CN116333228A - Synthesis method of polycarboxylic acid high-performance water reducer under low temperature condition - Google Patents
Synthesis method of polycarboxylic acid high-performance water reducer under low temperature condition Download PDFInfo
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- CN116333228A CN116333228A CN202310252525.3A CN202310252525A CN116333228A CN 116333228 A CN116333228 A CN 116333228A CN 202310252525 A CN202310252525 A CN 202310252525A CN 116333228 A CN116333228 A CN 116333228A
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention belongs to the technical field of high polymer materials and concrete additives, and discloses a synthesis method of a polycarboxylic acid high-performance water reducer under a low temperature condition. The synthesis method comprises the following steps: adding unsaturated polyoxyethylene ether and water into a reactor, stirring and dissolving uniformly to obtain a base material; adding unsaturated carboxylic acid, a vinyl silane coupling agent, a crosslinking monomer and an oxidant into water, and stirring and dissolving uniformly to obtain a material A; adding a chain transfer agent and a reducing agent into water, and uniformly stirring and dissolving to obtain a material B; and (3) simultaneously dripping the material A and the material B into the base material, reacting at the temperature of 5-40 ℃, and adding alkali to neutralize after the reaction is finished to obtain the polycarboxylic acid high-performance water reducer. The synthesis method can react at low temperature and room temperature (5-40 ℃) to obtain the high-performance polycarboxylate superplasticizer with good dispersibility and slump retention.
Description
Technical Field
The invention belongs to the technical field of high polymer materials and concrete additives, and particularly relates to a synthesis method of a polycarboxylic acid high-performance water reducer under a low temperature condition.
Background
The polycarboxylate water reducer is a copolymer with a comb structure, and is mainly prepared by the free radical copolymerization of unsaturated polyoxyethylene ether, unsaturated carboxylic acid and other unsaturated monomers. The polycarboxylic acid water reducer has high water reducing rate and slump retaining capacity, and is widely applied to building engineering. At present, most of the synthesis of the polycarboxylate superplasticizer is to heat the polycarboxylate superplasticizer into a system, the reaction temperature is controlled at 60-80 ℃, and the initiator is promoted to decompose to generate free radicals by heating, so that the technology has high energy consumption and high equipment maintenance cost. The main methods for synthesizing the polycarboxylate superplasticizer by heating are 3: copolymerization synthesis, functionalization method, in-situ polymerization and grafting. The main method of normal-temperature synthesis is copolymerization synthesis, free radicals are generated through oxidation-reduction reaction, and the selection range of the types of the relative polymerizable monomers of the polycarboxylic acid water reducer synthesized at normal temperature is supposed to be far smaller than the selection of the raw materials of the polycarboxylic acid water reducer synthesized by heating, so that the corresponding performance improvement space cannot be compared with that of the polycarboxylic acid water reducer synthesized by heating.
If the polymerization process can be improved, the reaction can save the investment of a heating source and a cooling water circulation system at low temperature and room temperature (5-30 ℃), meanwhile, the process is simplified, the production period is shortened, the production cost is reduced, and the economic benefit is improved.
For example, CN 104177557A adopts a redox system initiation system with low activation energy, so that the reactivity is improved, and the dispersibility and dispersibility retention capability of the product and the adaptability to a cementing material are improved by introducing carboxylate, sulfonate and phosphonate groups. The patent CN 104558435A adopts an initiator and a reducer of a low-temperature polymerization initiation system, and takes unsaturated polyoxyethylene ether, unsaturated carboxylic acid and unsaturated quaternary ammonium salt monomers as raw materials to synthesize the multi-branched polycarboxylic acid water reducer with high water reduction, high slump loss resistance and strong adaptability. The patent CN 106749957A is compounded by a multi-element initiator, and under the alternate combined action of the oxidant and the strong and weak reducing agent, the conversion rate of the product is greatly improved; the molecular mass distribution of the polycarboxylate water reducer is controlled by the dripping time, the initiator adding mode and the synthesis temperature, so that the water reducing rate and the slump retaining property are improved. The patent CN 114316158A adopts a redox system formed by a composite initiator to play a good role in activating and catalyzing polymerization reaction, and can perform stable and uniform reaction within the range of 0-40 ℃ without heat source supply, so that the polycarboxylate water reducer with good product performance is prepared.
According to the prior art, the reaction activity can be improved and the reaction temperature can be reduced by changing the initiation system; the key to improving the performance of the polycarboxylic acid high-performance water reducer under the low temperature condition is to develop a functional monomer capable of copolymerizing under the low temperature condition.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the primary purpose of the invention is to provide a synthesis method of a polycarboxylic acid high-performance water reducer under a low temperature condition.
The invention also aims to provide the polycarboxylic acid high-performance water reducer prepared by the method.
The invention aims at realizing the following technical scheme:
a method for synthesizing a polycarboxylic acid high-performance water reducer under a low temperature condition comprises the following steps:
(1) Adding unsaturated polyoxyethylene ether and water into a reactor, stirring and dissolving uniformly to obtain a base material;
(2) Adding unsaturated carboxylic acid, a vinyl silane coupling agent, a crosslinking monomer and an oxidant into water, and stirring and dissolving uniformly to obtain a material A;
(3) Adding a chain transfer agent and a reducing agent into water, and uniformly stirring and dissolving to obtain a material B;
(4) And (3) simultaneously dripping the material A and the material B into the base material in the step (1), reacting at the temperature of 5-40 ℃, and adding alkali for neutralization after the reaction is finished to obtain the polycarboxylic acid high-performance water reducer.
Further, the unsaturated polyoxyethylene ether in the step (1) is at least one of allyl polyoxyethylene ether, methallyl polyoxyethylene ether, isopentenyl polyoxyethylene ether and isobutenyl ether polyoxyethylene ether.
Further, the mass concentration of the primer in the step (1) is 30% -60%.
Further, the unsaturated carboxylic acid in the step (2) is at least one of acrylic acid, methacrylic acid, methyl acrylate, ethyl acrylate, maleic acid or itaconic acid.
Further, the vinyl silane coupling agent in the step (2) is at least one of methacryloxypropyl trimethoxysilane, vinyl triethoxysilane, allyl trimethoxysilane and allyl triethoxysilane.
According to the invention, the vinyl silane coupling agent is adopted for copolymerization, so that the anchoring capability of the polycarboxylic acid water reducer on the surface of cement particles can be improved, and the dispersion slump retaining effect of the polycarboxylic acid water reducer is improved.
Further, in the step (2), the crosslinking monomer is ethylene glycol dimethacrylate, polyethylene glycol dimethacrylate or unsaturated polyoxyethylene ether grafted cyclosiloxane. More preferably, the cyclic siloxane grafted by unsaturated polyoxyethylene ether is prepared by the following method:
adding tetramethyl cyclotetrasiloxane (D4H) and unsaturated polyoxyethylene ether into an organic solvent according to a molar ratio of 1:3-4, stirring and dissolving uniformly, heating to 70-90 ℃, adding an organotin catalyst for reaction for 1-6H, and vacuum drying to remove the solvent to obtain unsaturated polyoxyethylene ether grafted cyclosiloxane.
The crosslinking monomer can realize partial crosslinking in the polymerization process, so that the steric hindrance effect of the system is increased, and particularly, the effect of the unsaturated polyoxyethylene ether grafted cyclosiloxane crosslinking monomer is more remarkable, so that the dispersion slump retention of polycarboxylic acid is improved; meanwhile, under the alkaline condition in the application process, the ester bond or the silicon ether bond of the crosslinking monomer is partially hydrolyzed to release more polycarboxylic acid molecules, so that the dispersion performance is obviously improved. In addition, the unsaturated polyoxyethylene ether grafted cyclosiloxane crosslinking monomer also has the function of enhancing the compatibility of the vinyl silane coupling agent, and the copolymerization efficiency between the unsaturated polyoxyethylene ether grafted cyclosiloxane crosslinking monomer and unsaturated carboxylic acid under the low-temperature condition is obviously improved. Meanwhile, the unsaturated polyoxyethylene ether grafted cyclosiloxane has more crosslinking sites (3-4 functionalities), and the vinyl active end is fully stretched and less entangled due to the steric hindrance of the cyclosiloxane, so that the crosslinking activity is obviously enhanced, and the low-temperature (5-40 ℃) crosslinking under the condition of no heating can be realized.
Further, the molar ratio of the addition amount of the unsaturated carboxylic acid to the unsaturated polyoxyethylene ether in the step (2) is 2-5:1; the molar ratio of the addition amount of the vinyl silane coupling agent to the unsaturated carboxylic acid is 0.01-0.2:1; the addition amount of the crosslinking monomer is 0.5-10% of the mass of unsaturated carboxylic acid.
Further, in the step (2), the oxidant is at least one of hydrogen peroxide, sodium persulfate, potassium persulfate and ammonium persulfate.
Further, the chain transfer agent in the step (3) is one of thioglycollic acid or mercaptopropionic acid.
Further, in the step (3), the reducing agent is one of ascorbic acid, sodium sulfite or sodium bisulfite.
Further, the dripping time in the step (4) is 2-4 hours, and the reaction is continued for 1-4 hours after the dripping is completed.
Further, in the step (4), the alkali is sodium hydroxide solution.
The polycarboxylic acid high-performance water reducer is prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
(1) The synthesis method adopts a redox system initiation system with low activation energy, improves the reactivity, and can react at low temperature and room temperature (5-40 ℃) to obtain the high-performance polycarboxylate water reducer.
(2) According to the invention, the vinyl silane coupling agent comonomer is introduced into the molecules of the polycarboxylate superplasticizer, so that the anchoring capability of the polycarboxylate superplasticizer on the surfaces of cement particles is improved, and the dispersion slump retaining effect of the polycarboxylate superplasticizer is improved.
(3) The invention adopts the specific crosslinking monomer to improve the copolymerization efficiency of the vinyl silane coupling agent under the low-temperature condition, and further improves the dispersion slump retaining effect of the polycarboxylate water reducer.
(4) The invention adopts the specific crosslinking monomer to realize partial crosslinking, increases the steric hindrance effect of the system, has more crosslinking sites and strong crosslinking activity, can realize low-temperature (5-40 ℃) crosslinking under the condition of no heating, and improves the dispersion slump retaining effect of the polycarboxylate water reducer.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
Example 1
The synthesis method of the polycarboxylic acid high-performance water reducer under the low-temperature condition comprises the following steps:
(1) 500g of allyl polyoxyethylene ether APEG-2400 and 700mL of water are added into a reactor, stirred and dissolved uniformly, and a bottom material is obtained.
(2) 60g of acrylic acid, 10g of methacryloxypropyl trimethoxysilane, 2g of cross-linking monomer polyethylene glycol dimethacrylate (PEG-400 DMA) and 1g of oxidant potassium persulfate are added into 100ml of water, and stirred and dissolved uniformly to obtain a material A.
(3) 2g of chain transfer agent thioglycollic acid and 1g of reducing agent sodium bisulphite are added into 20ml of water, and evenly stirred and dissolved to obtain material B.
(4) And (3) simultaneously dripping the material A and the material B into the base material in the step (1), and reacting at normal temperature (25-30 ℃), wherein the dripping time of the material A is 3h, the dripping time of the material B is 1h, and continuing to react for 2h after the dripping is finished. And adding sodium hydroxide solution to neutralize after the reaction is finished, thus obtaining the polycarboxylic acid high-performance water reducer.
Example 2
The synthesis method of the polycarboxylic acid high-performance water reducer under the low-temperature condition comprises the following steps:
(1) 500g of isopentenol polyoxyethylene ether TPEG-2400 and 600mL of water are added into a reactor, stirred and dissolved uniformly, and a bottom material is obtained.
(2) 60g of acrylic acid, 8g of vinyl triethoxysilane, 1g of crosslinking monomer ethylene glycol dimethacrylate and 1g of oxidant potassium persulfate are added into 100ml of water, and stirred and dissolved uniformly to obtain a material A.
(3) 2g of chain transfer agent thioglycollic acid and 1g of reducing agent sodium bisulphite are added into 20ml of water, and evenly stirred and dissolved to obtain material B.
(4) And (3) simultaneously dripping the material A and the material B into the base material in the step (1), and reacting at normal temperature (25-30 ℃), wherein the dripping time of the material A is 3h, the dripping time of the material B is 1h, and continuing to react for 2h after the dripping is finished. And adding sodium hydroxide solution to neutralize after the reaction is finished, thus obtaining the polycarboxylic acid high-performance water reducer.
Example 3
Compared with the method in the embodiment 1, the synthetic method of the polycarboxylic acid high-performance water reducer adopts the unsaturated polyoxyethylene ether grafted cyclosiloxane with equal mass to replace the crosslinking monomer PEG-400DMA, and the rest is the same, and comprises the following steps:
(1) 500g of allyl polyoxyethylene ether APEG-2400 and 700mL of water are added into a reactor, stirred and dissolved uniformly, and a bottom material is obtained.
(2) 60g of acrylic acid, 10g of methacryloxypropyl trimethoxysilane, 2g of cyclosiloxane APEG-D4 grafted by unsaturated polyoxyethylene ether as a crosslinking monomer and 1g of potassium persulfate as an oxidant are added into 100ml of water, and stirred and dissolved uniformly to obtain a material A.
(3) 2g of chain transfer agent thioglycollic acid and 1g of reducing agent sodium bisulphite are added into 20ml of water, and evenly stirred and dissolved to obtain material B.
(4) And (3) simultaneously dripping the material A and the material B into the base material in the step (1), and reacting at normal temperature (25-30 ℃), wherein the dripping time of the material A is 3h, the dripping time of the material B is 1h, and continuing to react for 2h after the dripping is finished. And adding sodium hydroxide solution to neutralize after the reaction is finished, thus obtaining the polycarboxylic acid high-performance water reducer.
The unsaturated polyoxyethylene ether grafted cyclosiloxane APEG-D4 is prepared by the following method:
adding tetramethyl cyclotetrasiloxane D4H and allyl polyoxyethylene ether APEG-1000 into isopropanol solvent according to a molar ratio of 1:4, stirring and dissolving uniformly, heating to 75-80 ℃, adding dibutyl tin dilaurate catalyst for condensation reaction for 4H, and vacuum drying to remove the solvent to obtain unsaturated polyoxyethylene ether grafted cyclosiloxane APEG-D4.
Comparative example 1
This comparative example was compared to example 1, with the remainder being the same, without the addition of methacryloxypropyl trimethoxysilane as comonomer.
Comparative example 2
This comparative example was compared to example 3, with the remainder being the same, without the addition of methacryloxypropyl trimethoxysilane as comonomer.
Comparative example 3
In this comparative example, no crosslinking monomer APEG-D4 was added, as compared to example 3, the remainder being the same.
The polycarboxylic acid high-performance water reducer obtained in the above examples and comparative examples were tested for water reduction rate, initial fluidity of cement paste, fluidity with time and 1h slump loss, respectively (GB/8076-2008, cement used in the experiment was P.O42.5 standard cement, and the water reducer fold-solid mixing amount was 0.25%). The test results are shown in table 1 below.
TABLE 1
Rate of water reduction | Initial flowability | Flow over time | Slump loss of 1h | |
Example 1 | 30% | 238mm | 216mm | 41mm |
Example 2 | 32% | 245mm | 220mm | 36mm |
Example 3 | 37% | 258mm | 244mm | 22mm |
Comparative example 1 | 26% | 229mm | 202mm | 45mm |
Comparative example 2 | 22% | 205mm | 200mm | 30mm |
Comparative example 3 | 27% | 232mm | 189mm | 48mm |
As can be seen from the comparison results of examples 1 and examples 3 and 2 in Table 1, by adding methacryloxypropyl trimethoxysilane as a comonomer, the anchoring effect of the water reducing agent molecule to cement particles can be improved, and the dispersing ability can be improved, thereby improving the water reducing rate, fluidity and slump loss to some extent. As can be seen from the comparison of comparative examples 1 and 2, the APEG-D4 crosslinking alone has a somewhat reduced water reduction rate and flowability, while the slump retaining properties are significantly improved, compared to the PEG-400DMA crosslinking alone. As can be seen from the comparison of the results of the examples 1 and 3, the copolymerization of the vinyl silane coupling agent and the crosslinking combination of the APEG-D4 are adopted, compared with the copolymerization of the vinyl silane coupling agent and the crosslinking combination of the PEG-400DMA, the water reducing rate, the fluidity and the slump retaining performance are obviously improved, and the obvious synergistic effect is generated by the copolymerization of the vinyl silane coupling agent and the crosslinking combination of the APEG-D4, because the APEG-D4 can improve the compatibility of the vinyl silane coupling agent in a copolymerization system and enhance the reactivity of the vinyl silane coupling agent, thereby improving the copolymerization grafting efficiency of the vinyl silane coupling agent under the low-temperature condition. The comparison results of the example 3 and the comparative example 3 further prove that the copolymerization of the vinyl silane coupling agent and the crosslinking combination of the APEG-D4 can obviously improve the water reducing rate, the fluidity and the slump retaining performance of the polycarboxylate water reducer.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The synthesis method of the polycarboxylic acid high-performance water reducer under the low temperature condition is characterized by comprising the following steps of:
(1) Adding unsaturated polyoxyethylene ether and water into a reactor, stirring and dissolving uniformly to obtain a base material;
(2) Adding unsaturated carboxylic acid, a vinyl silane coupling agent, a crosslinking monomer and an oxidant into water, and stirring and dissolving uniformly to obtain a material A;
(3) Adding a chain transfer agent and a reducing agent into water, and uniformly stirring and dissolving to obtain a material B;
(4) And (3) simultaneously dripping the material A and the material B into the base material in the step (1), reacting at the temperature of 5-40 ℃, and adding alkali for neutralization after the reaction is finished to obtain the polycarboxylic acid high-performance water reducer.
2. The method for synthesizing the polycarboxylic acid high-performance water reducer at low temperature according to claim 1, wherein the unsaturated polyoxyethylene ether in the step (1) is at least one of allyl polyoxyethylene ether, methallyl polyoxyethylene ether, isopentenyl polyoxyethylene ether and isobutenyl ether polyoxyethylene ether; the mass concentration of the bottom material is 30% -60%.
3. The method for synthesizing a high-performance water reducing agent of polycarboxylic acid at low temperature according to claim 1, wherein the unsaturated carboxylic acid in the step (2) is at least one of acrylic acid, methacrylic acid, methyl acrylate, ethyl acrylate, maleic acid or itaconic acid.
4. The method for synthesizing the high-performance water reducer of the polycarboxylic acid under the low-temperature condition according to claim 1, wherein the vinyl silane coupling agent in the step (2) is at least one of methacryloxypropyl trimethoxysilane, vinyl triethoxysilane, allyl trimethoxysilane and allyl triethoxysilane.
5. The method for synthesizing the polycarboxylic acid high-performance water reducer at low temperature according to claim 1, wherein the crosslinking monomer in the step (2) is ethylene glycol dimethacrylate, polyethylene glycol dimethacrylate or unsaturated polyoxyethylene ether grafted cyclosiloxane.
6. The method for synthesizing the polycarboxylic acid high-performance water reducer at low temperature according to claim 5, wherein the crosslinking monomer is unsaturated polyoxyethylene ether grafted cyclosiloxane, and the method is characterized in that the method comprises the following steps:
adding tetramethyl cyclotetrasiloxane and unsaturated polyoxyethylene ether into an organic solvent according to a molar ratio of 1:3-4, stirring and dissolving uniformly, heating to 70-90 ℃, adding an organotin catalyst for reaction for 1-6 h, and vacuum drying to remove the solvent to obtain unsaturated polyoxyethylene ether grafted cyclosiloxane.
7. The method for synthesizing the polycarboxylic acid high-performance water reducer at low temperature according to claim 1, wherein the molar ratio of the addition amount of the unsaturated carboxylic acid to the unsaturated polyoxyethylene ether in the step (2) is 2-5:1; the molar ratio of the addition amount of the vinyl silane coupling agent to the unsaturated carboxylic acid is 0.01-0.2:1; the addition amount of the crosslinking monomer is 0.5-10% of the mass of unsaturated carboxylic acid.
8. The method for synthesizing the high-performance water reducer of the polycarboxylic acid under the low-temperature condition according to claim 1, wherein the oxidant in the step (2) is at least one of hydrogen peroxide, sodium persulfate, potassium persulfate and ammonium persulfate; the chain transfer agent in the step (3) is one of thioglycollic acid or mercaptopropionic acid, and the reducing agent is one of ascorbic acid, sodium sulfite or sodium bisulfite.
9. The method for synthesizing the high-performance water reducer of the polycarboxylic acid under the low-temperature condition according to claim 1, wherein the dropwise adding time in the step (4) is 2-4 h, the reaction is continued for 1-4 h after the dropwise adding is finished, and the alkali is sodium hydroxide solution.
10. A polycarboxylic acid high performance water reducing agent, characterized in that it is prepared by the method of any one of claims 1 to 9.
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