CN114369208B - Preparation method and application of mud-resistant high-adsorption water-reducing polycarboxylate superplasticizer - Google Patents

Preparation method and application of mud-resistant high-adsorption water-reducing polycarboxylate superplasticizer Download PDF

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CN114369208B
CN114369208B CN202111645559.6A CN202111645559A CN114369208B CN 114369208 B CN114369208 B CN 114369208B CN 202111645559 A CN202111645559 A CN 202111645559A CN 114369208 B CN114369208 B CN 114369208B
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aniline
water
parts
reducing
preparing
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CN114369208A (en
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陈展华
方云辉
饶帮礼
肖悦
柯余良
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Leizhi Chemical Fujian Co ltd
Kezhijie New Material Group Co Ltd
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Kezhijie New Material Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/26Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2605Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2618Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
    • C08G65/2621Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
    • C08G65/2627Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing aromatic or arylaliphatic amine groups
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention provides a preparation method and application of an anti-mud high-adsorption water-reducing polycarboxylate water reducer. The preparation method of the water reducer comprises the following steps: step 1, preparing an aniline ether intermediate from a substituted vinyl ether compound and aniline under the action of an initiator; step 2, polymerizing the aniline ether intermediate obtained in the step 1 with ethylene oxide under the action of a catalyst to prepare an aniline polyoxyethylene ether intermediate; and 3, further heating and polymerizing the aniline polyoxyethylene ether intermediate obtained in the step 2 and acrylic acid under the action of a reducing agent, an oxidizing agent and a chain transfer agent, and regulating the pH value to 7-8 by adopting a pH regulator after polymerization. The preparation process of the water reducer is simple and feasible, the conditions are mild, the synthesis efficiency is high, the advantages of low energy consumption and low carbon and environmental protection are achieved, and the obtained water reducer can ensure the usability under the condition of high soil content.

Description

Preparation method and application of mud-resistant high-adsorption water-reducing polycarboxylate superplasticizer
Technical Field
The invention belongs to the technical field of concrete building materials, and particularly relates to a preparation method and application of a mud-resistant high-adsorption water-reducing polycarboxylate water reducer.
Background
With the high-speed development of national economy in China, a large number of civil engineering construction promote the development of the building industry in China towards high efficiency, high performance and sustainable direction. Concrete is used as an important civil engineering material, and the performance of the concrete has a profound effect on the progress of construction technology. The use of various water reducers can not only influence the workability of the concrete in a new mixing stage, but also improve the structure of the hardened concrete body from microscopic and submicroscopic levels, so that the concrete can be modified by means of adding the water reducers, and the requirements on the concrete construction performance, mechanical performance, durability and the like are met. The polycarboxylate water reducer gradually replaces high-efficiency water reducers such as lignosulfonate water reducer, naphthalene water reducer and the like due to the unique advantages of designable molecular structure and performance, and becomes a main water reducer variety in the market.
In recent years, due to huge construction engineering quantity, the consumption of sand and stone each year is large, high-quality sand and stone resources are smaller and smaller, and most sand and stone have the problems of unreasonable grain shape and grading, higher mud content and the like, so that the strength and durability of concrete are reduced. It is generally considered that the polycarboxylate water reducer is adsorbed on cement particles after being contacted with cement paste, and then plays roles of steric hindrance and electrostatic repulsion, so that the fresh cement paste, mortar or concrete has good dispersion performance. The influence of clay mineral on the polycarboxylic acid performance is mainly in a competitive adsorption relation with cement, and the clay mineral can adsorb the polycarboxylic acid water reducer, so that in concrete with more clay mineral content, the requirement of concrete workability can be met by more mixing amount of the polycarboxylic acid water reducer, and the foundation cost can be greatly increased. Therefore, further development of a new water reducing agent which is resistant to mud high adsorption and simple to prepare and bring the water reducing agent to the market is needed.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation method and application of a mud-resistant high-adsorption water-reducing polycarboxylate superplasticizer. The technical scheme of the invention is as follows:
in a first aspect, the invention provides a preparation method of a mud-resistant high-adsorption water-reducing polycarboxylate superplasticizer, which comprises the following steps:
step 1, preparing an aniline ether intermediate from a substituted vinyl ether compound and aniline under the action of an initiator;
step 2, polymerizing the aniline ether intermediate obtained in the step 1 with ethylene oxide under the action of a catalyst to prepare an aniline polyoxyethylene ether intermediate;
and 3, further heating and polymerizing the aniline polyoxyethylene ether intermediate obtained in the step 2 and acrylic acid under the action of a reducing agent, an oxidizing agent and a chain transfer agent, and regulating the pH value to 7-8 by adopting a pH regulator after polymerization.
Further, the specific control process in the step 1 is as follows: mixing 100-200 parts of substituted vinyl ether compound, 500-600 parts of deionized water, 0.5-1 part of initiator and 90-110 parts of aniline, uniformly mixing the substituted vinyl ether compound, the deionized water and the aniline, dripping the initiator at 10-20 ℃, and carrying out heat preservation reaction for 3-4 hours after dripping to obtain the aniline ether intermediate.
Further, the substituted vinyl ether compound includes diethylene glycol divinyl ether, triethylene glycol divinyl ether, or tetraethylene glycol divinyl ether.
Further, the initiator is an aqueous solution of ammonium persulfate, sodium persulfate or potassium persulfate.
Further, the specific control process in the step 2 is as follows: mixing 100-120 parts of aniline ether intermediate, 1500-2000 parts of ethylene oxide and 1-2 parts of catalyst; firstly, carrying out dehydration treatment on an aniline ether intermediate; then adding a catalyst into the dehydrated aniline ether intermediate, introducing ethylene oxide under the anaerobic condition, and carrying out polymerization reaction under the conditions of 100-130 ℃ and 0.2-0.5 MPa; cooling to 80-90 ℃ after the reaction is finished, adding a neutralizing agent to neutralize the reaction liquid, and filtering to obtain the aniline polyoxyethylene ether intermediate.
Further, the temperature of the dehydration treatment is 60-70 ℃, and the water content of the dehydrated aniline ether intermediate is less than 0.1%.
Preferably, the catalyst is metallic sodium, metallic potassium, sodium methoxide, potassium hydroxide or sodium hydroxide.
Further, the molecular weight of the aniline polyoxyethylene ether intermediate is 800-1500.
Further, the specific control process in the step 3 is as follows: according to 420-440 parts of aniline polyoxyethylene ether intermediate, 1-2 parts of reducing agent, 1-2 parts of oxidant, 2-3 parts of chain transfer agent and 35-45 parts of acrylic acid; preparing a solution A, a solution B and a solution C from a reducing agent, 71.4-77.8% of acrylic acid and a chain transfer catalyst by deionized water respectively; mixing the aniline polyoxyethylene ether intermediate, the rest of acrylic acid, the oxidant and deionized water uniformly, simultaneously dripping the solution A, the solution B and the solution C into a reaction system at the constant temperature of 40-50 ℃, after dripping for 2-4 hours, cooling to room temperature, and adding a pH regulator to regulate the pH value of the system to 7-8.
Further, the reducing agent is sodium sulfite, sodium hypophosphite or sodium thiosulfate.
Further, the oxidant is hydrogen peroxide, ammonium persulfate or potassium persulfate.
Further, the chain transfer agent is thioglycollic acid, sodium bisulphite, mercaptoethanol or mercaptopropionic acid.
Further, the pH regulator is 30 (wt)% sodium hydroxide solution or 30 (wt)% potassium hydroxide solution.
Preferably, the constant temperature condition of 40-50 ℃ is realized by microwave heating, and the microwave heating power is 200-300W.
In a second aspect, the invention provides a mud-resistant high-adsorption water-reducing polycarboxylate superplasticizer, which is prepared by adopting the preparation method.
In a third aspect, the invention provides a concrete material comprising the anti-mud high-adsorption water-reducing polycarboxylate superplasticizer.
Compared with the prior art, the invention has the following outstanding advantages and positive effects:
1) According to the preparation method of the water reducer, a large number of benzene rings and amine structures are introduced into the initiator, so that the adsorption of kaolin, montmorillonite and the like on polycarboxylic acid is weakened, and the usability of the polycarboxylic acid water reducer under the condition of higher soil content is improved;
2) The preparation process of the water reducer is simple and feasible, the condition is mild, the synthesis efficiency is high, and the water reducer has the advantages of low energy consumption, low carbon and environmental protection.
Detailed Description
In the description of the present invention, it is to be noted that the specific conditions are not specified in the examples, and the description is performed under the conventional conditions or the conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The present invention will be described in further detail with reference to the following specific embodiments, so as to assist those skilled in the art in a more complete, accurate and thorough understanding of the inventive concept and technical solution of the present invention, and the scope of the present invention includes, but is not limited to, the following examples, any modifications made in the details and form of the technical solution of the present invention falling within the scope of the present invention without departing from the spirit and scope of the present application.
Example 1
The embodiment provides a preparation method of an anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which comprises the following steps of:
(1) 500g of deionized water, 100g of diethylene glycol divinyl ether and 90g of aniline are sequentially added into a 1000ml three-neck flask, the mixture is placed into a water bath at 10 ℃ for full stirring, then 0.5g of ammonium persulfate solution is slowly added dropwise, and the mixture is reacted for 3 hours at constant temperature to obtain an aniline ether solution.
(2) Adding 100g of the aniline ether solution prepared in the step (1) into a high-pressure reaction kettle, heating to 60 ℃, decompressing to-0.07 Mpa, and dehydrating until the water meets the reaction requirement. After dehydration, 1g of metallic sodium was added. Pumping the pressure in the reaction kettle to-0.07 Mpa, then filling 0.4Mpa nitrogen, and repeating the process for three times to remove redundant oxygen in the system. After the degassing, 2000g of ethylene oxide was introduced and polymerized at 120℃under a pressure of 0.4 MPa. Cooling to 80-90 ℃ after the reaction is finished, adding 1g of glacial acetic acid for neutralization, and filtering to obtain the aniline polyoxyethylene ether with the molecular weight of 800-1500.
(3) Accurately weighing 420g of aniline polyoxyethylene ether, 10g of acrylic acid and 1.1g of hydrogen peroxide, putting into a four-mouth reaction flask, putting into a microwave reactor, installing a stirrer and a thermometer, adding 50mL of deionized water after sealing, and uniformly stirring the mixture solution.
Preparing solution A: sodium sulfite 1g+20g deionized water
Preparing a solution B: 25g+20g acrylic acid deionized water
Preparing a solution C: thioglycollic acid 2g+20g deionized water
Starting the microwave reactor, heating the solution by adopting microwave power of 200W, and respectively and simultaneously dripping the solution A, the solution B and the solution C at the constant temperature for 2-4 hours after the temperature reaches 40-50 ℃. After the dripping is finished, after the reaction solution is cooled to room temperature, adding a proper amount of 30 (wt)% sodium hydroxide solution to adjust the pH to 7-8, and obtaining the water reducer.
Example 2
The embodiment provides a preparation method of an anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which comprises the following steps of:
(1) 500g of deionized water, 100g of triethylene glycol divinyl ether and 90g of aniline are sequentially added into a 1000ml three-neck flask, the mixture is placed into a water bath at 10 ℃ for full stirring, then 0.5g of sodium persulfate solution is slowly added dropwise, and the mixture is reacted for 3 hours at constant temperature to obtain an aniline ether solution.
(2) 110g of the aniline ether solution prepared in (1) is added into a high-pressure reaction kettle, heated to 60 ℃, decompressed to-0.07 Mpa and dehydrated until the water meets the reaction requirement. After dehydration, 1.5g of sodium methoxide was added. Pumping the pressure in the reaction kettle to-0.07 Mpa, then filling 0.4Mpa nitrogen, and repeating the process for three times to remove redundant oxygen in the system. After the degassing, 2000g of ethylene oxide was introduced and polymerized at 120℃under a pressure of 0.4 MPa. Cooling to 80-90 ℃ after the reaction is finished, adding 1g of glacial acetic acid for neutralization, and filtering to obtain the aniline polyoxyethylene ether with the molecular weight of 800-1500.
(3) Accurately weighing 440g of aniline polyoxyethylene ether, 10g of acrylic acid and 1.1g of ammonium persulfate, putting into a four-mouth reaction flask, putting into a microwave reactor, installing a stirrer and a thermometer, adding 50mL of deionized water after sealing, and uniformly stirring the mixture solution.
Preparing solution A: sodium hypophosphite 1g+20g deionized water
Preparing a solution B: acrylic acid 30g+20g deionized water
Preparing a solution C: sodium bisulphite 2g+20g deionized water
Starting the microwave reactor, heating the solution by adopting microwave power of 200W, and respectively and simultaneously dripping the solution A, the solution B and the solution C at the constant temperature for 2-4 hours after the temperature reaches 40-50 ℃. After the dripping is finished, after the reaction solution is cooled to room temperature, adding a proper amount of 30 (wt)% sodium hydroxide solution to adjust the pH to 7-8, and obtaining the water reducer.
Example 3
The embodiment provides a preparation method of an anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which comprises the following steps of:
(1) 500g of deionized water, 100g of tetraethylene glycol divinyl ether and 90g of aniline are sequentially added into a 1000ml three-neck flask, the mixture is placed into a water bath at 10 ℃ for full stirring, then 0.5g of ammonium persulfate solution is slowly added dropwise, and the mixture is reacted for 3 hours at constant temperature to obtain an aniline ether solution.
(2) Adding 100g of the aniline ether solution prepared in the step (1) into a high-pressure reaction kettle, heating to 60 ℃, decompressing to-0.07 Mpa, and dehydrating until the water meets the reaction requirement. After dehydration, 2g of potassium hydroxide was added. Pumping the pressure in the reaction kettle to-0.07 Mpa, then filling 0.4Mpa nitrogen, and repeating the process for three times to remove redundant oxygen in the system. After the degassing, 2000g of ethylene oxide was introduced and polymerized at 120℃under a pressure of 0.4 MPa. Cooling to 80-90 ℃ after the reaction is finished, adding 1g of glacial acetic acid for neutralization, and filtering to obtain the aniline polyoxyethylene ether with the molecular weight of 800-1500.
(3) Accurately weighing 430g of polyoxyethylene aniline ether, 10g of acrylic acid and 1.1g of potassium persulfate, putting into a four-mouth reaction flask, putting into a microwave reactor, installing a stirrer and a thermometer, adding 50mL of deionized water after sealing, and uniformly stirring the mixture solution.
Preparing solution A: sodium thiosulfate 1g+20g deionized water
Preparing a solution B: 35g+20g acrylic acid deionized water
Preparing a solution C: mercaptoethanol 2g+20g deionized water
Starting the microwave reactor, heating the solution by adopting microwave power of 200W, and respectively and simultaneously dripping the solution A, the solution B and the solution C at the constant temperature for 2-4 hours after the temperature reaches 40-50 ℃. After the dripping is finished, after the reaction solution is cooled to room temperature, adding a proper amount of 30 (wt)% potassium hydroxide solution to adjust the pH to 7-8, and obtaining the water reducer.
Comparative example 1
The water reducing agent was obtained in the same manner as in example 1 except that diethylene glycol divinyl ether in example 1 was replaced with 4-hydroxybutyl acrylate.
Comparative example 2
The microwave heating in the step (3) in the embodiment 1 is changed into a common electric heating mode, and the water reducer is obtained in the same manner as in the embodiment 1.
Concrete tests were performed on the water reducers of examples 1 to 3 and comparative examples 1 to 2:
slump of concrete was tested using Minfu P.042.5 cement, and concrete mix designs for testing were as described in Table 1 with reference to JGJ 55, ordinary concrete mix design rules. The concrete performance test is referred to GB/T50080-2016 method for testing the performance of common concrete mixture and GB/T50081-2016 method for testing the mechanical performance of common concrete. The test data are shown in Table 2.
TABLE 1 concrete mix/m 3
Intensity level Cement/kg Machine-made sand/kg Crushed stone (10-20 mm)/kg Water/kg
C30 370 780 1080 173
Table 2 concrete test results
As can be seen from Table 2, under the conditions that the water reducer is equally folded and mixed and not mixed with montmorillonite, the commercial water reducer has equivalent dispersion performance, but when the montmorillonite mixing amount is increased to 5%, the dispersion performance of the commercial water reducer is obviously reduced, and the dispersion performance of the high-adsorption-performance polycarboxylic acid water reducer prepared by the method is not greatly different from that of the non-mixed montmorillonite, which indicates that the polycarboxylic acid water reducer obtained by the method has good dispersion retention property, high adsorption performance and mud resistance, and is obviously superior to the water reducer obtained by the commercial water reducer and the comparative example.
In conclusion, the preparation method of the water reducer of the invention is beneficial to weakening the adsorption of kaolin, montmorillonite and the like to polycarboxylic acid by introducing a large number of benzene rings and amino structures into the initiator, and improving the service performance of the polycarboxylic acid water reducer under the condition of higher soil content; and the process temperature is controlled by adopting a microwave radiation mode, so that the introduction of N can be reduced 2 The method has the advantages of improving the dispersibility of the water reducer, improving the water reducing rate, along with low energy consumption, low carbon, environmental protection and high yield.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (10)

1. A preparation method of an anti-mud high-adsorption water-reducing polycarboxylate superplasticizer is characterized by comprising the following steps of: comprising the following steps:
step 1, preparing an aniline ether intermediate from a substituted vinyl ether compound and aniline under the action of an initiator;
step 2, polymerizing the aniline ether intermediate obtained in the step 1 with ethylene oxide under the action of a catalyst to prepare an aniline polyoxyethylene ether intermediate;
and 3, further heating and polymerizing the aniline polyoxyethylene ether intermediate obtained in the step 2 and acrylic acid under the action of a reducing agent, an oxidizing agent and a chain transfer agent, and regulating the pH value to 7-8 by adopting a pH regulator after polymerization.
2. The method for preparing the anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which is disclosed in claim 1, is characterized by comprising the following steps: the specific control process of the step 1 is as follows: mixing 100-200 parts of substituted vinyl ether compound, 500-600 parts of deionized water, 0.5-1 part of initiator and 90-110 parts of aniline, uniformly mixing the substituted vinyl ether compound, the deionized water and the aniline, dripping the initiator at 10-20 ℃, and carrying out heat preservation reaction for 3-4 hours after dripping to obtain the aniline ether intermediate.
3. The method for preparing the anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which is disclosed in claim 1 or 2, is characterized by comprising the following steps: the substituted vinyl ether compound includes diethylene glycol divinyl ether, triethylene glycol divinyl ether or tetraethylene glycol divinyl ether.
4. The method for preparing the anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which is disclosed in claim 1, is characterized by comprising the following steps: the specific control process of the step 2 is as follows: mixing 100-120 parts of aniline ether intermediate, 1500-2000 parts of ethylene oxide and 1-2 parts of catalyst; firstly, carrying out dehydration treatment on an aniline ether intermediate; then adding a catalyst into the dehydrated aniline ether intermediate, introducing ethylene oxide under the anaerobic condition, and carrying out polymerization reaction under the conditions of 100-130 ℃ and 0.2-0.5 MPa; cooling to 80-90 ℃ after the reaction is finished, adding a neutralizing agent to neutralize the reaction liquid, and filtering to obtain the aniline polyoxyethylene ether intermediate.
5. The method for preparing the anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which is disclosed in claim 1, is characterized by comprising the following steps: the specific control process of the step 3 is as follows: according to 420-440 parts of aniline polyoxyethylene ether intermediate, 1-2 parts of reducing agent, 1-2 parts of oxidant, 2-3 parts of chain transfer agent and 35-45 parts of acrylic acid; preparing a solution A, a solution B and a solution C from a reducing agent, 71.4-77.8% of acrylic acid and a chain transfer catalyst by deionized water respectively; mixing the aniline polyoxyethylene ether intermediate, the rest of acrylic acid, the oxidant and deionized water uniformly, simultaneously dripping the solution A, the solution B and the solution C into a reaction system at the constant temperature of 40-50 ℃, after dripping for 2-4 hours, cooling to room temperature, and adding a pH regulator to regulate the pH value of the system to 7-8.
6. The method for preparing the anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which is disclosed in claim 1 or 5, is characterized by comprising the following steps: the reducing agent is sodium sulfite, sodium hypophosphite or sodium thiosulfate.
7. The method for preparing the anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which is disclosed in claim 1 or 5, is characterized by comprising the following steps: the oxidant is hydrogen peroxide, ammonium persulfate or potassium persulfate.
8. The method for preparing the anti-mud high-adsorption water-reducing polycarboxylate superplasticizer, which is disclosed in claim 5, is characterized in that: the constant temperature condition of 40-50 ℃ is realized by microwave heating, and the microwave heating power is 200-300W.
9. The utility model provides a mud resistant high absorption water-reducing type polycarboxylate water reducing agent which characterized in that: is obtained by the preparation method according to any one of claims 1 to 8.
10. A concrete material characterized by: comprising the water reducing agent obtained by the production method according to any one of claims 1 to 8 or the water reducing agent according to claim 9.
CN202111645559.6A 2021-12-29 2021-12-29 Preparation method and application of mud-resistant high-adsorption water-reducing polycarboxylate superplasticizer Active CN114369208B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271885A (en) * 2015-09-24 2016-01-27 四川恒泽建材有限公司 Mud resistance and slump loss resistance type high-performance polycarboxylic acid water reducer and preparation method thereof
CN108484840A (en) * 2018-03-26 2018-09-04 厦门宏发先科新型建材有限公司 A kind of anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105713151A (en) * 2015-12-31 2016-06-29 江苏苏博特新材料股份有限公司 Application and preparation method of concrete superplasticizer with phosphorous acid group

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271885A (en) * 2015-09-24 2016-01-27 四川恒泽建材有限公司 Mud resistance and slump loss resistance type high-performance polycarboxylic acid water reducer and preparation method thereof
CN108484840A (en) * 2018-03-26 2018-09-04 厦门宏发先科新型建材有限公司 A kind of anti-chamotte mould polycarboxylate water-reducer of ester ether mixed structure and preparation method thereof

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