CN110951011A - Preparation method of anti-mud polycarboxylic acid sustained-release agent for concrete - Google Patents
Preparation method of anti-mud polycarboxylic acid sustained-release agent for concrete Download PDFInfo
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- CN110951011A CN110951011A CN201911268051.1A CN201911268051A CN110951011A CN 110951011 A CN110951011 A CN 110951011A CN 201911268051 A CN201911268051 A CN 201911268051A CN 110951011 A CN110951011 A CN 110951011A
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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
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention provides a preparation method of an anti-mud polycarboxylic acid sustained release agent for concrete, which comprises the following steps: (1) adding prenyl polyoxyethylene ether (TPGE-2400) into a reaction vessel, slowly heating, heating to 80 ℃, adding phthalic anhydride, and stirring for 2 hours; (2) adding deionized water into the reaction container in the step (1), uniformly stirring, and adding benzoyl peroxide; (3) preparing a mixed solution from a molecular weight regulator AMSD, acrylamide, acrylic acid, hydroxyethyl acrylate and deionized water; (4) and (3) dropwise adding the mixed solution prepared in the step (3) into the product obtained in the step (2) at 75-80 ℃, wherein the dropwise adding time is 0.5-2 hours, and after the dropwise adding is finished, keeping the temperature at 60-80 ℃ for 2-4 hours to obtain the anti-mud slow release agent with the concentration of 50%. The invention increases the volume of the branched chain and increases the functional group of the cation by designing and adjusting the molecular structure, thereby reducing the intercalation adsorption of the sustained release agent on the branched chain in the concrete and achieving the effective sustained release effect.
Description
Technical Field
The invention relates to the technical field of concrete admixtures, in particular to a preparation method of a mud-resistant polycarboxylic acid slow-release agent for concrete.
Background
Because of the lack of natural sand, a great deal of machine-made sand has begun to be used in concrete structures and projects. The machine-made sand has the following advantages: the quality of the sand is guaranteed in the factory production. The physical and mechanical properties of the sand are good, the hard rock can be selected consciously to produce the machine-made sand, and soft and weathered rocks are avoided. The chemical components are consistent with those of the parent metal and the broken stone, and the concrete has no negative effect on the concrete and is suitable for being used as high-strength concrete. The fineness modulus and the grain composition of the machine-made sand can be adjusted according to the requirement of engineering.
Because of the advantages of machine-made sand, and the lack of natural sand, it is increasingly used by concrete members and projects. But the machine-made sand contains a certain amount of stone powder and clay. The clay is adsorbed on the surface of the sand, which hinders the bonding of the sand and the cement, and not only has strict requirements on concrete additives, especially on a polycarboxylic acid water reducing agent. The effect of clay on the performance of concrete water reducing agents, this problem is also present in slow release agents used to maintain slump in concrete. The clay has great negative effect on the working performance of concrete doped with the slow release agent, and the strong adsorbability is mainly caused by the layered structure and the large specific surface area of the clay. Although research and development are carried out for years aiming at the influence of machine-made sand on the admixture, and a water reducing agent product is researched and developed, no development report is found for the slow release agent with the mud resistance.
Therefore, the anti-mud slow release agent for concrete is developed, achieves the effect of natural sand in the using process, and has the following significance: the waste of chemical resources is reduced, the performance of the machine-made sand concrete is improved, the machine-made sand is better applied, and various performances of the concrete and the quality of the concrete are guaranteed.
At present, an improved water reducing agent specially aiming at machine-made sand exists, and the adsorption of clay to an additive is inhibited by adding a small compound material. Wherein, cation and phosphate are polymerized on the molecular main chain, so that the intercalation adsorption of the clay to the water reducing agent branched chain is reduced. This only moderately alleviates the deficiencies of water reducers, while slump retention, one of the important indicators of concrete performance, requires a slow release agent to maintain. However, the sustained release agent of the polycarboxylic acid is used in the machine-made sand concrete in an amount which is more than one time than that of the natural sand concrete under the same mixing ratio condition. For example: the water reducing agent is used for natural sand concrete, the water reducing agent is 7 parts, the slow release agent is 3 parts, the mixing amount is 0.2%, the water reducing rate is 26%, the slump in 2 hours is not lost, and 6 parts of the machine-made sand, the water reducing agent is 7 parts, and the slow release agent are required to reach the water reducing rate and slump index of the natural sand. An enterprise selling 10 ten thousand tons of additives every year uses about 700 tons of common slow release agents for machine-made sand concrete, wherein 350 tons of the slow release agents are increased dosage caused by clay adsorption, and the cost of consumed raw materials is 175 ten thousand yuan. The national market volume is estimated to be more than 100 million tons/year, and the cost of raw materials consumed by clay is more than 20 million yuan. The slow release agent with the anti-mud function for the machine-made sand is researched and invented, and the market demand is huge. Has great economic benefit and social benefit.
The slow release agent controls the dispersion process of water reducing agent molecules on cement particles in a physical or chemical mode, and the dispersion of the slow release agent molecules on the cement particles is continuously and slowly carried out within a certain time. The method is mainly used for maintaining the slump of the ready-mixed concrete after long-time transportation or avoiding the evaporation of mixing water caused by long-time transportation at high temperature. In addition, the slow release agent can be prepared into micro-slump concrete used in water conservancy dam engineering and the like, so that the defects of aggregate separation of roller compacted concrete, weak interlayer combination and easy formation of a micro leakage channel can be reduced, and good tensile, shear and frost resistance properties are achieved.
The release mechanism of the sustained release agent is generally chemical sustained release. The slow release effect is realized by breaking chemical bonds. They can be classified into intramolecular reaction type and crosslinking type. The molecules of the intramolecular reaction type slow-release water reducing agent generally contain amide groups, acyl anhydrides and esters which can be hydrolyzed into hydrophilic groups such as carboxylic acid under an alkaline environment, and the hydrophilic groups continuously adsorb and disperse cement particles in the gradual hydrolysis reaction process. The crosslinking sustained-release agent can directly introduce a monomer with multiple double bonds in the polymerization reaction or carry out micro-crosslinking on the polymerized macromolecules, can also carry out ionic crosslinking through coordination bonds formed between oxygen on carboxyl and metal elements, and releases macromolecules with a dispersion effect through the hydrolysis of molecules in an alkaline environment so as to achieve the sustained-release effect.
For concrete with larger mud content, the performance of the concrete is obviously reduced after montmorillonite adsorbs the branch chain of the sustained-release agent.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a mud-resistant polycarboxylic acid slow-release agent for concrete, the produced mud-resistant polycarboxylic acid slow-release agent has a mud-resistant function on machine-made sand, the defect that no slow-release agent with the mud-resistant function aiming at the machine-made sand exists in the prior art is overcome, and the mud-resistant polycarboxylic acid slow-release agent overcomes the influence of montmorillonite in concrete on the slow-release agent to achieve an effective slow-release effect.
The technical scheme of the invention is as follows: a preparation method of an anti-mud polycarboxylic acid slow release agent for concrete comprises the following steps:
(1) adding prenyl polyoxyethylene ether (TPGE-2400) into a reaction vessel, slowly heating, heating to 80 ℃, adding phthalic anhydride, and stirring for 2 hours;
(2) adding deionized water into the reaction container in the step (1), uniformly stirring, and adding benzoyl peroxide;
(3) preparing a mixed solution from a molecular weight regulator AMSD, acrylamide, acrylic acid, hydroxyethyl acrylate and deionized water;
(4) and (3) dropwise adding the mixed solution prepared in the step (3) into the product obtained in the step (2) at 75-80 ℃, wherein the dropwise adding time is 0.5-2 hours, and after the dropwise adding is finished, keeping the temperature at 60-80 ℃ for 2-4 hours to obtain the anti-mud slow release agent with the concentration of 50%.
In the step (1), the mol ratio of the prenyl alcohol polyoxyethylene ether to the phthalic anhydride is 1: 0.85.
the amount of initiator used was 0.317% of the total mass of all monomers.
Acrylic acid acrylamide hydroxyethyl acrylate: the mole ratio of the prenyl polyoxyethylene ether is 0.7:0.68:3.0: 1.0.
The molecular weight regulator AMSD accounts for 0.476 percent of the total mass of the prenol polyoxyethylene ether.
The reaction temperature in the step (4) is 80 ℃, the reaction time is 2 hours, the dripping time is 45 minutes, the heat preservation temperature is 70-80 ℃, and the heat preservation time is 3 hours.
Hydroxyl at the tail end of TPEG is utilized and phthalic anhydride is used for esterification, so that the volume of the large branched chain is increased, the intercalation adsorption of montmorillonite on the branched chain of the slow release agent is prevented, the steric hindrance dispersion capability of the branched chain is exerted, and the dosage of the collapse-protecting agent in the concrete admixture with high sand making value or methylene blue value is reduced.
The invention has the beneficial effects that: by redesigning and adjusting the molecular structure, the spacing distance and the HLB value of the branched chain are researched, the volume of the branched chain is increased, and the functional group of the cation is increased, so that the intercalation adsorption of the sustained-release agent on the branched chain in the concrete is reduced, and the effective sustained-release effect is achieved. In application, the defects of large using amount, unstable slump, hysteresis bleeding and poor fluidity in the concrete with high machine-made sand or methylene blue value are eliminated, and various performance indexes of the concrete meet the design requirements.
Detailed Description
In order to make the object, technical solution and technical effect of the present invention more apparent, the present invention will be further described with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
A preparation method of an anti-mud polycarboxylic acid slow release agent for concrete comprises the following steps:
(1) adding 200g of prenyl polyoxyethylene ether (TPGE-2400) into a reaction vessel, slowly heating to 80 ℃, adding 12.3g of phthalic anhydride, and stirring for 2 hours;
(2) adding 200g of deionized water into the reaction vessel in the step (1), uniformly stirring, and adding 0.8g of benzoyl peroxide;
(3) preparing a mixed solution by taking 1.2g of molecular weight regulator AMSDF, 4g of acrylamide, 4.2g of acrylic acid, 22g of hydroxyethyl acrylate and 50g of deionized water;
(4) and (3) dropwise adding the mixed solution prepared in the step (3) into the product obtained in the step (2) at 80 ℃, wherein the dropwise adding time is 1 hour, and after the dropwise adding is finished, keeping the temperature at 65 ℃ for 3 hours to obtain the anti-mud slow release agent with the concentration of 50%.
Example two
A preparation method of an anti-mud polycarboxylic acid slow release agent for concrete comprises the following steps:
(1) adding 200g of prenyl polyoxyethylene ether (TPGE-2400) into a reaction vessel, slowly heating to 80 ℃, adding 12.3g of phthalic anhydride, and stirring for 2 hours;
(2) adding 200g of deionized water into the reaction vessel in the step (1), uniformly stirring, and adding 0.8g of benzoyl peroxide;
(3) preparing a mixed solution by taking 1.2g of molecular weight regulator AMSDF, 4g of acrylamide, 4.2g of acrylic acid, 22g of hydroxyethyl acrylate and 50g of deionized water;
(4) and (3) dropwise adding the mixed solution prepared in the step (3) into the product obtained in the step (2) at 75 ℃, wherein the dropwise adding time is 45 minutes, and after the dropwise adding is finished, keeping the temperature at 75 ℃ for 3 hours to obtain the anti-mud slow release agent with the concentration of 50%.
EXAMPLE III
A preparation method of an anti-mud polycarboxylic acid slow release agent for concrete comprises the following steps:
(1) adding 200g of prenyl polyoxyethylene ether (TPGE-2400) into a reaction vessel, slowly heating to 80 ℃, adding 12.3g of phthalic anhydride, and stirring for 2 hours;
(2) adding 200g of deionized water into the reaction vessel in the step (1), uniformly stirring, and adding 0.8g of benzoyl peroxide;
(3) preparing a mixed solution by taking 1.2g of molecular weight regulator AMSDF, 4g of acrylamide, 4.2g of acrylic acid, 22g of hydroxyethyl acrylate and 50g of deionized water;
(4) and (3) dropwise adding the mixed solution prepared in the step (3) into the product obtained in the step (2) at 75 ℃, wherein the dropwise adding time is 0.5 hour, and after the dropwise adding is finished, keeping the temperature at 60 ℃ for 4 hours to obtain the anti-mud slow release agent with the concentration of 50%.
Example four
A preparation method of an anti-mud polycarboxylic acid slow release agent for concrete comprises the following steps:
(1) adding 200g of prenyl polyoxyethylene ether (TPGE-2400) into a reaction vessel, slowly heating to 80 ℃, adding 12.3g of phthalic anhydride, and stirring for 2 hours;
(2) adding 200g of deionized water into the reaction vessel in the step (1), uniformly stirring, and adding 0.8g of benzoyl peroxide;
(3) preparing a mixed solution by taking 1.2g of molecular weight regulator AMSDF, 4g of acrylamide, 4.2g of acrylic acid, 22g of hydroxyethyl acrylate and 50g of deionized water;
(4) and (3) dropwise adding the mixed solution prepared in the step (3) into the product obtained in the step (2) at 78 ℃, wherein the dropwise adding time is 2 hours, and after the dropwise adding is finished, keeping the temperature at 80 ℃ for 4 hours to obtain the anti-mud slow release agent with the concentration of 50%.
EXAMPLE five
A preparation method of an anti-mud polycarboxylic acid slow release agent for concrete comprises the following steps:
(1) adding 200g of prenyl polyoxyethylene ether (TPGE-2400) into a reaction vessel, slowly heating to 80 ℃, adding 12.3g of phthalic anhydride, and stirring for 2 hours;
(2) adding 200g of deionized water into the reaction vessel in the step (1), uniformly stirring, and adding 0.8g of benzoyl peroxide;
(3) preparing a mixed solution by taking 1.2g of molecular weight regulator AMSDF, 4g of acrylamide, 4.2g of acrylic acid, 22g of hydroxyethyl acrylate and 50g of deionized water;
(4) and (3) dropwise adding the mixed solution prepared in the step (3) into the product obtained in the step (2) at 80 ℃, wherein the dropwise adding time is 0.5 hour, and after the dropwise adding is finished, keeping the temperature at 80 ℃ for 2 hours to obtain the anti-mud slow release agent with the concentration of 50%.
In order to detect the concrete anti-mud polycarboxylic acid sustained release agent obtained by the invention, the applicant detects the concrete anti-mud polycarboxylic acid sustained release agent obtained in the example 1, and the detection method and the detection result are as follows:
reference standard
GB/T8077 and 2012 test method for homogeneity of concrete admixture
GB8076-2008 concrete admixture
JG/T223-2007 polycarboxylic acid high-performance water reducing agent
GB/T50080-2002 Standard of Performance test methods for common concrete mixtures
GB/T50081-2002 Standard for testing mechanical properties of ordinary concrete
TABLE 1 main homogeneity index
TABLE 2 fluidity (comparison with the fluidity of a conventional sustained-release agent under pure cement conditions)
TABLE 3 Cement paste fluidity test with montmorillonite (compare with ordinary slow release agent)
Comparison of concrete Properties
Table 4-1 concrete mix ratios:
TABLE 4-2 compounding of additives
TABLE 4-3 concrete Performance test (2.0%)
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the present invention pertains, the architecture form can be flexible and varied without departing from the concept of the present invention, and a series of products can be derived. But rather a number of simple derivations or substitutions are made which are to be considered as falling within the scope of the invention as defined by the appended claims.
Claims (6)
1. A preparation method of an anti-mud polycarboxylic acid slow release agent for concrete is characterized by comprising the following steps:
(1) adding prenyl polyoxyethylene ether (TPGE-2400) into a reaction vessel, slowly heating, heating to 80 ℃, adding phthalic anhydride, and stirring for 2 hours;
(2) adding deionized water into the reaction container in the step (1), uniformly stirring, and adding benzoyl peroxide;
(3) preparing a mixed solution from a molecular weight regulator AMSD, acrylamide, acrylic acid, hydroxyethyl acrylate and deionized water;
(4) and (3) dropwise adding the mixed solution prepared in the step (3) into the product obtained in the step (2) at 75-80 ℃, wherein the dropwise adding time is 0.5-2 hours, and after the dropwise adding is finished, keeping the temperature at 60-80 ℃ for 2-4 hours to obtain the anti-mud slow release agent with the concentration of 50%.
2. The method for preparing the mud-resistant polycarboxylic acid slow-release agent for concrete according to claim 1, wherein in the step (1), the mole ratio of the prenyl polyoxyethylene ether to the phthalic anhydride is 1: 0.85.
3. the method for preparing the mud-resistant polycarboxylic acid slow-release agent for concrete according to claim 1, wherein the dosage of the benzoyl peroxide is 0.317 percent of the total mass of the prenyl polyoxyethylene ether.
4. The method for preparing the mud-resistant polycarboxylic acid slow-release agent for concrete according to claim 1, wherein the weight ratio of acrylic acid, acrylamide, hydroxyethyl acrylate: the mole ratio of the prenyl polyoxyethylene ether is 0.7:0.68:3.0: 1.0.
5. The method for preparing the mud-resistant polycarboxylic acid slow-release agent for concrete according to claim 1, wherein the molecular weight regulator AMSD is 0.476% of the total mass of the prenyl polyoxyethylene ether.
6. The method for preparing the mud-resistant polycarboxylic acid slow-release agent for concrete according to claim 1, wherein the reaction temperature in the step (4) is 80 ℃, the reaction time is 2 hours, the dropping time is 45 minutes, the heat preservation temperature is 70-80 ℃, and the heat preservation time is 3 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114276088A (en) * | 2022-01-18 | 2022-04-05 | 中国矿业大学 | High-strength building block material with high content of fly ash and preparation method thereof |
| CN114920889A (en) * | 2022-06-28 | 2022-08-19 | 江苏博思通新材料有限公司 | Long side chain adsorption type mud-resistant slump retaining agent and preparation method thereof |
Citations (2)
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| CN108948283A (en) * | 2018-05-31 | 2018-12-07 | 靖西市秀美边城农业科技有限公司 | A kind of phthalic anhydride modified polycarboxylic acid water-reducing agent and preparation method thereof |
| CN109734350A (en) * | 2019-01-10 | 2019-05-10 | 江苏福吉利亚建材有限公司 | A kind of polycarboxylate superplasticizer mother liquor and preparation method thereof |
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2019
- 2019-12-11 CN CN201911268051.1A patent/CN110951011A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108948283A (en) * | 2018-05-31 | 2018-12-07 | 靖西市秀美边城农业科技有限公司 | A kind of phthalic anhydride modified polycarboxylic acid water-reducing agent and preparation method thereof |
| CN109734350A (en) * | 2019-01-10 | 2019-05-10 | 江苏福吉利亚建材有限公司 | A kind of polycarboxylate superplasticizer mother liquor and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114276088A (en) * | 2022-01-18 | 2022-04-05 | 中国矿业大学 | High-strength building block material with high content of fly ash and preparation method thereof |
| CN114920889A (en) * | 2022-06-28 | 2022-08-19 | 江苏博思通新材料有限公司 | Long side chain adsorption type mud-resistant slump retaining agent and preparation method thereof |
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Application publication date: 20200403 |