CN114195421A - Preparation method of polycarboxylic acid admixture for machine-made sand concrete - Google Patents
Preparation method of polycarboxylic acid admixture for machine-made sand concrete Download PDFInfo
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- CN114195421A CN114195421A CN202010981041.9A CN202010981041A CN114195421A CN 114195421 A CN114195421 A CN 114195421A CN 202010981041 A CN202010981041 A CN 202010981041A CN 114195421 A CN114195421 A CN 114195421A
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/32—Polyethers, e.g. alkylphenol polyglycolether
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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
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
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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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
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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
- 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
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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
Abstract
The invention relates to a preparation method of a polycarboxylic admixture for machine-made sand concrete, which comprises the following steps: (1) preparing an anti-mud polycarboxylic acid water reducer mother liquor taking ethylene glycol monovinyl polyglycol ether (EPEG) monomers as a main reaction unit, and (2) compounding the anti-mud polycarboxylic acid water reducer mother liquor, polyether phosphate, a foam control agent, a concrete viscosity regulator and water according to a proportion at normal temperature to obtain the polycarboxylic acid admixture for machine-made sand concrete. The polycarboxylic acid admixture for machine-made sand concrete provided by the invention has the advantages of high water reducing rate, strong material adaptability, stronger slump loss control capability and concrete workability improvement effect by inhibiting concrete large air bubbles, and has obvious workability improvement and strength increase effects on machine-made sand concrete with graded composition and containing much stone powder (6-12%).
Description
Technical Field
The invention belongs to the field of cement-based concrete admixtures, is suitable for machine-made sand concrete with serious gradation and high stone powder content, and particularly relates to a preparation method of a polycarboxylic acid admixture for the machine-made sand concrete.
Background
Because the situation of resource shortage is not relieved more and more, the machine-made sand concrete is widely applied as an important building material in recent years, and because the phenomenon of grading is serious and the content of stone powder is high, the mixed concrete mixture has high viscosity, poor fluidity and poor working performance, and is easy to generate the phenomena of bleeding and segregation. The main method for solving the problems is to compound a proper amount of air entraining agent by an aliphatic water reducing agent and a naphthalene water reducing agent, and the aliphatic water reducing agent and the naphthalene water reducing agent belong to a second-generation water reducing agent, so that the production cost is high, the environmental pollution is easily caused, the water reducing rate of the concrete is low although the aliphatic water reducing agent and the naphthalene water reducing agent have the advantage of good material adaptability, and the performance of the concrete can not meet the requirements when high-performance concrete is prepared. Although the water reducing rate of the common polycarboxylic acid water reducing agent can meet the requirement, the common polycarboxylic acid water reducing agent has poor adaptability to machine-made sand with large stone powder content fluctuation and fine sand with large mud content fluctuation, and phenomena of segregation, bleeding, bottom scraping and the like are caused frequently, so that the working performance, the strength and other performances of concrete are influenced.
For example, patent publication No. CN 109627394A discloses a water reducer for adaptive machine-made sand concrete and a preparation method thereof. Specifically, the method comprises the steps of initiating a free copolymerization reaction by using isobutenol polyoxyethylene ether, acrylic acid and 2-acrylamidododecyl sulfonic acid as main reaction units at the temperature of 55-75 ℃ under an oxidation-reduction reaction system, and neutralizing by using organic base after the reaction is finished to obtain the polycarboxylic acid water reducing agent suitable for machine-made sand concrete. The scheme provided by the patent is based on the idea of taking the polyoxyethylene methacrylate as a reaction main body, and has the advantages of limited performance space, complex production process and higher production energy consumption compared with the idea of ethylene glycol monovinyl polyglycol ether (EPEG) monomer.
Also, for example, patent publication No. CN 111153627A discloses a mud-resistant admixture suitable for machine-made sand concrete and a compounding method thereof. The main method is to compound the viscosity reduction type polycarboxylate superplasticizer, the lignin superplasticizer, water and the defoaming agent. The performance of the machine-made sand is changed by changing the mass ratio and the adding sequence of the lignin water reducing agent, and compared with the prior art, the cohesiveness and the compressive strength of the machine-made sand concrete can be improved. The patent mainly describes that a viscosity reduction type polycarboxylate superplasticizer, a lignin water reducer and a defoaming agent are compounded to prepare a mud-resistant additive suitable for machine-made sand concrete. The main raw material of the viscosity-reducing polycarboxylic acid provided by the patent is methacrylic acid-polyethylene glycol methyl ether ester, and the production process of the raw material needs a high-temperature esterification process, so that the production period is long, and the energy consumption is high. And the slump loss resistance of the concrete is poor by utilizing the lignosulfonate water reducing agent of the anti-mud additive product.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to overcome the defects in the prior art, a novel preparation method of a polycarboxylic acid admixture for machine-made sand concrete is provided.
The technical scheme adopted by the invention is as follows: a preparation method of a polycarboxylic admixture for machine-made sand concrete is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: dissolving ethylene glycol monovinyl polyglycol ether monomer in water to obtain a solution as a bottom material, dissolving acrylic acid and a chain transfer agent in water to obtain a mixed solution as a material A, and dissolving a reducing agent in water to obtain a solution as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 27.5% hydrogen peroxide by mass into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1-1.5 h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40% to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water in proportion at normal temperature, wherein the mass parts of the materials are as follows:
thus obtaining the polycarboxylic acid admixture for machine-made sand concrete.
Ethylene glycol monovinyl polyglycol ether (EPEG) monomer is taken as a main synthesis unit and is copolymerized with acrylic acid and derivatives thereof under the action of an oxidation-reduction initiation system to synthesize the anti-mud water reducer with a comb-type molecular structure, and the water reducing rate of concrete is more than or equal to 32 percent; the problems of large slump loss, poor material adaptability and the like are solved by compounding the concrete with polyether phosphate and an organic foam control agent, and the strength of the concrete can be obviously improved; by compounding with the concrete viscosity regulator, the phenomena of segregation, bleeding, bottom scraping and the like caused by machine-made sand grading, stone powder fluctuation and fine sand mud content fluctuation are solved.
The molar ratio of the ether group of the ethylene glycol monovinyl polyglycol ether in the bottom material in the step (1) I to the acid group of the acrylic acid in the material A is 3-5: 1.
in the step (1) I, the mass ratio of the base material to the solute of the material A is 1: 0.05 to 0.15.
The molecular weight of the ethylene glycol monovinyl polyglycol ether in the base material in the step (1) I is 2400, 3000 or 6000.
In the step (1) I, the chain transfer agent in the material A is one or a mixture of two of mercaptopropionic acid and mercaptoacetic acid.
The reducing agent of the material B in the step (1) I is a low-temperature reducing agent (H001) which can perform oxidation-reduction reaction with hydrogen peroxide under the low-temperature condition.
In the step (1) II, the mass ratio of the hydrogen peroxide to the solute of the material B is 0.8-2: 1.
the ratio of the solute mass sum of the base material monomer EPEG in the step (1) II to the hydrogen peroxide and the B material is 100: 0.3 to 0.8.
The concrete water reducing rate of the anti-mud polycarboxylic acid water reducing agent prepared in the step (1) can reach more than 32%, and the anti-mud polycarboxylic acid water reducing agent has certain slump retaining performance.
The organic foam control agent in the step (2) is organic alkynol substances, has the effects of inhibiting the generation of large concrete bubbles and introducing micro bubbles, and can directly replace the combination of the traditional organic silicon, polyether foam control agent and air entraining agent.
And (3) the polyether phosphate in the step (2) is an organic micromolecule substance which has certain retarding and slump retaining effects on concrete and can increase the compressive strength.
The concrete viscosity regulator in the step (2) is a biological polymerization additive, can change the rheological property of concrete, has a certain water retention effect, and ensures that the phenomena of segregation, bleeding, bottom raking and the like are not easy to occur when the concrete uses the step-off machine-made sand and contains more stone powder.
The synthesized polycarboxylate superplasticizer mother liquor is prepared by taking ethylene glycol monovinyl polyglycol ether (EPEG) monomer as a main raw material and carrying out free radical copolymerization reaction with acrylic acid or derivatives thereof under the initiation action of an oxidation-reduction reaction system to generate a polycarboxylate superplasticizer with a comb-type molecular structure. Compared with a polycarboxylic acid water reducing agent synthesized by traditional isobutenol polyoxyethylene ether (HPEG) and prenol polyoxyethylene ether (TPEG), the polycarboxylic acid water reducing agent has a larger rotation angle, and because double bonds in EPEG molecules are of a substituted structure, the space resistance of swinging of a polyether side chain is further reduced, so that the swinging of the polyether side chain is more free, and the moving range is larger; the increase of the swinging freedom degree of the polyether side chain improves the wrapping property and the winding property of the polyether side chain, so that the synthesized polycarboxylate superplasticizer has better adaptability, and particularly has obvious effects on the conditions of poor quality of sand and stone materials and high mud content.
The polyether phosphate selected in the invention is mainly an organic molecular compound containing phosphate ester structure, has obvious inhibition effect on excessive adsorption of stone powder and fine sand in machine-made sand to the polycarboxylic acid water reducing agent, mainly has the effect of controlling slump loss, has certain dispersion effect on cement, and can effectively increase the middle and later stage strength of concrete.
The organic alkynol foam control agent can control the size of bubbles in concrete, eliminate large bubbles which have harmful effects on the concrete, and leave small bubbles which have the effect of improving the fluidity and durability of the concrete, so that the traditional components of a defoaming agent and an air entraining agent are replaced; and the modified polycarboxylate superplasticizer has good compatibility with a polycarboxylate superplasticizer, and quality fluctuation caused by layering is not easy to occur.
Under the condition that the content of stone powder in machine-made sand and the content of mud in fine sand are high, a water reducing agent synthesized by using HPEG and TPEG monomers as main raw materials is easy to be absorbed too fast, the slump loss is high, the workability of mixed concrete is poor, the phenomena of segregation and bleeding are serious, and the performance of the concrete cannot be obviously improved by simply increasing the mixing amount of the water reducing agent. Therefore, the invention synthesizes the polycarboxylate superplasticizer with smaller polyether side chain space activity resistance and larger freedom degree by taking the EPEG as a main body, and has better effect on the aspects of preparing machine-made sand and high-fine sand containing mud. The addition of the polyether phosphate can significantly reduce slump loss and can increase strength. The introduction of the organic foam control agent can obviously adjust the bubble structure of the concrete, eliminate large bubbles, introduce small bubbles and improve the fluidity of the concrete. The concrete viscosity regulating material has the functions of improving the water retention of concrete and improving segregation and bleeding phenomena.
Compared with the prior art, the invention has the following advantages:
1. the polycarboxylate superplasticizer prepared by the invention effectively solves the problems of large concrete slump loss, poor workability, insufficient strength and the like caused by large content of machine-made sand powder and broken gradation.
2. The invention combines the anti-mud polycarboxylic mother liquor with polyether phosphate, organic alkynol foam control agent, viscosity regulator and water, and obviously overcomes the defects of large concrete loss, poor fluidity and poor workability.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the embodiments of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: a solution obtained by dissolving 300 parts by mass of ethylene glycol monovinyl polyglycol ether (EPEG-3000) monomer in 200 parts by mass of water is used as a base material, a mixed solution obtained by dissolving 35 parts by mass of acrylic acid and 1.8 parts by mass of mercaptopropionic acid in 15 parts by mass of water is used as a material A, and a solution obtained by dissolving 0.6 part by mass of reducing agent in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 3.5 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
and obtaining the polycarboxylic acid admixture for machine-made sand concrete, wherein the initial slump/expansion, 1h slump/expansion, 7d compressive strength and 28d compressive strength of the obtained anti-mud polycarboxylic acid admixture are 230/580 × 570mm, 200/510 × 500mm, 25.5MP and 33.5MP respectively.
Example 2
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: a solution of 240 parts by mass of ethylene glycol monovinyl polyglycol ether (EPEG-2400) monomer dissolved in 200 parts by mass of water is used as a base material, a mixed solution of 35 parts by mass of acrylic acid and 1.8 parts by mass of mercaptopropionic acid dissolved in 15 parts by mass of water is used as a material A, and a solution of 0.6 part by mass of a reducing agent dissolved in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 3.5 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
the polycarboxylic acid admixture for machine-made sand concrete is obtained, and the initial slump/expansion, 1h slump/expansion, 7d compressive strength and 28d compressive strength of the obtained anti-mud polycarboxylic acid admixture are 230/580 × 580mm, 200/510 × 520mm, 25.0MP and 33.8MP respectively.
Example 3
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: 300 parts by mass of a solution obtained by dissolving ethylene glycol monovinyl polyglycol ether (EPEG-6000) monomer in 200 parts by mass of water is used as a base material, a mixed solution obtained by dissolving 30 parts by mass of acrylic acid and 1.5 parts by mass of mercaptopropionic acid in 15 parts by mass of water is used as a material A, and a solution obtained by dissolving 1.0 part by mass of a reducing agent in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 4.0 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
the polycarboxylic acid admixture for machine-made sand concrete is obtained, and the initial slump/expansion, 1h slump/expansion, 7d compressive strength and 28d compressive strength of the obtained anti-mud polycarboxylic acid admixture are 230/575 × 570mm, 190/500 × 530mm, 26.6MP and 34.5MP respectively.
Example 4
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: a solution obtained by dissolving 300 parts by mass of ethylene glycol monovinyl polyglycol ether (EPEG-3000) monomer in 200 parts by mass of water is used as a base material, a mixed solution obtained by dissolving 30 parts by mass of acrylic acid and 1.8 parts by mass of mercaptopropionic acid in 15 parts by mass of water is used as a material A, and a solution obtained by dissolving 0.8 part by mass of reducing agent in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 3.5 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
the polycarboxylic acid admixture for machine-made sand concrete is obtained, and the initial slump/expansion, 1h slump/expansion, 7d compressive strength and 28d compressive strength of the obtained anti-mud polycarboxylic acid admixture are 230/590 × 580mm, 210/530 × 520mm, 26.5MP and 35.2MP respectively.
Example 5
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: a solution obtained by dissolving 300 parts by mass of ethylene glycol monovinyl polyglycol ether (EPEG-3000) monomer in 200 parts by mass of water is used as a base material, a mixed solution obtained by dissolving 30 parts by mass of acrylic acid and 1.8 parts by mass of mercaptopropionic acid in 15 parts by mass of water is used as a material A, and a solution obtained by dissolving 0.8 part by mass of reducing agent in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 3.5 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
the polycarboxylic acid admixture for machine-made sand concrete is obtained, and the obtained anti-mud polycarboxylic acid admixture has the concrete initial slump/expansion, 1h slump/expansion, 7d compressive strength and 28d compressive strength of 230/580 × 580mm, 220/530 × 550mm, 27.0MP and 36.9MP respectively.
Example 6
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: a solution obtained by dissolving 300 parts by mass of ethylene glycol monovinyl polyglycol ether (EPEG-3000) monomer in 200 parts by mass of water is used as a base material, a mixed solution obtained by dissolving 30 parts by mass of acrylic acid and 1.8 parts by mass of mercaptopropionic acid in 15 parts by mass of water is used as a material A, and a solution obtained by dissolving 0.8 part by mass of reducing agent in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 3.5 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
and obtaining the polycarboxylic acid admixture for machine-made sand concrete, wherein the initial slump/expansion, 1h slump/expansion, 7d compressive strength and 28d compressive strength of the obtained anti-mud polycarboxylic acid admixture are 240/590 × 600mm, 220/550 × 560mm, 28.9MP and 37.8MP respectively.
Example 7
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: a solution obtained by dissolving 300 parts by mass of ethylene glycol monovinyl polyglycol ether (EPEG-3000) monomer in 200 parts by mass of water is used as a base material, a mixed solution obtained by dissolving 30 parts by mass of acrylic acid and 1.8 parts by mass of mercaptopropionic acid in 15 parts by mass of water is used as a material A, and a solution obtained by dissolving 0.8 part by mass of reducing agent in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 3.5 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
and obtaining the polycarboxylic acid admixture for the machine-made sand concrete, wherein the initial slump/expansion, the 1h slump/expansion, the 7d compressive strength and the 28d compressive strength of the obtained anti-mud polycarboxylic acid admixture are 230/580 × 575mm, 200/510 × 505mm, 25.9MP and 33.8MP respectively.
Example 8
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: a solution obtained by dissolving 300 parts by mass of ethylene glycol monovinyl polyglycol ether (EPEG-3000) monomer in 200 parts by mass of water is used as a base material, a mixed solution obtained by dissolving 30 parts by mass of acrylic acid and 1.8 parts by mass of mercaptopropionic acid in 15 parts by mass of water is used as a material A, and a solution obtained by dissolving 0.8 part by mass of reducing agent in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 3.5 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
the polycarboxylic acid admixture for machine-made sand concrete is obtained, and the initial slump/expansion, 1h slump/expansion, 7d compressive strength and 28d compressive strength of the obtained anti-mud polycarboxylic acid admixture are 230/580 × 580mm, 200/510 × 510mm, 26.3MP and 34.7MP respectively.
Example 9
A method for preparing a polycarboxylic acid admixture for machine-made sand concrete comprises the following steps,
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: a solution obtained by dissolving 300 parts by mass of ethylene glycol monovinyl polyglycol ether (EPEG-3000) monomer in 200 parts by mass of water is used as a base material, a mixed solution obtained by dissolving 30 parts by mass of acrylic acid and 1.8 parts by mass of mercaptopropionic acid in 15 parts by mass of water is used as a material A, and a solution obtained by dissolving 0.6 part by mass of reducing agent in 40 parts by mass of water is used as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 3.5 parts by mass of 27.5% hydrogen peroxide into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1.5h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40%, so as to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer, wherein the water reducing rate of the concrete is more than or equal to 32%;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water at normal temperature (10-35 ℃) in proportion, wherein the mass parts of the materials are as follows:
the polycarboxylic acid admixture for machine-made sand concrete is obtained, and the initial slump/expansion, 1h slump/expansion, 7d compressive strength and 28d compressive strength of the obtained anti-mud polycarboxylic acid admixture are 240/590 × 610mm, 220/550 × 570mm, 29.3MP and 38.4MP respectively.
Concrete properties of the concrete of the mud resistant polycarboxylic acid admixture prepared in the above examples 1 to 9 are shown in the following Table 1.1.
TABLE 1.1 comparison of concrete Properties
The polycarboxylic acid admixture concrete for machine-made sand concrete prepared by the embodiment has high water reducing rate, strong slump loss resistance and good concrete workability, and the compressive strength of the concrete is obviously improved by 7d and 28 d.
The embodiments described above are described to facilitate understanding and invention by those of ordinary skill in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made and the generic principles described herein may be applied to other embodiments. The present invention is not limited to the above embodiments, and those skilled in the art can make improvements and modifications without departing from the scope of the present invention by interpreting the present invention.
Claims (9)
1. A preparation method of a polycarboxylic admixture for machine-made sand concrete is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of anti-mud polycarboxylate superplasticizer mother liquor
I. Preparing materials: dissolving ethylene glycol monovinyl polyglycol ether monomer in water to obtain a solution as a bottom material, dissolving acrylic acid and a chain transfer agent in water to obtain a mixed solution as a material A, and dissolving a reducing agent in water to obtain a solution as a material B;
II, oxidation reduction: adding the base material obtained in the step I into a reaction kettle, controlling the temperature in the reaction kettle to be 5-16 ℃, adding 27.5% hydrogen peroxide by mass into the reaction kettle, uniformly stirring, dropwise adding the material A and the material B into the reaction kettle for 1-1.5 h, and preserving the temperature of the reaction kettle for 1h at 25-35 ℃;
neutralization: adding alkali liquor into the product obtained in the step (II) for neutralization, adjusting the pH value to 5-7.5, and adding water until the solid content is 40% to obtain a mother liquor of the anti-mud polycarboxylate superplasticizer;
(2) compounding
Compounding the anti-mud polycarboxylate superplasticizer mother liquor obtained in the step (1) III with polyether phosphate, a foam control agent, a viscosity regulator and water in proportion at normal temperature, wherein the mass parts of the materials are as follows:
thus obtaining the polycarboxylic acid admixture for machine-made sand concrete.
2. The method for preparing a polycarboxylic acid admixture for machine-made sand concrete according to claim 1, characterized in that: the mole ratio of the ether group of the ethylene glycol monovinyl polyglycol ether in the bottom material in the step (1) I to the acid group of the acrylic acid in the material A is 3.5-5: 1.
3. the method for preparing a polycarboxylic acid admixture for machine-made sand concrete according to claim 1, characterized in that: in the step (1) I, the mass ratio of the base material to the solute of the material A is 1: 0.05 to 0.15.
4. The method for preparing a polycarboxylic acid admixture for machine-made sand concrete according to claim 1, characterized in that: the molecular weight of the ethylene glycol monovinyl polyglycol ether in the base material in the step (1) I is 2400, 3000 or 6000.
5. The method for preparing a polycarboxylic acid admixture for machine-made sand concrete according to claim 1, characterized in that: in the step (1) I, the chain transfer agent in the material A is one or a mixture of two of mercaptopropionic acid and mercaptoacetic acid.
6. The method for preparing a polycarboxylic acid admixture for machine-made sand concrete according to claim 1, characterized in that: in the step (1) II, the mass ratio of the hydrogen peroxide to the solute of the material B is 0.8-2: 1.
7. the method for preparing a polycarboxylic acid admixture for machine-made sand concrete according to claim 1, characterized in that: the ratio of the mass of the ethylene glycol monovinyl polyglycol ether monomer serving as the base material in the step (1) II to the mass sum of the solutes of the hydrogen peroxide and the material B is 100: 0.3 to 0.8.
8. The method for preparing a polycarboxylic acid admixture for machine-made sand concrete according to claim 1, characterized in that: the organic foam control agent in the step (2) is organic alkynol.
9. The method for preparing a polycarboxylic acid admixture for machine-made sand concrete according to claim 1, characterized in that: the viscosity regulator in the step (2) is a biological polymerization additive.
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