CN102659989A - Preparation method of low-cost concrete polycarboxylic acid water reducing agent - Google Patents
Preparation method of low-cost concrete polycarboxylic acid water reducing agent Download PDFInfo
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- CN102659989A CN102659989A CN2012101525811A CN201210152581A CN102659989A CN 102659989 A CN102659989 A CN 102659989A CN 2012101525811 A CN2012101525811 A CN 2012101525811A CN 201210152581 A CN201210152581 A CN 201210152581A CN 102659989 A CN102659989 A CN 102659989A
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Abstract
The invention discloses a low-cost concrete polycarboxylic acid water reducing agent and a preparation method thereof. The preparation method comprises the following steps: a. dissolving unsaturated polyethenoxy ether in water, adding a comonomer and a molecular weight regulator, and evenly mixing; b. adding an initiator and part of residual comonomer to carry out polymerization; c. keeping the temperature for polymerization while supplementing the initiator so that the reaction is sufficient; and d. after finishing keeping the temperature, cooling and neutralizing. The polycarboxylic acid water reducing agent disclosed by the invention adopts the free-radical polymerization method, and uses water as the solvent. The used comonomer is a cheap novel comonomer, the properties of the water reducing agent are basically not changed, and the cost performance of the product is enhanced. The whole synthetic process does not need heating, does not use any organic solvent; and thus, the invention saves energy, does not cause pollution, has the advantage of low cost, and can be widely used in industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of concrete polycarboxylate water-reducer cheaply, particularly a kind of comonomer of cheapness is produced the method for concrete polycarboxylate water-reducer.
Background technology
Along with being in full swing of China's construction work, architectural concrete amounts such as railway, highway, bridge increase greatly.Simultaneously, the production of high performance concrete such as durable, weather-proof, high-strength more and more depends on high-performance water reducing agent, this wherein takes the lead with railway construction, and the whole nation is popularized in an all-round way and used, just high performance water reducing agent of polyocarboxy acid.
Polycarboxylate water-reducer, be by unsaturated fatty acids and polyoxyethylene glycol through graft polymerization, the high branched polymer dispersion agent that obtains.Compare with water reducer in the past, polycarboxylate water-reducer change in the past progressively be polymerized to chain reaction polymerization, this polyreaction does not have small molecules to produce, and does not produce the three wastes basically, reaction simultaneously is very fast, satisfies supply requirement easily.
In recent years, along with the rise of oil price, the price of petroleum products is also one the tunnel high, and vinylformic acid wherein is the main raw material(s) of producing polycarboxylate water-reducer.Through following the contrast same period last year, acrylic acid price has increased by one times, and how the material cost of the polycarboxylate water-reducer that this improves greatly reduces cost, an important topic that has become polycarboxylate water-reducer to face.
Summary of the invention
Technical problem to be solved by this invention is, produces and the similar product of original polycarboxylate water-reducer performance with cheap starting material, and can be applied in the industrial production.
For solving the problems of the technologies described above; The invention provides a kind of method of producing concrete polycarboxylate water-reducer with cheap starting material; May further comprise the steps: a. is dissolved in the water unsaturated polyoxy Vinyl Ether, adds comonomer and molecular weight regulator, stirs to make it mix; B. drop into the remaining comonomer of initiator and part and make its polymerization; C. add initiator between polymerization period, make its polymerization abundant; The d insulation finishes back cooling neutralization.
Described concrete polycarboxylate water-reducer preparation method, in step a, described unsaturated polyoxy Vinyl Ether can be preferably the alkyl Soxylat A 25-7, and alkyl wherein is preferably isopentene group.
Said concrete polycarboxylate water-reducer preparation method; In step a, the amount of the comonomer that is added is more than 1/2nd of said comonomer total amount; Said comonomer can be 3～10 unsaturated carboxylic acid or acid anhydrides for carbon number, is preferably maleic anhydride and fumaric acid
Said concrete polycarboxylate water-reducer preparation method, in step a, described molecular weight regulator can be preferably sodium allylsulfonate.
Said concrete polycarboxylate water-reducer preparation method, the initiator that in step b, drops into is preferably ammonium persulphate.
Said concrete polycarboxylate water-reducer preparation method, in step b, described part residual monomer is the monomer that can help maleic anhydride or fumaric acid copolymerization, is preferably vinylformic acid or acrylic amide.
Said concrete polycarboxylate water-reducer preparation method, in step c, the described initiator of adding is preferably ammonium persulphate.
Said concrete polycarboxylate water-reducer preparation method in step c, the said time of adding initiator, is preferably and adds once soaking time two/a period of time, or soaking time 1/3rd and three/two o'clock respectively adds once.
Said concrete polycarboxylate water-reducer preparation method, in step c, said soaking time is preferably 3 hours.
Said concrete polycarboxylate water-reducer preparation method, the sodium hydroxide solution that in steps d, adds, its concentration can be preferably 40%, makes said solvent be neutralized to the pH value more than or equal to 7.
For solving the problems of the technologies described above, the present invention also provides a kind of water reducer of aforementioned each the said preparation method of concrete polycarboxylate water-reducer cheaply preparation.
For solving the problems of the technologies described above, the present invention provides a kind of aforementioned each said water reducer application in concrete placement again.
Beneficial technical effects of the present invention is: polycarboxylate water-reducer of the present invention adopts free radical polymerisation process, is solvent with water.Entire synthesis process need not heating, and not with an organic solvent, both save energy did not pollute again, and was with low cost, and in industrial production, can widely apply.
Embodiment
The method that the present invention produces concrete polycarboxylate water-reducer with cheap starting material, may further comprise the steps: a. is dissolved in the water unsaturated polyoxy Vinyl Ether, adds comonomer and molecular weight regulator, stirs to make it mix; B. drop into the remaining comonomer of initiator and part and make its polymerization; C. add initiator between polymerization period, make its polymerization abundant; The d insulation finishes back cooling neutralization.
Described concrete polycarboxylate water-reducer preparation method, in step a, described unsaturated polyoxy Vinyl Ether can be preferably the alkyl Soxylat A 25-7, and alkyl wherein is preferably isopentene group.
Said concrete polycarboxylate water-reducer preparation method; In step a, the amount of the comonomer that is added is more than 1/2nd of said comonomer total amount; Said comonomer can be 3～10 unsaturated carboxylic acid or acid anhydrides for carbon number, is preferably maleic anhydride and fumaric acid
Said concrete polycarboxylate water-reducer preparation method, in step a, described molecular weight regulator can be preferably sodium allylsulfonate.
Said concrete polycarboxylate water-reducer preparation method, the initiator that in step b, drops into is preferably ammonium persulphate.
Said concrete polycarboxylate water-reducer preparation method, in step b, described part residual monomer is the monomer that can help maleic anhydride or fumaric acid copolymerization, is preferably vinylformic acid or acrylic amide.
Said concrete polycarboxylate water-reducer preparation method, in step c, the described initiator of adding is preferably ammonium persulphate.
Said concrete polycarboxylate water-reducer preparation method in step c, the said time of adding initiator, is preferably and adds once soaking time two/a period of time, or soaking time 1/3rd and three/two o'clock respectively adds once.
Said concrete polycarboxylate water-reducer preparation method, in step c, said soaking time is preferably 3 hours.
Said concrete polycarboxylate water-reducer preparation method, the sodium hydroxide solution that in steps d, adds, its concentration can be preferably 40%, makes said solvent be neutralized to the pH value more than or equal to 7.
In another embodiment of the present invention, a kind of water reducer of aforementioned each the said preparation method of concrete polycarboxylate water-reducer cheaply preparation is provided also.
In an embodiment more of the present invention, a kind of aforementioned each said water reducer application in concrete placement is provided again.
Below will combine form and specific embodiment to specify embodiment of the present invention, how the utilisation technology means solve technical problem to the present invention whereby, and the implementation procedure of reaching technique effect can make much of and implement according to this.
The raw material umber is mass ratio among all embodiment.
Embodiment 1:
During normal temperature, in the four-hole boiling flask that TM, whisking appliance are housed, add 90 parts of entry, 4 parts of 60 parts of maleic anhydrides of isopentene Soxylat A 25-7,1.3 parts of sodium allyl sulfonates constantly stir so that it all is dissolved in the water and heats up; Add 1 part of acrylic amide in the time of 80 ℃, 0.4 part in vinylformic acid, 0.6 part of ammonium persulphate, and insulation.When being incubated 1.5 hours, add 0.2 part of ammonium persulphate.Be incubated cooling after 3 hours, 7 parts of the sodium hydroxide solutions of adding 40%, continuing to stir promptly obtains product.
Embodiment 2:
During normal temperature, in the four-hole boiling flask that TM, whisking appliance are housed, add 90 parts of entry, 5.2 parts of 60 parts of maleic anhydrides of isopentene Soxylat A 25-7,1.3 parts of sodium allyl sulfonates constantly stir so that it all is dissolved in the water and heats up; Add 1 part of acrylic amide in the time of 80 ℃, 0.6 part of ammonium persulphate, and insulation.Be incubated 1 hour and 2 hours the time, respectively add 0.15 part of ammonium persulphate.Be incubated cooling after 3 hours, 7 parts of the sodium hydroxide solutions of adding 40%, continuing to stir promptly obtains product.
In the another embodiment of the present invention, provided the market value of raw material, like following table:
Last product price is:
Statistical item result
Solid content concentration 0.453538813
Every kg of pure article price 15.81261012
Calculate through above table, can learn, therefore the preparation cost of product of the present invention is a kind of concrete polycarboxylate water-reducer cheaply far below the preparation cost of like product.
Claims (5)
1. a concrete polycarboxylate water-reducer preparation method cheaply is characterized in that, may further comprise the steps:
A. unsaturated polyoxy Vinyl Ether is dissolved in the water, adds comonomer and molecular weight regulator, stirring makes it mix;
B. drop into the remaining comonomer of initiator and part and make its polymerization;
C. be incubated polymerization, during add initiator, make its sufficient reacting;
The d insulation finishes back cooling neutralization;
In step a, described unsaturated polyoxy Vinyl Ether is the alkyl Soxylat A 25-7, and alkyl wherein is optimized for isopentene group;
In step a, the amount of the comonomer that is added is more than 1/2nd of said comonomer total amount, and said comonomer is that carbon number is 3～10 unsaturated carboxylic acid or acid anhydrides, is preferably maleic anhydride, fumaric acid;
In step a, described molecular weight regulator is a sodium allylsulfonate;
Described initiator is an ammonium persulphate;
In step b, described part residual monomer is the monomer that can help maleic anhydride or fumaric acid copolymerization, is preferably vinylformic acid or acrylic amide;
In step c, the described initiator of adding is preferably ammonium persulphate;
In step c, the said time of adding initiator, be preferably and add once soaking time two/a period of time, or soaking time 1/3rd and three/two o'clock respectively add once.
2. according to the said concrete polycarboxylate water-reducer cheaply of claim 1 preparation method, it is characterized in that in step c, said soaking time is preferably 3 hours.
3. according to the said concrete polycarboxylate water-reducer cheaply of claim 1 preparation method, it is characterized in that, in steps d, the sodium hydroxide solution of adding, its concentration can be preferably 40%, makes said solvent be neutralized to the pH value more than or equal to 7.
4. water reducer like each said preparation method of concrete polycarboxylate water-reducer cheaply preparation in the claim 1～3.
5. the application of the said water reducer of claim 4 in concrete placement.
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| CN2012101525811A CN102659989A (en) | 2011-12-16 | 2012-05-17 | Preparation method of low-cost concrete polycarboxylic acid water reducing agent |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483505A (en) * | 2013-09-25 | 2014-01-01 | 山东省水利科学研究院 | Polycarboxylate superplasticizer catalyzing production technology without high temperature |
| CN103588414A (en) * | 2013-11-21 | 2014-02-19 | 中建商品混凝土有限公司 | High-performance polycarboxylic acid water reducer and special compound admixture containing the water reducer for limestone powder concrete |
| CN103723945A (en) * | 2013-11-28 | 2014-04-16 | 中建商品混凝土有限公司 | Fast hydrolyzable slow releasing polycarboxylate superplasticizer and preparation method thereof |
| CN105347718A (en) * | 2015-10-08 | 2016-02-24 | 南京瑞迪高新技术有限公司 | Viscosity-control type polycarboxylate superplasticizer for lean cemented concrete and preparation method of viscosity-control type polycarboxylate superplasticizer |
| CN105732910A (en) * | 2014-12-11 | 2016-07-06 | 天津冶建特种材料有限公司 | Synthetic method for polycarboxylic additive |
| CN105949403A (en) * | 2016-04-29 | 2016-09-21 | 华侨大学 | Chitosan containing ether type polycarboxylic acid concrete admixture and preparation method therefor |
| CN105968274A (en) * | 2016-04-29 | 2016-09-28 | 华侨大学 | Chitosan-containing polycarboxylic concrete additive and preparation method thereof |
| CN107056992A (en) * | 2016-12-31 | 2017-08-18 | 武汉理工大学 | A kind of feature ethers polycarboxylic acid water reducing agent and preparation method thereof |
| CN108726912A (en) * | 2018-06-15 | 2018-11-02 | 山西中铁铁诚建材科技有限公司 | A kind of polycarboxylate water-reducer and its preparation process |
| CN113214438A (en) * | 2021-06-29 | 2021-08-06 | 安徽海螺新材料科技有限公司 | Polycarboxylic acid water reducing agent containing maleic anhydride and preparation method thereof |
-
2012
- 2012-05-17 CN CN2012101525811A patent/CN102659989A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483505A (en) * | 2013-09-25 | 2014-01-01 | 山东省水利科学研究院 | Polycarboxylate superplasticizer catalyzing production technology without high temperature |
| CN103588414A (en) * | 2013-11-21 | 2014-02-19 | 中建商品混凝土有限公司 | High-performance polycarboxylic acid water reducer and special compound admixture containing the water reducer for limestone powder concrete |
| CN103588414B (en) * | 2013-11-21 | 2015-03-04 | 中建商品混凝土有限公司 | High-performance polycarboxylic acid water reducer and special compound admixture containing the water reducer for limestone powder concrete |
| CN103723945A (en) * | 2013-11-28 | 2014-04-16 | 中建商品混凝土有限公司 | Fast hydrolyzable slow releasing polycarboxylate superplasticizer and preparation method thereof |
| CN103723945B (en) * | 2013-11-28 | 2016-05-18 | 中建商品混凝土有限公司 | A kind of fast hydrolysis sustained-release polycarboxylic water reducer and preparation method thereof |
| CN105732910A (en) * | 2014-12-11 | 2016-07-06 | 天津冶建特种材料有限公司 | Synthetic method for polycarboxylic additive |
| CN105347718A (en) * | 2015-10-08 | 2016-02-24 | 南京瑞迪高新技术有限公司 | Viscosity-control type polycarboxylate superplasticizer for lean cemented concrete and preparation method of viscosity-control type polycarboxylate superplasticizer |
| CN105949403A (en) * | 2016-04-29 | 2016-09-21 | 华侨大学 | Chitosan containing ether type polycarboxylic acid concrete admixture and preparation method therefor |
| CN105968274A (en) * | 2016-04-29 | 2016-09-28 | 华侨大学 | Chitosan-containing polycarboxylic concrete additive and preparation method thereof |
| CN107056992A (en) * | 2016-12-31 | 2017-08-18 | 武汉理工大学 | A kind of feature ethers polycarboxylic acid water reducing agent and preparation method thereof |
| CN108726912A (en) * | 2018-06-15 | 2018-11-02 | 山西中铁铁诚建材科技有限公司 | A kind of polycarboxylate water-reducer and its preparation process |
| CN113214438A (en) * | 2021-06-29 | 2021-08-06 | 安徽海螺新材料科技有限公司 | Polycarboxylic acid water reducing agent containing maleic anhydride and preparation method thereof |
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Application publication date: 20120912 |