CN104892856A - Preparation method of polycarboxylate superplasticizer - Google Patents
Preparation method of polycarboxylate superplasticizer Download PDFInfo
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- CN104892856A CN104892856A CN201510277968.3A CN201510277968A CN104892856A CN 104892856 A CN104892856 A CN 104892856A CN 201510277968 A CN201510277968 A CN 201510277968A CN 104892856 A CN104892856 A CN 104892856A
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Abstract
The invention relates to a preparation method of a polycarboxylate superplasticizer, belonging to the technical fields of building materials and cement concrete admixtures. The polycarboxylate superplasticizer is prepared by taking methylallyl polyethylene glycol and acrylamide as reaction monomers and sodium dodecyl sulfonate as a surface absorption activator, adding a chain transfer agent and an initiator, and finally, regulating the PH value to 6-7 by using an alkaline solution. The polycarboxylate superplasticizer is high in yield and good in performance; and due to the addition of sodium dodecyl sulfonate, the saturation rate of charges adsorbed by particles on a concrete surface can be increased, the flowability of cement in concrete stirring can be improved, the stirring time can be shortened, the efficiency can be increased, and an anti-adhesion effect is better taken. The polycarboxylate superplasticizer is simple in preparation process, low in cost, high in water reducing efficiency, good in cement and concrete compatibility and capable of effectively improving the flowability, slump constant, superstrength and durability of concrete.
Description
Technical field
The invention belongs to material of construction and cement concrete admixture technical field, be specially a kind of polycarboxylate water-reducer and preparation method thereof.
Background technology
Concrete is maximum, the most widely used material of construction of consumption in the world.Recent decades, concrete technology enters new developmental stage, and its range of application is also in further expansion.Pump concrete, self-compacting concrete, non-dispersible underwater concrete, sprayed concrete, polymer concrete etc., the demand for development concrete of the new technologies such as high-strength high-performance concrete have adjust solidifying, reduce hydration heat, degree of mobilization, high-strength, lightweight and high-durability performance, also require that preparation energy consumption is low, cost is low, be suitable for the concrete of rapid construction simultaneously.
In order to meet the requirement of concrete high-performance, need to add admixture adjusted.Admixture can make coagulation head meet various different construction requirement, and there is less investment, instant effect, apply easily, the feature such as technical economic benefit is remarkable.And cement water reducing agent is most widely used in concrete admixture, that usage quantity is maximum one.High-performance water reducing agent is the important materials meeting high performance concrete requirement, due to good plasticity-and excellent application performance, high-efficiency water-reducing agent of poly-carboxylic acid substitutes the condensation polymer type water reducers such as naphthalene system, trimeric cyanamide gradually, in the many important engineerings of China, as in the construction works such as high-speed railway, bridge, airport, water conservancy and hydropower, be widely used.And these engineerings are day by day vigorous to the needs of high performance concrete, this high-performance polycarboxylic acids water reducing agent product just needing performance good, moderate.
The domestic preparation method to polycarboxylate water-reducer mainly contains two kinds at present: the 1. method of first esterification post polymerization, namely first methacrylic acid or vinylformic acid carry out esterification with methoxy poly (ethylene glycol) and form the polymeric monomer being with double bond, then the polymeric monomer with double bond is methacrylic acid or acroleic acid polymerization, obtains High-efficiency polycarboxylic acid water reducer.This method needs first to synthesize polymeric monomer, repolymerization, complicated process of preparation, and cost is high, and esterification is reversible reaction, needs the raw product water of removing in time, reaction just can be made to carry out to the direction producing polymeric monomer, add difficulty and the complexity of reaction.2. direct polymerization method, namely with the ethers of double bond or alcohols macromole and vinylformic acid or maleic anhydride, under the effect of chain-transfer agent and initiator, direct reaction polymerization generates polycarboxylate water-reducer, direct polymerization method generating process is simple, produce without intermediate material, and reaction product polycarboxylate water-reducer being effective, is a kind of method preparing polycarboxylate water-reducer relatively more conventional at present.
Summary of the invention
The object of the present invention is to provide that one is prepared simply, cost is low, diminishing efficiency is high and cement, concrete consistency is good, improves the polycarboxylate water-reducer of concrete flowability, the slump, superpower property, weather resistance etc.The present invention is achieved through the following technical solutions:
A preparation method for polycarboxylate water-reducer, comprises the following steps:
1) under the effect of stirring, in reaction vessel, add methacrylic polyoxyethylene glycol, and add deionized water and make it dissolve;
2) be heated to methacrylic polyoxyethylene glycol while stirring dissolve completely, when temperature reaches 65 ~ 80 DEG C, respectively to dripping acrylamide and the basic sodium sulfonate of dodecane 3 ~ 4.5 hours in reaction vessel, and dripped initiator and chain-transfer agent 4 ~ 6 hours simultaneously;
3) drip rear insulation 4 hours, cool to 35 DEG C, add alkali lye and regulate pH value to 6 ~ 7 to obtain polycarboxylate water-reducer.
Preferred as one, the mass ratio of described methacrylic polyoxyethylene glycol and deionized water is 1:2 ~ 3.
Preferred as one, described methacrylic polyoxyethylene glycol and acrylamide and mass ratio are 1:2 ~ 4.
Preferred as one, the basic sodium sulfonate of described dodecane is 1 ~ 3% of methacrylic polyoxyethylene glycol quality.
Preferred as one, described initiator is ammonium persulphate, and ammonium persulphate is 1 ~ 6% of methacrylic polyoxyethylene glycol quality.
Preferred as one, described chain-transfer agent is Thioglycolic acid, and Thioglycolic acid is 1 ~ 5% of methacrylic polyoxyethylene glycol quality.
Preferred as one, described alkali lye is the sodium hydroxide solution of concentration 35%.
The preparation method of polycarboxylate water-reducer of the present invention has the methacrylic polyoxyethylene glycol polymeric monomer of double bond and acrylamide minor comonomer to react by double bond fragmentation polymerization the water reducer generated under the effect of chain-transfer agent and initiator.In this reaction, the acrylic or methacrylic acid in ordinary method is instead of with acrylamide, because the activity of double bond is higher in vinylformic acid, methacrylic acid, and the double bond activity of methacrylic polyoxyethylene glycol is lower, when both copolyreaction, a large amount of vinylformic acid, methacrylic acid molecules autohemagglutination can be caused, reduce the synthetic ratio of product, add use cost, the water reducer buck impaired performance simultaneously prepared, reduces concrete action effect.The double bond activity of acrylamide is lower, can be better with methacrylic polyoxyethylene glycol double bond generation fragmentation polymerization in reaction process, and acrylamide auto-polymerization not easily occurs reacts.
Could start to drip acrylamide when needing temperature to reach 65 ~ 80 DEG C in reaction, because double bond activity is more weak in methylpropenyl polyoxyethylene glycol, need higher temperature to increase the activity of double bond, provide energy to double bond fracture, be conducive to polyreaction that is follow-up and acrylamide.
Polycarboxylate water-reducer, to the action effect of cement concrete, is not realized by chemical reaction, but by changing the surface adsorption character of coagulating cement soil particle, plays the effect of dispersion diminishing.In preparation method of the present invention, add sodium laurylsulfonate, be the agent of a kind of electronegative anionic surface adsorption activity, it adds the absorption property that can add strength water-reducing agent and cement concrete particle surface.Polycarboxylate water-reducer is joined in cement concrete, and be fully uniformly mixed, at this moment the water reducer molecule added can with concrete generation adsorption, a large amount of polycarboxylate water-reducer molecules can be attached on the surface of concrete particle molecule, because water reducer itself is with electronegative hydrophilic group, so the concrete surface adsorbed by water reducer also can with negative electricity.Adding of sodium laurylsulfonate, as surface adsorption promoting agent on the one hand, the surface adsorption property of strength water-reducing agent to concrete particle can be added, simultaneously because with negative electricity, the negative electricity effect of water reducer can be strengthened, strengthen the negative charge amount on concrete particle surface, surface charge absorption is saturated also faster.Due to identical electrical between concrete particle, according to the principle of two like magnetic poles repel each other, can mutually repel between concrete particle, produce very large mutual repulsive force, cause the adhesion structure between cement granules easily to be destroyed, be scattered in water solvent gradually, increase the flowing property of cement in concrete-agitating, reduce churning time, raise the efficiency, better play the effect of anti.
Ammonium persulphate, as the initiator in preparation process, can be strengthened the fracture of reacting methacrylic polyoxyethylene glycol double bond, improve efficiency of conversion, have soluble in water, low price, initiating activity high.Thioglycolic acid, as the chain-transfer agent of preparation process, can improve molecular weight product and molecular weight distribution, reaches the object improving product performance.
In reaction process, adopting the mode dripped continuously minor comonomer, initiator and chain-transfer agent to be added, its objective is by supplementing minor comonomer and initiator successively, constant with monomer composition in maintenance system, the product multipolymer ratio of components obtained is more homogeneous.Simultaneously, the time for adding of initiator must be greater than the time for adding of polymerization minor comonomer, because, only could there is free crowd and develop in acrylamide minor comonomer under the existence of initiator, be added dropwise to complete if initiator is limited to polymerization single polymerization monomer, remaining acrylamide cannot carry out being polymerized or autohemagglutination occur and affects performance and the quality of product, so the time dripping initiator in this preparation method is greater than the time for adding of acrylamide.
Beneficial effect of the present invention: the present invention adopts acrylamide as reaction monomers, its double bond activity is lower, and autohemagglutination ratio is low, improves the polyreaction with methacrylic polyoxyethylene glycol, decreases raw-material waste, reduce cost.Introduce sodium laurylsulfonate as surface adsorption promoting agent simultaneously, strengthen absorption property and the charge adsorption amount on water reducer and concrete particle surface, improve Particle surface charge saturation efficiency, reduce churning time, increase concrete mobility, preventing adhesiving effect is better.Polycarboxylate water-reducer preparation technology of the present invention is simple, cost is low, diminishing efficiency is high and cement, and concrete consistency is good, effectively can improve concrete mobility, the slump, superpower property and weather resistance.
Embodiment
More intuitively, simply understanding to have technical solution of the present invention and effect, below in conjunction with specific embodiment, explanation detailed complete further being done to the present invention.
Embodiment 1:
Under the effect of stirring, methacrylic polyoxyethylene glycol 10g and 25g deionized water is added in reaction vessel, reacting by heating container also stirs methacrylic polyoxyethylene glycol, when temperature reaches 65 DEG C, acrylamide 30g and the basic sodium sulfonate 0.2g of dodecane is dripped in reaction vessel, time for adding is 3 hours, and drips ammonium persulphate 0.4g and Thioglycolic acid 0.3g simultaneously, and time for adding is 4 hours; Drip rear insulation 4 hours, cool to 35 DEG C, add concentration be 35% sodium hydroxide solution regulate pH value to 6 can obtain polycarboxylate water-reducer.
Embodiment 2:
Under the effect of stirring, methacrylic polyoxyethylene glycol 15g and 35g deionized water is added in reaction vessel, reacting by heating container also stirs methacrylic polyoxyethylene glycol, when temperature reaches 70 DEG C, acrylamide 45g and the basic sodium sulfonate 0.4g of dodecane is dripped in reaction vessel, time for adding is 3.5 hours, and drips ammonium persulphate 0.6g and Thioglycolic acid 0.5g simultaneously, and time for adding is 5 hours; Drip rear insulation 4 hours, cool to 35 DEG C, add concentration be 35% sodium hydroxide solution regulate pH value to 7 can obtain polycarboxylate water-reducer.
Embodiment 3:
Under the effect of stirring, methacrylic polyoxyethylene glycol 20g and 55g deionized water is added in reaction vessel, reacting by heating container also stirs methacrylic polyoxyethylene glycol, when temperature reaches 80 DEG C, acrylamide 60g and the basic sodium sulfonate 0.6g of dodecane is dripped in reaction vessel, time for adding is 4.5 hours, and drips ammonium persulphate 1g and Thioglycolic acid 0.8g simultaneously, and time for adding is 6 hours; Drip rear insulation 4 hours, cool to 35 DEG C, add concentration be 35% sodium hydroxide solution regulate pH value to 7 can obtain polycarboxylate water-reducer.
In order to verify the performance effect of polycarboxylate water-reducer of the present invention to cement, with conventional polycarboxylate water-reducer on the market for simultaneous test, contrast adds quiet slurry degree of mobilization and the slump of cement after water reducer.Test structure is as shown in table 1 below:
As can be seen from table 1 test result, the embodiment of the present invention 1, embodiment 2, the initial paste flowing degree ratio of water reducer water reducer paste flowing degree on the market prepared by embodiment 3, the slump is slightly high, and all slightly decline after 20min, but when 120min, obviously can find out that the flowing degree of net paste of cement and slump reducing amount that add embodiment of the present invention water reducer are at about 20mm, and add the flowing degree of net paste of cement of water reducer on the market and slump reducing amount at about 60mm, illustrate that polycarboxylate water-reducer of the present invention is to the reinforcement cement slump, mobility has good effect.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a preparation method for polycarboxylate water-reducer, is characterized in that, comprises the following steps:
1) under the effect of stirring, in reaction vessel, add methacrylic polyoxyethylene glycol, and add deionized water and make it dissolve;
2) be heated to methacrylic polyoxyethylene glycol while stirring dissolve completely, when temperature reaches 65 ~ 80 DEG C, respectively to dripping acrylamide and the basic sodium sulfonate of dodecane 3 ~ 4.5 hours in reaction vessel, and dripped initiator and chain-transfer agent 4 ~ 6 hours simultaneously;
3) drip rear insulation 4 hours, cool to 35 DEG C, add alkali lye and regulate pH value to 6 ~ 7 to obtain polycarboxylate water-reducer.
2. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, it is characterized in that, the mass ratio of described methacrylic polyoxyethylene glycol and deionized water is 1:2 ~ 3.
3. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, is characterized in that, described methacrylic polyoxyethylene glycol and acrylamide and mass ratio are 1:2 ~ 4.
4. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, it is characterized in that, the basic sodium sulfonate of described dodecane is 1 ~ 3% of methacrylic polyoxyethylene glycol quality.
5. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, it is characterized in that, described initiator is ammonium persulphate, and ammonium persulphate is 1 ~ 6% of methacrylic polyoxyethylene glycol quality.
6. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, it is characterized in that, described chain-transfer agent is Thioglycolic acid, and Thioglycolic acid is 1 ~ 5% of methacrylic polyoxyethylene glycol quality.
7. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, it is characterized in that, described alkali lye is the sodium hydroxide solution of concentration 35%.
8. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, it is characterized in that, described polycarboxylate water-reducer is prepared by the following method: under the effect of stirring, methacrylic polyoxyethylene glycol 10g and 25g deionized water is added in reaction vessel, reacting by heating container also stirs methacrylic polyoxyethylene glycol, when temperature reaches 65 DEG C, acrylamide 30g and the basic sodium sulfonate 0.2g of dodecane is dripped in reaction vessel, time for adding is 3 hours, and dripping ammonium persulphate 0.4g and Thioglycolic acid 0.3g simultaneously, time for adding is 4 hours; Drip rear insulation 4 hours, cool to 35 DEG C, add concentration be 35% sodium hydroxide solution regulate pH value to 6 can obtain polycarboxylate water-reducer.
9. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, it is characterized in that, described polycarboxylate water-reducer is prepared by the following method: under the effect of stirring, methacrylic polyoxyethylene glycol 15g and 35g deionized water is added in reaction vessel, reacting by heating container also stirs methacrylic polyoxyethylene glycol, when temperature reaches 70 DEG C, acrylamide 45g and the basic sodium sulfonate 0.4g of dodecane is dripped in reaction vessel, time for adding is 3.5 hours, and dripping ammonium persulphate 0.6g and Thioglycolic acid 0.5g simultaneously, time for adding is 5 hours; Drip rear insulation 4 hours, cool to 35 DEG C, add concentration be 35% sodium hydroxide solution regulate pH value to 7 can obtain polycarboxylate water-reducer.
10. the preparation method of a kind of polycarboxylate water-reducer as claimed in claim 1, it is characterized in that, described polycarboxylate water-reducer is prepared by the following method: under the effect of stirring, methacrylic polyoxyethylene glycol 20g and 55g deionized water is added in reaction vessel, reacting by heating container also stirs methacrylic polyoxyethylene glycol, when temperature reaches 80 DEG C, acrylamide 60g and the basic sodium sulfonate 0.6g of dodecane is dripped in reaction vessel, time for adding is 4.5 hours, and dripping ammonium persulphate 1g and Thioglycolic acid 0.8g simultaneously, time for adding is 6 hours; Drip rear insulation 4 hours, cool to 35 DEG C, add concentration be 35% sodium hydroxide solution regulate pH value to 7 can obtain polycarboxylate water-reducer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105388946A (en) * | 2015-12-15 | 2016-03-09 | 德阳九鼎智远知识产权运营有限公司 | Intelligent control system and method for concrete early strength agent |
| CN115449023A (en) * | 2021-06-09 | 2022-12-09 | 西南科技大学 | Method for synthesizing polycarboxylate superplasticizer through zinc oxide heterogeneous catalytic ternary copolymerization of 6C polyether macromonomer |
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| CN111234128A (en) * | 2020-01-09 | 2020-06-05 | 昆明承曜建材有限公司 | Efficient preparation method of polycarboxylate superplasticizer |
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Patent Citations (4)
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| CN102516475A (en) * | 2011-12-31 | 2012-06-27 | 上海多纶化工有限公司 | Polycarboxylic concrete water reducer |
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| CN105388946A (en) * | 2015-12-15 | 2016-03-09 | 德阳九鼎智远知识产权运营有限公司 | Intelligent control system and method for concrete early strength agent |
| CN115449023A (en) * | 2021-06-09 | 2022-12-09 | 西南科技大学 | Method for synthesizing polycarboxylate superplasticizer through zinc oxide heterogeneous catalytic ternary copolymerization of 6C polyether macromonomer |
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