CN113861354A - Anti-mud polycarboxylate superplasticizer mother liquor and preparation method thereof - Google Patents
Anti-mud polycarboxylate superplasticizer mother liquor and preparation method thereof Download PDFInfo
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- CN113861354A CN113861354A CN202111308057.4A CN202111308057A CN113861354A CN 113861354 A CN113861354 A CN 113861354A CN 202111308057 A CN202111308057 A CN 202111308057A CN 113861354 A CN113861354 A CN 113861354A
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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
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- 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 discloses a mud-resistant polycarboxylate superplasticizer mother liquor and a preparation method thereof, and solves the technical problems that in the prior art, a polycarboxylate superplasticizer has high sensitivity to mud content of aggregate, is easy to increase the mixing amount in use, and affects the workability and strength of the superplasticizer. The modified phenolic aldehyde comprises unsaturated acid, unsaturated polyether, unsaturated ester, a chain transfer agent, an oxidant, a reducing agent and a side chain modifier, wherein the side chain modifier is one or more of hydroxyphenyl lignin, beta-cyclodextrin and 2-chloro-5-methylpyridine. The modified polycarboxylic acid water reducer is used for adding concrete, can effectively achieve the effects of retarding coagulation and reducing water, and meanwhile, the modified side chain can prevent the comb-shaped structure of the polycarboxylic acid water reducer from being inserted into layered clay, so that the increase of the mixing amount of the water reducer caused by the increase of the mud content in aggregate is avoided.
Description
Technical Field
The invention relates to a polycarboxylate superplasticizer mother liquor and a preparation method thereof, in particular to an anti-mud polycarboxylate superplasticizer mother liquor and a preparation method thereof.
Background
Concrete is a building material with the largest application amount and the widest application range in the current society. To obtain high performance concrete, a high performance water reducing agent is usually added thereto. The polycarboxylic acid water reducing agent is used as a third-generation water reducing agent, is prepared by copolymerizing unsaturated monomers containing carboxyl and other monomers, has the remarkable advantages of low mixing amount, high water reducing rate, small concrete slump loss, no obvious delayed coagulation, good cement adaptability, low content of harmful components, suitability for preparing high-performance concrete and the like in the concrete mixing field, and is widely applied to the concrete mixing field.
However, with the development of the construction industry and the increasing scale of domestic construction, the construction materials used in concrete casting are gradually deteriorated, wherein aggregates such as sand and stone are the most obvious, and a large amount of sand with high mud content is directly used in concrete. At this time, the defects of the polycarboxylic acid water reducing agent are reflected, the polycarboxylic acid water reducing agent is extremely sensitive to the content of mud in the sandstone, the main component of the mud is clay, and the layered structure of the clay has super strong adsorption capacity on the polycarboxylic acid water reducing agent, so that the dispersing performance of cement is reduced, and the workability of fresh concrete and the later strength and structural stability of structures are further damaged. The reason for this is that the PEO side chains in the polycarboxylic acid molecules are easily inserted between the aluminosilicate layers of the clay to form ineffective adsorption, resulting in the polycarboxylic acid water-reducing agent losing its dispersing property for cement. The concrete has adverse effects on the workability, strength, durability and the like of the concrete with the polycarboxylic acid water reducing agent in the prepared concrete in use.
Disclosure of Invention
The invention aims to provide a mud-resistant polycarboxylate superplasticizer mother liquor and a preparation method thereof, and aims to solve the technical problems that in the prior art, a polycarboxylate superplasticizer has high sensitivity to mud content of aggregate, is easy to increase the mixing amount in use, and has adverse effects on the workability, strength and durability of concrete.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides an anti-mud polycarboxylate superplasticizer mother liquor, which comprises the following chemical components: 25-125mol of unsaturated acid, 10-50mol of unsaturated polyether, 15-75mol of unsaturated ester, 1-5mol of chain transfer agent, 1-5mol of oxidant, 0.2-1mol of reducing agent and 10mol of side chain modifier;
the side chain modifier is one or more of hydroxyphenyl lignin, beta-cyclodextrin and 2-chloro-5-methylpyridine, and the unsaturated ester is an ester containing a siloxy group.
Optionally or preferably, the unsaturated acid is one or more of acrylic acid, methacrylic acid, maleic anhydride and siloxy acrylic acid.
Optionally or preferably, the unsaturated ester is one or more of hydroxyethyl siloxane acrylate, hydroxypropyl siloxane acrylate and methyl siloxane acrylate.
Optionally or preferably, the unsaturated polyether is one or more of methallyl polyoxyethylene ether, methallyl polyoxypropylene ether, methallyl butyl polyoxyethylene ether, methallyl polyoxypropylene ether, 4-hydroxybutyl vinyl polyoxyethylene ether, 4-hydroxybutyl vinyl polyoxypropylene ether, diethylene glycol monovinyl polyoxyethylene ether, diethylene glycol monovinyl polyoxypropylene ether, methoxy allyl polyoxyethylene ether, methoxy allyl polyoxypropylene ether, methoxy allyl butyl polyoxyethylene ether and methoxy allyl butyl polyoxypropylene ether.
Optionally or preferably, the chain transfer agent is one or more of 3-mercaptopropionic acid, mercaptoacetic acid, mercaptoethanol and isopropanol.
Optionally or preferably, the oxidant is any one or more of hydrogen peroxide, ammonium persulfate and tert-butyl hydroperoxide.
Optionally or preferably, the reducing agent is any one or more of ascorbic acid, sodium sulfite, sodium hypophosphite, thiourea dioxide, glucose and sodium formaldehyde sulfoxylate.
The invention provides a preparation method of a mud-resistant polycarboxylate superplasticizer mother liquor, which comprises the following steps:
s1: preparing solution A and solution B: mixing unsaturated acid, unsaturated ester monomer and deionized water to prepare solution A; mixing a reducing agent, a chain transfer agent and deionized water to prepare a solution B;
s2: mixing and reacting, namely uniformly mixing the unsaturated polyether macromonomer, the oxidant and the deionized water, pouring the mixture into a reaction container, and controlling the mixed solution to be uniformly stirred; keeping the temperature constant at 30-80 deg.C during the reaction, adding dropwise solution A and solution B into the mixed solution at constant speed within a controlled time, reacting for 20-60min after the dropwise addition is completed, adding side chain modifier, and continuing to react for 20-60 min;
s3: and (3) adjusting the pH, after the reaction is finished, cooling the reaction liquid to normal temperature, and adjusting the pH to 6-8 to obtain the anti-mud polycarboxylate superplasticizer mother liquid.
Optionally or preferably, in step S2, the control time for dropping the solution a and the solution B into the reaction vessel at a constant speed is 20-30 min.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
(1) the anti-mud polycarboxylate superplasticizer mother liquor provided by the invention further modifies the end group on the basis of the polycarboxylate superplasticizer, and a group with larger steric hindrance effect is grafted on the comb-shaped structure of the polycarboxylate superplasticizer; on the basis of the function of delaying the coagulation of cement particles by the comb-shaped structure, the side chain of the polycarboxylic water reducer is not easy to insert into the layered structure of clay, so that good mud-resistant and water-reducing effects are achieved.
(2) The anti-mud polycarboxylate superplasticizer mother liquor provided by the invention can play a good retarding role simultaneously, and carboxyl and Ca play a role in retarding2+Ion action to form complex and reduce Ca in solution2+Ionic concentration, retarding Ca (OH)2Crystals are formed, and cement hydration is delayed; carboxyl is adsorbed on cement particlesThe surface of the particles makes the cement particles have negative charges, so that electrostatic repulsion is generated among the cement particles to disperse. Meanwhile, the mother liquor of the anti-mud polycarboxylate superplasticizer also has carboxyl (-COOH), hydroxyl (-OH), polyoxyalkyl (-O-R)nPolar groups with strong affinity with water can provide dispersion and flow properties for cement particles through surface active actions such as adsorption, dispersion, wetting, lubrication and the like, and the workability of fresh concrete is improved by reducing the frictional resistance among the cement particles and reducing the free energy of the cement particles and the water interface.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
1.1 starting materials
The concrete raw material formulation adopted by the anti-mud polycarboxylate superplasticizer mother liquor prepared in example 1 is shown in table 1.
Table 1 specific raw material ratios
| Chemical composition | Specific compounds | Amount of substance/mol |
| Unsaturated acid | Acrylic acid | 120 |
| Unsaturated polyethers | Methyl allyl polyoxyethylene ether | 40 |
| Unsaturated esters | Siloxane hydroxyethyl acrylate | 45 |
| Chain transfer agent | 3-mercaptopropionic acid | 4 |
| Oxidizing agent | Hydrogen peroxide solution | 4 |
| Reducing agent | Ascorbic acid | 0.5 |
| Side chain modifiers | Hydroxyphenyl lignin | 10 |
1.2 preparation method
The preparation method of the anti-mud polycarboxylate superplasticizer mother liquor in the embodiment 1 comprises the following steps:
s1: preparing solution A and solution B: mixing unsaturated acid, unsaturated ester monomer and deionized water to prepare solution A; mixing a reducing agent, a chain transfer agent and deionized water to prepare a solution B;
s2: mixing and reacting, namely uniformly mixing the unsaturated polyether macromonomer, the oxidant and the deionized water, pouring the mixture into a reaction container, and controlling the mixed solution to be uniformly stirred; keeping the temperature constant at 30-50 deg.C during the reaction process, adding dropwise solution A and B into the mixed solution at constant speed for 20min, reacting for 40min, adding side chain modifier, and continuing to react for 40 min;
s3: and (3) adjusting the pH, after the reaction is finished, cooling the reaction liquid to normal temperature, and adjusting the pH to 6-8 to obtain the mother liquor KN1 of the anti-mud polycarboxylic acid water reducing agent.
Example 2
2.1 starting materials
The concrete raw material formulation adopted by the anti-mud polycarboxylate superplasticizer mother liquor prepared in example 2 is shown in table 2.
TABLE 2 concrete raw material ratios
| Chemical composition | Specific compounds | Amount of substance/mol |
| Unsaturated acid | Methacrylic acid | 75 |
| Unsaturated polyethers | 4-hydroxybutyl vinyl polyoxyethylene ether | 30 |
| Unsaturated esters | Siloxane hydroxypropyl acrylate | 45 |
| Chain transfer agent | Thioglycollic acid | 3 |
| Oxidizing agent | Ammonium persulfate | 3 |
| Reducing agent | Sodium sulfite | 1 |
| Side chain modifiers | Beta-cyclodextrin | 10 |
2.2 preparation method
The preparation method of the anti-mud polycarboxylate superplasticizer mother liquor in the embodiment 2 comprises the following steps:
s1: preparing solution A and solution B: mixing unsaturated acid, unsaturated ester monomer and deionized water to prepare solution A; mixing a reducing agent, a chain transfer agent and deionized water to prepare a solution B;
s2: mixing and reacting, namely uniformly mixing the unsaturated polyether macromonomer, the oxidant and the deionized water, pouring the mixture into a reaction container, and controlling the mixed solution to be uniformly stirred; keeping the temperature constant at 50-80 deg.C during the reaction process, adding dropwise solution A and B into the mixed solution at constant speed within 30min, reacting for 60min, adding side chain modifier, and continuing to react for 60 min;
s3: and (3) adjusting the pH, after the reaction is finished, cooling the reaction liquid to normal temperature, and adjusting the pH to 6-8 to obtain the mother liquor KN2 of the anti-mud polycarboxylic acid water reducing agent.
Example 3
3.1 starting materials
The concrete raw material formulation adopted by the anti-mud polycarboxylate superplasticizer mother liquor prepared in example 3 is shown in table 3.
TABLE 3 concrete raw material ratios
| Chemical composition | Specific compounds | Amount of substance/mol |
| Unsaturated acid | Siloxane based acrylic acid | 125 |
| Unsaturated polyethers | Methoxy allyl polyoxyethylene ether | 50 |
| Unsaturated esters | Siloxane based methyl acrylate | 75 |
| Chain transfer agent | Mercaptoethanol | 5 |
| Oxidizing agent | Tert-butyl hydroperoxide | 5 |
| Reducing agent | Sodium hypophosphite | 1 |
| Side chain modifiers | 2-chloro-5-methylpyridine | 10 |
3.2 preparation method
The preparation method of the anti-mud polycarboxylate superplasticizer mother liquor in the embodiment 3 comprises the following steps:
s1: preparing solution A and solution B: mixing unsaturated acid, unsaturated ester monomer and deionized water to prepare solution A; mixing a reducing agent, a chain transfer agent and deionized water to prepare a solution B;
s2: mixing and reacting, namely uniformly mixing the unsaturated polyether macromonomer, the oxidant and the deionized water, pouring the mixture into a reaction container, and controlling the mixed solution to be uniformly stirred; keeping the temperature constant at 40-60 deg.C during the reaction process, adding dropwise solution A and B into the mixed solution at constant speed within 25min, reacting for 20min, adding side chain modifier, and continuing to react for 20 min;
s3: and (3) adjusting the pH, after the reaction is finished, cooling the reaction liquid to normal temperature, and adjusting the pH to 6-8 to obtain the mother liquor KN3 of the anti-mud polycarboxylic acid water reducing agent.
Example 4
4.1 starting materials
The concrete raw material formulation adopted by the anti-mud polycarboxylate superplasticizer mother liquor prepared in example 4 is shown in table 4.
TABLE 4 concrete raw material ratios
| Chemical composition | Specific compounds | Amount of substance/mol |
| Unsaturated acid | Acrylic acid | 25 |
| Unsaturated polyethers | 4-hydroxybutyl vinyl polyoxyethylene ether | 10 |
| Unsaturated esters | Siloxane based methyl acrylate | 15 |
| Chain transfer agent | Thioglycollic acid | 1 |
| Oxidizing agent | Ammonium persulfate | 1 |
| Reducing agent | Thiourea dioxide | 1 |
| Side chain modifiers | Beta-cyclodextrin | 10 |
4.2 preparation method
The preparation method of the anti-mud polycarboxylate superplasticizer mother liquor in the embodiment 4 comprises the following steps:
s1: preparing solution A and solution B: mixing unsaturated acid, unsaturated ester monomer and deionized water to prepare solution A; mixing a reducing agent, a chain transfer agent and deionized water to prepare a solution B;
s2: mixing and reacting, namely uniformly mixing the unsaturated polyether macromonomer, the oxidant and the deionized water, pouring the mixture into a reaction container, and controlling the mixed solution to be uniformly stirred; keeping the temperature constant at 30-80 deg.C during the reaction process, adding dropwise solution A and B into the mixed solution at constant speed within 25min, reacting for 35min, adding side chain modifier, and continuing to react for 35 min;
s3: and (3) adjusting the pH, after the reaction is finished, cooling the reaction liquid to normal temperature, and adjusting the pH to 6-8 to obtain the mother liquor KN4 of the anti-mud polycarboxylic acid water reducing agent.
Example 5
5.1 starting materials
The concrete raw material formulation adopted by the anti-mud polycarboxylate superplasticizer mother liquor prepared in example 5 is shown in Table 5.
Table 5 specific raw material ratios
| Chemical composition | Specific compounds | Amount of substance/mol |
| Unsaturated acid | Acrylic acid | 60 |
| Unsaturated polyethers | Methoxyalkenylbutyl polyoxypropylene ether | 30 |
| Unsaturated esters | Siloxane based methyl acrylate | 20 |
| Chain transfer agent | Thioglycollic acid | 50 |
| Oxidizing agent | Hydrogen peroxide solution | 2 |
| Reducing agent | Hanging white block | 0.2 |
| Side chain modifiers | Hydroxyphenyl lignin | 10 |
5.2 preparation method
The preparation method of example 5 is the same as that of example 1, and the anti-mud polycarboxylate superplasticizer mother liquor KN5 is obtained.
Example 6
6.1 starting materials
The concrete raw material formulation adopted by the anti-mud polycarboxylate superplasticizer mother liquor prepared in example 6 is shown in table 6.
TABLE 6 specific raw material ratios
6.2 preparation method
The preparation method of example 6 was the same as that of example 1, and a mud-resistant polycarboxylate superplasticizer mother liquor KN6 was obtained.
Detection experiment
The mud-resistant polycarboxylate water reducing agent mother liquors KN1, KN2, KN3, KN4, KN5 and KN6 prepared in examples 1 to 6 were subjected to a cement paste fluidity test and a concrete performance test, and compared with a conventional polycarboxylate water reducing agent mother liquor OXPC-500 commercially available from Oako, Sichuan chemical Co., Ltd. Except for the mother liquor of the mud-resistant polycarboxylate superplasticizer prepared in the embodiment of the invention and the OXPC-500 sample for comparison and detection, other third additives are not used in all test experiments. 1. Experimental comparison of fluidity of cement paste
The test of the fluidity of the cement paste refers to the detection standard: GB/T8077 and 2012 test method for homogeneity of concrete admixture, cement: yadong P.O 42.5.5R, water: 87g, the water-cement ratio is 0.29. The test results are shown in Table 7.
TABLE 7 Cement paste fluidity test results
The test results in Table 7 show that after the sodium-based montmorillonite is added under the same conditions, the initial and 60-min net slurry fluidity of the anti-mud polycarboxylic acid water reducer mother liquor prepared according to the invention is obviously superior to OXPC-500, and the anti-mud polycarboxylic acid water reducer mother liquor prepared according to the invention has a certain adsorption resistance effect on the clay added in a simulation mode, not only the initial dispersibility of the cement is increased, but also the dispersion retention performance is improved to different degrees.
2. Fresh concrete Performance test
The concrete performance experiment refers to the detection standard: GB 8076 plus 2008 concrete admixture, GB/T50080-2016 common concrete mixture performance test method standard and GB/T50081 plus 2019 concrete physical and mechanical property test method standard. Cement: and P.O 42.5.5R, wherein the sand is medium sand with fineness modulus M of 2.65, the content of mud is 3.7%, and the particle size of the pebbles is 5-25 mm. The concrete mix ratio is shown in Table 8.
TABLE 8 concrete mix proportion (unit: kg/m)3)
The concrete was freshly mixed under the above conditions and mixing ratio, and the initial slump, initial extension, slump and extension loss after 1 hour, and 7-day and 28-day strength of the concrete were measured, and the test results are shown in Table 9.
TABLE 9 fresh concrete Properties (folded solid content: 0.16%)
The concrete performance test results in Table 9 show that the initial slump, the expansion degree and the time loss of the concrete of the anti-mud polycarboxylic acid water reducing agent mother liquor prepared according to the invention are all superior to OXPC-500, and the strength is obviously improved in 7 days and 28 days. The anti-mud polycarboxylate superplasticizer mother liquor prepared by the invention has a certain adsorption resistance effect on mud in concrete gravel materials, so that the workability of fresh concrete is improved to a certain extent, and the slump, the expansion retention performance and the concrete compressive strength are obviously improved.
The anti-mud polycarboxylate superplasticizer mother liquor provided by the invention further modifies the end group on the basis of the polycarboxylate superplasticizer, and a group with larger steric hindrance effect is grafted on the comb-shaped structure of the polycarboxylate superplasticizer; on the basis of the function of delaying the coagulation of cement particles by the comb-shaped structure, the side chain of the polycarboxylic water reducer is not easy to insert into the layered structure of clay, so that good mud-resistant and water-reducing effects are achieved.
The anti-mud polycarboxylate superplasticizer mother liquor provided by the invention can play a good retarding role simultaneously, and carboxyl and Ca play a role in retarding2+Ion action to form complex and reduce Ca in solution2+Ionic concentration, retarding Ca (OH)2Crystals are formed, and cement hydration is delayed; the carboxyl is adsorbed on the surface of the cement particles, so that the cement particles are negatively charged, and electrostatic repulsion is generated among the cement particles to be dispersed. Meanwhile, the mother liquor of the anti-mud polycarboxylate superplasticizer also has carboxyl (-COOH), hydroxyl (-OH), polyoxyalkyl (-O-R)nPolar groups with strong affinity with water, can provide dispersion and flow performance for cement particles through surface active actions such as adsorption, dispersion, wetting, lubrication and the like, and reduce friction among the cement particlesResistance, and free energy reduction at the interface between cement particles and water to increase the workability of fresh concrete.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. The mud-resistant polycarboxylate superplasticizer mother liquor is characterized by comprising the following chemical components: 25-125mol of unsaturated acid, 10-50mol of unsaturated polyether, 15-75mol of unsaturated ester, 1-5mol of chain transfer agent, 1-5mol of oxidant, 0.2-1mol of reducing agent and 10mol of side chain modifier;
the side chain modifier is one or more of hydroxyphenyl lignin, beta-cyclodextrin and 2-chloro-5-methylpyridine, and the unsaturated ester is an ester containing a siloxy group.
2. The anti-mud polycarboxylate superplasticizer mother liquor as claimed in claim 1, characterized in that: the unsaturated acid is one or more of acrylic acid, methacrylic acid, maleic anhydride and siloxy acrylic acid.
3. The anti-mud polycarboxylate superplasticizer mother liquor as claimed in claim 1, characterized in that: the unsaturated ester is one or more of siloxane hydroxyethyl acrylate, siloxane hydroxypropyl acrylate and siloxane methyl acrylate.
4. The anti-mud polycarboxylate superplasticizer mother liquor as claimed in claim 1, characterized in that: the unsaturated polyether is one or more of methyl allyl polyoxyethylene ether, methyl allyl polyoxypropylene ether, methyl allyl butyl polyoxyethylene ether, methyl allyl butyl polyoxypropylene ether, 4-hydroxybutyl vinyl polyoxyethylene ether, 4-hydroxybutyl vinyl polyoxypropylene ether, diethylene glycol monovinyl polyoxyethylene ether, diethylene glycol monovinyl polyoxypropylene ether, methoxy allyl polyoxyethylene ether, methoxy allyl polyoxypropylene ether, methoxy allyl butyl polyoxyethylene ether and methoxy allyl butyl polyoxypropylene ether.
5. The anti-mud polycarboxylate superplasticizer mother liquor as claimed in claim 1, characterized in that: the chain transfer agent is one or more of 3-mercaptopropionic acid, thioglycolic acid, mercaptoethanol and isopropanol.
6. The anti-mud polycarboxylate superplasticizer mother liquor as claimed in claim 1, characterized in that: the oxidant is any one or more of hydrogen peroxide, ammonium persulfate and tert-butyl hydroperoxide.
7. The anti-mud polycarboxylate superplasticizer mother liquor as claimed in claim 1, characterized in that: the reducing agent is any one or more of ascorbic acid, sodium sulfite, sodium hypophosphite, thiourea dioxide, glucose and sodium formaldehyde sulfoxylate.
8. The preparation method of the anti-mud polycarboxylate superplasticizer mother liquor as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
s1: preparing solution A and solution B: mixing unsaturated acid, unsaturated ester monomer and deionized water to prepare solution A; mixing a reducing agent, a chain transfer agent and deionized water to prepare a solution B;
s2: mixing and reacting, namely uniformly mixing the unsaturated polyether macromonomer, the oxidant and the deionized water, pouring the mixture into a reaction container, and controlling the mixed solution to be uniformly stirred; keeping the temperature constant at 30-80 deg.C during the reaction, adding dropwise solution A and solution B into the mixed solution at constant speed within a controlled time, reacting for 20-60min after the dropwise addition is completed, adding side chain modifier, and continuing to react for 20-60 min;
s3: and (3) adjusting the pH, after the reaction is finished, cooling the reaction liquid to normal temperature, and adjusting the pH to 6-8 to obtain the anti-mud polycarboxylate superplasticizer mother liquid.
9. The preparation method of the anti-mud polycarboxylate superplasticizer mother liquor as claimed in claim 8, characterized in that: in the step S2, the liquid a and the liquid B are dropped into the reaction vessel at a constant speed for 20-30 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114591020A (en) * | 2022-03-30 | 2022-06-07 | 石家庄市长安育才建材有限公司 | Concrete water reducing agent suitable for machine-made sand and preparation method and application thereof |
| CN114874400A (en) * | 2022-04-27 | 2022-08-09 | 河北凯瑞化工有限公司 | Preparation method of novel high-dispersity and high-slump-retaining polycarboxylate superplasticizer |
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