限公司 | Frost resistant concrete compositions and method of making same |
| CN111377673A (en) * | 2018-12-27 | 2020-07-07 | 东莞市易发混凝土有限公司 | Corrosion-resistant concrete material and preparation method thereof |
| CN111377675A (en) * | 2018-12-27 | 2020-07-07 | 东莞市易发混凝土有限公司 | Anti-crack concrete and preparation method thereof |
| CN111393095A (en) * | 2019-01-03 | 2020-07-10 | 东莞市易发混凝土有限公司 | Pervious concrete and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0846090A1 (en) * | 1996-06-21 | 1998-06-10 | Kao Corporation | Concrete admixture |
| CN101066851A (en) * | 2007-06-18 | 2007-11-07 | 江苏博特新材料有限公司 | Concrete slump maintaining agent of polycarboxylate |
| CN101209911A (en) * | 2007-12-25 | 2008-07-02 | 南京瑞迪高新技术公司 | Carboxylic acid polyalcohol water reducing agent capable of controlling concrete slump loss |
| CN101851323A (en) * | 2010-05-28 | 2010-10-06 | 浙江五龙化工股份有限公司 | Multi-branched polycarboxylic water reducer with excellent function of slump protection and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3507281B2 (en) * | 1996-06-21 | 2004-03-15 | 花王株式会社 | Concrete admixture |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0846090A1 (en) * | 1996-06-21 | 1998-06-10 | Kao Corporation | Concrete admixture |
| CN101066851A (en) * | 2007-06-18 | 2007-11-07 | 江苏博特新材料有限公司 | Concrete slump maintaining agent of polycarboxylate |
| CN101209911A (en) * | 2007-12-25 | 2008-07-02 | 南京瑞迪高新技术公司 | Carboxylic acid polyalcohol water reducing agent capable of controlling concrete slump loss |
| CN101851323A (en) * | 2010-05-28 | 2010-10-06 | 浙江五龙化工股份有限公司 | Multi-branched polycarboxylic water reducer with excellent function of slump protection and preparation method thereof |
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