CN114249866A - High-efficiency polycarboxylic acid water reducing agent and preparation method and application thereof - Google Patents
High-efficiency polycarboxylic acid water reducing agent and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Abstract
The invention provides a high-efficiency polycarboxylic acid water reducing agent and a preparation method thereof, wherein a low-activity small monomer is added into a reaction bottom material, so that the reaction resistance is increased, and the initial reaction rate is well inhibited; the low-activity small monomer is added into the material A, so that the overall reaction activity of the small monomer acrylic acid in the material A is reduced; a certain amount of low-activity small monomer is added in a timed manner in the reaction process, so that the reaction rate of the whole polymerization reaction process is further ensured to be effectively regulated and controlled. Through the steps, the activity of the monomers in the reaction system is always controlled at a certain level, so that the polymerization reaction is uniformly and continuously carried out, the conversion rate of the synthesis reaction is improved, and the performance of the water reducing agent is improved. Meanwhile, after the reaction process is controlled by the method, the reaction does not need low-temperature (8-12 ℃) to carry out polymerization reaction, so that the reaction rate can be effectively controlled, and the production cost of the water reducing agent is reduced.
Description
Technical Field
The invention belongs to the field of concrete admixture industry, and particularly relates to a high-efficiency polycarboxylic acid water reducing agent, and a preparation method and application thereof.
Background
The EPEG type polyether monomer (ethylene glycol monoethyl polyoxyethylene ether) is used as a novel polyether monomer appearing in recent years, and due to the special molecular structure design, the double-bond electron cloud density is high, the steric hindrance is low, and high reaction activity is shown. When the method is applied to synthesis of the polycarboxylic acid water reducing agent, the polymerization reaction time can be greatly shortened, and the production efficiency of the water reducing agent is improved. Meanwhile, the double bonds in the molecules of the water reducing agent are of a substituted structure, so that the space resistance of swinging of the polyether side chains is reduced, the swinging of the polyether side chains is more flexible, the wrapping property and the winding property of the polyether side chains are improved, and the adaptability and the slump retaining property of the synthesized water reducing agent are better.
Compared with the conventional common polyether monomers HPEG (methyl allyl polyoxyethylene ether), TPEG (isopentenol polyoxyethylene ether) and the like, the EPEG type polyether monomer has obviously higher reaction activity, can obviously shorten the reaction time, and improves the production efficiency of the water reducer. However, in the practical application process, the EPEG type polyether monomer has the reaction activity exceeding the actual requirement of the reaction under the normal temperature condition (about 25 ℃). The EPEG polyether monomer is used for synthesizing the water reducing agent under the normal temperature condition, so that the early reaction speed is too high, the polyether monomer and the acrylic acid can not be reasonably and effectively polymerized, and even the reaction is terminated in advance. Therefore, when the EPEG type polyether monomer is used to synthesize a water-reducing agent, the higher the initial reaction temperature is, the lower the conversion rate is, and the worse the water-reducing agent performance is.
In order to overcome the problems, the prior art generally needs to maintain the reaction system to be carried out under the low-temperature condition so as to reduce the reaction activity of the EPEG type polyether monomer, prevent the too high early rate of the synthesis reaction, lead the reaction to tend to stable and effective homopolymerization, improve the conversion rate of the reaction and improve the performance of the synthesized water reducing agent. It is worth noting that the low temperature condition will undoubtedly increase the production cost of the water reducing agent product, and increase the difficulty of large-scale industrial production of the product. Meanwhile, although the problem that the initial reaction rate of the water reducing agent synthesized by using the EPEG type polyether monomer is too high can be improved to a certain extent under the low-temperature condition, from the monitoring result of the change condition of the conversion rate in the synthesis reaction process, when the dripping time of the water reducing agent synthesized by using the EPEG type polyether monomer under the low-temperature condition reaches more than half, the GPC detection result of the reaction is relatively close to the GPC detection result after the reaction is completed, which indicates that the synthesis reaction may tend to be terminated when the dripping time reaches half, and acrylic acid subsequently entering a reaction system may not effectively participate in the polymerization reaction, so that the problems of high early rate and early termination of the polymerization reaction cannot be well solved under the low-temperature condition.
Disclosure of Invention
The invention aims to provide a high-efficiency polycarboxylic acid water reducing agent and a preparation method thereof.
The invention also aims to provide application of the high-efficiency polycarboxylate superplasticizer in preparing concrete.
The specific technical scheme of the invention is as follows:
a preparation method of a high-efficiency polycarboxylic acid water reducing agent comprises the following steps:
1) putting the polyether monomer into water, stirring until the polyether monomer is completely dissolved, and then sequentially adding the small monomer, the low-activity small monomer, the oxidant, the catalyst and the chain transfer agent;
2) simultaneously dripping the material A and the material B into the base material in the step 1); simultaneously, respectively dripping low-activity small monomers in the 5-10min, 15-20min, 25-30min and 35-45min of the reaction;
3) after the material A and the material B are both dripped, heating the reaction system to 40-50 ℃, preserving the heat for 1.0-1.5 hours, and adjusting the pH of the system to 5-8 to obtain the mother liquor of the high-efficiency polycarboxylic acid water reducing agent.
In the step 1), the method can be carried out under the condition of normal temperature without specially controlling the temperature; preferably, the temperature of the reaction system is 20-25 ℃;
in the step 1), the polyether monomer is ethylene glycol monovinyl polyoxyethylene ether and is selected from EPEG-3000, EPEG-4000, EPEG-5000 or EPEG-6000.
In the step 1), the mass ratio of the polyether monomer to water is 1: 0.6-1.5;
in the step 1), the molar ratio of the polyether monomer to the small monomer is 1: 1-2;
in the step 1), the small monomer is selected from acrylic acid;
in the step 1), the low-activity small monomer is selected from maleic anhydride, hydroxyethyl acrylate and hydroxypropyl acrylate;
the low-activity small monomer in the step 1) is a synthesized substance which can be used for increasing reaction resistance and reducing the reaction activity of the polyether monomer and the small monomer; the mole ratio of the low-activity small monomer to the polyether monomer is 1: 1-4;
in the step 1), the chain transfer agent is thioglycolic acid, and the using amount of the chain transfer agent is 0.30-0.60% of the mass of the polyether monomer;
the catalyst in the step 1) is copper sulfate; the mass ratio of the catalyst to the water in the step 1) is 1-8: 30000.
In the step 1), the oxidant is a hydrogen peroxide aqueous solution with the mass concentration of 30%, and the dosage of the oxidant is 0.8-1.2% of the mass of the polyether monomer.
The preparation method of the material A in the step 2) comprises the following steps: dissolving a mixture of small monomers and a chain transfer agent in water, adding the small monomers with low activity, and stirring the solution to be uniform to be used as a material A;
in the step 2), the molar ratio of the small monomer used in the preparation method of the material A to the polyether monomer in the step 1) is 2-4: 1;
the chain transfer agent used in the preparation method of the material A is thioglycolic acid, and the using amount of the chain transfer agent is 0.4-0.8% of the mass of the polyether monomer in the step 1);
in the preparation method of the material A, the water consumption is 4-6 times of the total mass of the small monomer and the chain transfer agent.
In the preparation method of the material A, the addition amount of the low-activity small monomer is 1-3% of the mass of the polyether monomer in the step 1).
The preparation method of the material B comprises the following steps: taking the water solution of the sodium formaldehyde sulfoxylate mixture as a material B; wherein the dosage of the sodium formaldehyde sulfoxylate mixture is 0.6-1.0% of the mass of the polyether monomer in the step 1).
The preparation method of the aqueous solution of the sodium formaldehyde sulfoxylate mixture comprises the following steps: and dissolving the sodium formaldehyde sulfoxylate mixture in water with the mass of 20-40 times of that of the sodium formaldehyde sulfoxylate mixture to obtain the sodium formaldehyde sulfoxylate-formaldehyde sulfoxylate composite.
The sodium formaldehyde sulfoxylate mixture is the sodium formaldehyde sulfoxylate block.
In the step 2), the dripping time of the material A is controlled to be 1.2-1.5 hours, and the dripping time of the material B is controlled to be 0.25-0.5 hour after the dripping of the material A is finished.
The molar ratio of the amount of the low-activity small monomer added in each time in the step 2) to the polyether monomer in the step 1) is as follows: 1: 2-5.
In the step 3), potassium hydroxide aqueous solution with the mass concentration of 20% is used for adjusting the pH.
The high-efficiency polycarboxylate superplasticizer provided by the invention is prepared by adopting the method.
The invention provides an application of a high-efficiency polycarboxylic acid water reducing agent in preparation of concrete.
According to the invention, the low-activity small monomer is added into the reaction bottom material, so that the reaction resistance is increased, and the initial reaction rate is well inhibited; the low-activity small monomer is added into the material A, so that the overall reaction activity of the small monomer acrylic acid in the material A is reduced; a certain amount of low-activity small monomer is added in a timed manner in the reaction process, so that the reaction rate of the whole polymerization reaction process is further ensured to be effectively regulated and controlled. Through the steps, the activity of the monomers in the reaction system is always controlled at a certain level, so that the polymerization reaction is uniformly and continuously carried out, the conversion rate of the synthesis reaction is improved, and the performance of the water reducing agent is improved. Meanwhile, after the reaction process is controlled by the method, the reaction does not need low-temperature (8-12 ℃) to carry out polymerization reaction, so that the reaction rate can be effectively controlled, and the production cost of the water reducing agent is reduced.
Drawings
FIG. 1 is a GPC chromatogram of product No. U091601 prepared in comparative example 1;
FIG. 2 is a GPC chromatogram of product No. U091602, prepared in comparative example 1;
FIG. 3 is a GPC chromatogram of the product No. U091701 prepared in comparative example 1;
FIG. 4 is a GPC chromatogram of product No. U091702 prepared in comparative example 1;
FIG. 5 is a GPC chromatogram of product No. U091801 prepared in comparative example 1;
FIG. 6 is a GPC chart of the product No. U111701 prepared in example 1;
FIG. 7 is a GPC chart of the product No. U111702 prepared in example 1.
FIG. 8 is a GPC chart of the product No. U111802 prepared in example 2;
FIG. 9 is a GPC chart of the product No. U111902 prepared in example 2.
Detailed Description
Comparative example 1
The preparation method of the water reducer by using the EPEG type polyether monomer and adopting a common process comprises the following steps:
1) 0.1mol of polyether monomer EPEG-3000 is placed in 240g of water and stirred until the EPEG-3000 is completely dissolved, and then 0.15mol of acrylic acid, a 30% hydrogen peroxide aqueous solution with the mass concentration of 0.8% of the mass of the polyether monomer, 20mg of copper sulfate and 0.4% of chain transfer agent thioglycolic acid with the mass of the polyether monomer are sequentially added; the temperature of the reaction system is controlled to be (10 +/-0.5) - (18 +/-0.5) DEG C in the whole process;
2)0.3mol of a mixture of acrylic acid and thioglycolic acid with the mass of 0.6 percent of that of the polyether monomer is dissolved in water with the mass 4 times that of the total mass of the acrylic acid and the thioglycolic acid to be used as material A; dissolving a sodium formaldehyde sulfoxylate mixture accounting for 0.5 percent of the mass of the polyether monomer in water accounting for 30 times of the mass of the sodium formaldehyde sulfoxylate mixture to obtain a material B;
simultaneously dripping the material A and the material B into the base material in the step 1); the dripping time of the material A is controlled to be 1.2 hours, and the dripping time of the material B is controlled to be 1.5 hours after the dripping of the material A is finished;
3) after the material A and the material B are added dropwise, continuously stirring for 1.0 hour, and adjusting the pH of the system to 5-8 by using a potassium hydroxide aqueous solution with the mass concentration of 20% to obtain a polycarboxylic acid water reducer mother liquor.
In the reaction process, the temperature of the reaction system is controlled to be 10 ℃, 12 ℃, 14 ℃, 16 ℃ and 18 ℃ (± 0.5 ℃), and five groups of water reducing agents are synthesized by using a common process (the activity of monomers in the reaction system is regulated and controlled by using low-activity small monomers in the whole reaction system), as shown in the following table 1.
TABLE 1 comparative example 1 product GPC measurement
| Serial number | Numbering | Conversion rate/% | Raw material/%) | Mn | Mw | Mw/Mn | Reaction temperature/. |
| 1 | U091601 | 85.19 | 5.40 | 47869 | 69157 | 1.4447 | 10(±0.5) |
| 2 | U091602 | 84.57 | 6.02 | 48414 | 70121 | 1.4484 | 12(±0.5) |
| 3 | U091701 | 84.30 | 6.39 | 48855 | 70924 | 1.4517 | 14(±0.5) |
| 4 | U091702 | 83.57 | 7.29 | 48715 | 70933 | 1.4561 | 16(±0.5) |
| 5 | U091801 | 83.04 | 8.15 | 48368 | 70897 | 1.4658 | 18(±0.5) |
As can be seen from the above table, the conversion rate of the synthesized water reducing agent is gradually reduced along with the increase of the temperature of the reaction system, which indicates that the synthesis of the water reducing agent by using the EPEG type polyether monomer is suitable for being carried out under the low-temperature condition. The relative GPC measurement maps are shown in FIGS. 1 to 5.
And (3) synthesizing the water reducing agent of the comparative example 1 at different temperatures for comparative evaluation of the performance of the cement paste: the water cement ratio is 0.29, 300g of PO42.5 conch cement, 10 percent of solid content of water reducing agent and 0.14 percent of folded solid content.
TABLE 2 evaluation test of fluidity of cement paste
As can be seen from the table above, the performance of the water reducing agent synthesized by using the EPEG type polyether monomer is poorer along with the increase of the reaction temperature, so that the water reducing agent produced according to the common process needs to be controlled at a lower temperature of below 12 ℃, and the production cost is high.
Example 1
A preparation method of a high-efficiency polycarboxylic acid water reducing agent comprises the following steps:
1) 0.1mol of polyether monomer EPEG-3000 (ethylene glycol monoethyl polyoxyethylene ether) is placed in 200g of water and stirred until being completely dissolved, 0.12mol of acrylic acid, 0.08mol of low-activity small monomer maleic anhydride, 30 mass percent hydrogen peroxide aqueous solution with the mass concentration of 0.9 mass percent of polyether monomer, 20mg of copper sulfate and 0.3 mass percent thioglycolic acid of polyether monomer are sequentially added, the reaction temperature of the system does not need to be operated and controlled, and the reaction system is at the temperature of 20-25 ℃ and is close to the normal temperature.
2) And the material A is a mixture of 0.25mol of acrylic acid and thioglycolic acid accounting for 0.45 percent of the mass of the polyether monomer, the mixture is dissolved in water 4 times of the total mass of the acrylic acid and the thioglycolic acid, and finally low-activity small monomer maleic anhydride accounting for 1.5 percent of the mass of the polyether monomer is added, and the solution is stirred uniformly to obtain the material A.
3) The B material is sodium formaldehyde sulfoxylate mixture which accounts for 0.6 percent of the mass of the used polyether monomer and is dissolved in water with the mass of 25 times of the mass of the sodium formaldehyde sulfoxylate mixture.
4) During synthesis, the material A and the material B are simultaneously dripped, the dripping time of the material A is controlled to be 1.2 hours, the dripping time of the material B is controlled to be 0.5 hour after the dripping of the material A is finished, and 0.05mol, 0.04mol, 0.03mol and 0.02mol of low-activity small monomers are directly added into a reaction system respectively at 10min, 20min, 30min and 40min of the reaction, so that the reaction rate is controlled.
5) A, B, heating the reaction system to 40 ℃ after the dropwise addition is finished, keeping the temperature for 1.0 hour, and adjusting the pH of the system to 5-8 by using 20% potassium hydroxide solution to obtain a polycarboxylate superplasticizer sample with efficient water reducing and slump retaining effects.
The 2 samples, numbered U111701 and U111702, produced by the same process as in example 1 were compared with the water reducing agent No. U091601 product synthesized by the conventional process, and the results are shown in Table 3.
Table 3 comparison of GPC measurement performance of the product of example 1 with that of the product of comparative document 1
As can be seen from the table above, the water reducing agent synthesized by the improved process under the normal temperature condition has the same conversion rate as the water reducing agent synthesized by the common process under the low temperature condition, the temperature of the system does not need to be controlled and reduced, and the experimental repeatability of the improved process is better.
The water reducing agent synthesized by the improved process under the normal temperature condition and the water reducing agent synthesized by the common process under the low temperature condition are used for carrying out comparative evaluation on the cement paste performance: the water cement ratio is 0.29, 300g of PO42.5 conch cement, 10 percent of solid content of water reducing agent and 0.14 percent of folded solid content. The results are shown in Table 4.
TABLE 4 evaluation test of fluidity of cement paste
As can be seen from the table below, the water reducing agent synthesized by the improved process under normal temperature condition has obviously better performance than the water reducing agent synthesized by the common process under low temperature condition.
And (3) evaluating the performance of the cement paste with a commercial water reducing agent: the water cement ratio is 0.29, 300g of PO42.5 conch cement, 10 percent of solid content of water reducing agent and 0.12 percent of folded solid content. The results are shown in Table 5.
TABLE 5 Water reducing agent Cement paste Properties
The initial water reducing rate of the synthesized water reducing agent is highest, the fluidity of the synthesized water reducing agent is increased by 6mm after 1 hour, the fluidity of the synthesized water reducing agent is increased by 1mm after 2 hours, and the water reducing and slump retaining effects of the synthesized water reducing agent are obviously superior to those of the water reducing agent sold in the market.
The concrete performance evaluation was carried out with a commercially available water reducing agent, and the PO42.5 conch cement had a solid content of 10% and a folded solid content of 0.21%, and the concrete mix ratio and test results are shown in Table 6 below.
As can be seen from the table above, the water reducing agent synthesized by the improved process under normal temperature condition has better performance than the water reducing agent synthesized by the common process under low temperature condition, and is also better than the water reducing agent sold in the market.
Example 2
A preparation method of a high-efficiency polycarboxylic acid water reducing agent comprises the following steps:
1) 0.1mol of polyether monomer EPEG-6000 (ethylene glycol monoethyl polyoxyethylene ether) is placed in 800g of water and stirred until being completely dissolved, 0.18mol of acrylic acid is sequentially added, 0.03mol of low-activity small monomer hydroxyethyl acrylate is added, 30% hydrogen peroxide aqueous solution with the mass concentration of 1.15% of the mass of the polyether monomer, 140mg of copper sulfate and 0.3% of mercaptoacetic acid with the mass of the polyether monomer are added, and the reaction system does not need to be operated and controlled at the temperature of 20-25 ℃ and close to the normal temperature.
2) And (2) dissolving a mixture of 0.35mol of acrylic acid as a material A and 0.75% of thioglycolic acid in mass of the polyether monomer in the step 1) in water 6 times of the total mass of the acrylic acid and the thioglycolic acid, finally adding a small low-activity monomer hydroxyethyl acrylate in mass of 2.5% of the polyether monomer, and stirring the solution uniformly to obtain the material A.
3) The material B is a sodium formaldehyde sulfoxylate mixture which accounts for 0.9 percent of the mass of the polyether monomer in the step 1) and is dissolved in water accounting for 35 times of the mass of the sodium formaldehyde sulfoxylate mixture.
4) During synthesis, the material A and the material B are simultaneously dripped, the dripping time of the material A is controlled to be 1.5 hours, the dripping time of the material B is controlled to be 0.5 hour after the dripping of the material A is finished, and 0.04mol, 0.03mol, 0.02mol and 0.02mol of low-activity small monomers are directly added into a reaction system respectively at 10min, 20min, 30min and 40min of the reaction to control the reaction rate.
5) A, B, after the dropwise addition, heating the reaction system to 50 ℃, keeping the temperature for 1.25 hours, and adjusting the pH of the system to 5-8 by using 20% potassium hydroxide solution to obtain a polycarboxylate superplasticizer sample with high-efficiency water reducing and slump retaining effects.
2 samples of example 2, numbered U111802 and U111902, respectively, were produced by the same process and compared with the water reducing agent synthesized by the conventional process, and the results are shown in Table 7.
TABLE 7 comparison of GPC measurement Performance of the product of example 1 with that of the product of comparative document 1
As can be seen from the table above, the water reducing agent synthesized by the improved process under the normal temperature condition has the same conversion rate as the water reducing agent synthesized by the common process under the low temperature condition, and the experimental repeatability of the improved process is better.
The water reducing agent synthesized by the improved process under the normal temperature condition and the water reducing agent synthesized by the common process under the low temperature condition are used for carrying out comparative evaluation on the cement paste performance: the water cement ratio is 0.29, 300g of PO42.5 conch cement, 10 percent of solid content of water reducing agent and 0.14 percent of folded solid content. The results are shown in Table 8.
TABLE 8 evaluation test for fluidity of cement paste
As can be seen from the table below, the water reducing agent synthesized by the improved process under normal temperature condition has obviously better performance than the water reducing agent synthesized by the common process under low temperature condition.
And (3) evaluating the performance of the cement paste with a commercial water reducing agent: the water cement ratio is 0.29, 300g of PO42.5 conch cement, 10 percent of solid content of water reducing agent and 0.12 percent of folded solid content. The results are shown in Table 9.
TABLE 9 Water reducing agent Cement paste Properties
The initial water reducing rate of the synthesized water reducing agent is highest, the fluidity of the synthesized water reducing agent is increased by 3mm after 1 hour, the fluidity of the synthesized water reducing agent is increased by 1mm after 2 hours, and the water reducing and slump retaining effects of the synthesized water reducing agent are obviously superior to those of the water reducing agent sold in the market.
The concrete performance evaluation was carried out with a commercially available water reducing agent, PO42.5 conch cement, water reducing agent solid content 10%, the folded solid content 0.22%, concrete mix proportion and test results are shown in the following table.
As can be seen from the table above, the water reducing agent synthesized by the improved process under normal temperature condition has better performance than the water reducing agent synthesized by the common process under low temperature condition, and is also better than the water reducing agent sold in the market.
Claims (10)
1. The preparation method of the high-efficiency polycarboxylic acid water reducing agent is characterized by comprising the following steps:
1) putting the polyether monomer into water, stirring until the polyether monomer is completely dissolved, and then sequentially adding the small monomer, the low-activity small monomer, the oxidant, the catalyst and the chain transfer agent;
2) simultaneously dripping the material A and the material B into the base material in the step 1); simultaneously, respectively dripping low-activity small monomers in the 5-10min, 15-20min, 25-30min and 35-45min of the reaction;
3) after the material A and the material B are both dripped, heating the reaction system to 40-50 ℃, preserving the heat for 1.0-1.5 hours, and adjusting the pH of the system to 5-8 to obtain the mother liquor of the high-efficiency polycarboxylic acid water reducing agent.
2. The production method according to claim 1, wherein in the step 1), the temperature of the reaction system is 20 to 25 ℃.
3. The production method according to claim 1 or 2, characterized in that, in step 1), the polyether monomer is ethylene glycol monovinyl polyoxyethylene ether.
4. The preparation method according to claim 1, wherein in step 1), the molar ratio of the polyether monomer to the small monomer is 1: 1-2; the small monomer is acrylic acid.
5. The preparation method of claim 1, wherein the molar ratio of the low-activity small monomer to the polyether monomer in the step 1) is 1: 1-4.
6. The method according to claim 1, wherein the molar ratio of the amount of the low-activity small monomer added in each time in the step 2) to the polyether monomer in the step 1) is: 1: 2-5.
7. The method according to claim 1 or 4, wherein the method for preparing A in step 2) is: dissolving the mixture of the small monomer and the chain transfer agent in water, adding the small monomer with low activity, and stirring the solution to be uniform to be used as material A.
8. The preparation method of claim 7, wherein the molar ratio of the small monomers used in the preparation method of the material A to the polyether monomers in the step 1) is 2-4: 1.
9. a high-efficiency polycarboxylic acid water reducing agent prepared by the preparation method of any one of claims 1 to 8.
10. The application of the high-efficiency polycarboxylic acid water reducer prepared by the preparation method of any one of claims 1 to 8, which is characterized by being used for concrete.
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| CN109293271A (en) * | 2018-09-28 | 2019-02-01 | 上海东大化学有限公司 | A kind of high-adaptability poly carboxylic acid series water reducer and its preparation and application |
| CN109627401A (en) * | 2018-12-04 | 2019-04-16 | 山西佳维新材料股份有限公司 | A kind of preparation method of polyethers synthesis collapse protective poly-carboxylic acid water reducing agent |
| CN109651568A (en) * | 2019-01-08 | 2019-04-19 | 山西佳维新材料股份有限公司 | A kind of preparation method of novel polyether synthesis sustained-release polycarboxylic water reducer |
| CN109705282A (en) * | 2019-01-08 | 2019-05-03 | 山西佳维新材料股份有限公司 | A kind of preparation method of novel polyether synthesis superelevation water reducing type polycarboxylate water-reducer |
| CN111607039A (en) * | 2019-09-11 | 2020-09-01 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Slow-release high slump loss resistant polycarboxylic acid concrete water reducer and preparation method thereof |
| CN111995717A (en) * | 2020-08-20 | 2020-11-27 | 安徽海螺新材料科技有限公司 | High-performance polycarboxylate superplasticizer, preparation method thereof and concrete |
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