CN112608058B - Concrete micro-foaming agent and preparation method thereof - Google Patents
Concrete micro-foaming agent and preparation method thereof Download PDFInfo
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- CN112608058B CN112608058B CN202011394872.2A CN202011394872A CN112608058B CN 112608058 B CN112608058 B CN 112608058B CN 202011394872 A CN202011394872 A CN 202011394872A CN 112608058 B CN112608058 B CN 112608058B
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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
- C04B24/16—Sulfur-containing compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/02—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
- C07C319/12—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by reactions not involving the formation of mercapto groups
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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 concrete micro-foaming agent which comprises the following components in parts by weight: sulfonating agent: 100-150 parts; alkali agent: 0 to 100 portions; unilateral condensing agent: 100-200 parts; a coupling agent: 200-400 parts; water: 250-600 parts of the concrete micro-foaming agent, which is a small molecular polymer and is obtained by carrying out unilateral condensation reaction on a unilateral condensing agent and other components, and has the advantages of good bubble stability, small influence of concrete stirring time and storage time, greatly improved workability, fluidity and construction performance of concrete, and higher water reducing rate and cost performance.
Description
Technical Field
The invention relates to the technical field of concrete additives, in particular to a concrete micro-foaming agent and a preparation method thereof.
Background
The concrete admixture has gradually outstanding technical advantages in the aspect of improving the performance of concrete, and the concrete microfoaming agent is used as one of the concrete admixtures, so that the workability of the concrete can be greatly improved, and the durability of the concrete can be greatly improved.
At present, the common concrete micro-foam agent in the market is an anionic surfactant, has surface active effects of air entraining, dispersing, wetting and the like, and mainly takes the air entraining effect as the main part, and mostly belongs to the category of rosin air entraining agents. The common anionic surfactant is mainly rosin sodium salt, however, the concrete micro-foaming agent of the anionic surfactant has the problems of poor stability, poor workability and excessive sensitivity to storage and stirring time in use. Therefore, the invention of the concrete micro-foaming agent with good stability, good workability and insensitivity to storage and stirring time has important significance for improving the performance of concrete.
Disclosure of Invention
Based on the above, there is a need to provide a concrete micro-foaming agent and a preparation method thereof, so as to realize the advantages of good stability, good workability and insensitivity to stirring time of the concrete micro-foaming agent.
In order to achieve the above object, the present invention provides a concrete micro-foaming agent, which comprises the following components in parts by weight:
sulfonating agent: 100-150 parts;
alkali agent: 0 to 100 portions;
unilateral condensing agent: 100-200 parts;
a coupling agent: 200-400 parts;
water: 250-600 parts.
Preferably, the sulfonating agent comprises one or more of sulfite, pyrosulfite and bisulfite.
Preferably, the sulfonating agent comprises one or more of sodium sulfite, sodium metabisulfite and sodium bisulfite.
Preferably, the one-sided condensing agent comprises one or more of butanone and butanone derivatives.
Preferably, the butanone derivative comprises one or more of methyl isobutyl ketone, 3-hydroxy butanone and 3-mercapto-2-butanone.
Preferably, the bridging agent comprises one or more of formaldehyde and acetaldehyde.
Preferably, the concentration of formaldehyde is 37%.
Preferably, the alkaline agent is one or more of sodium hydroxide and potassium hydroxide.
The invention also provides a preparation method of the concrete micro-foaming agent, which comprises the following steps:
(1) Mixing 100-150 parts of sulfonating agent and 200-400 parts of water, adding 0-100 parts of alkaline agent to adjust the pH value to 9.0-11.0, and fully stirring at 50-65 ℃ until the sulfonating agent and the alkaline agent are completely dissolved in the water to obtain a dissolved solution;
(2) Controlling the temperature in the step (1) to rise to 60-70 ℃, adding 100-200 parts of unilateral condensing agent and 200-400 parts of coupling agent into the dissolved solution, controlling the temperature to be 95-100 ℃, then preserving the heat for 4.0-6.0 h, and supplementing 50-200 parts of water after the heat preservation is finished, thus obtaining the concrete micro-foaming agent.
Preferably, in the step (1), the mixture is fully stirred at the temperature of between 50 and 65 ℃ for 10 to 30 minutes until the sulfonating agent and the alkaline agent are completely dissolved in the water, so as to obtain a dissolved solution.
The concrete micro-foaming agent has the beneficial effects that:
compared with the prior art, the concrete micro-foaming agent provided by the embodiment of the invention is prepared by carrying out unilateral condensation reaction on a unilateral condensation agent and other components to obtain the concrete micro-foaming agent of a small molecular polymer, and in addition, the concrete micro-foaming agent has the advantages of good bubble stability, small influence of concrete stirring time and storage time, great improvement on the workability, the flowability and the construction performance of concrete, and higher water reduction rate and cost performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The experimental procedures in the following examples are all conventional ones unless otherwise specified. Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified. In the quantitative tests in the following examples, three replicates were set, and the data are the mean value or the mean value ± standard deviation of the three replicates.
In addition, "and/or" in the whole text includes three schemes, taking a and/or B as an example, including a technical scheme, and a technical scheme that a and B meet simultaneously; in addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The embodiment of the invention provides a concrete micro-foaming agent, which comprises the following components in parts by weight:
sulfonating agent: 100-150 parts;
alkali agent: 0 to 100 portions;
unilateral condensing agent: 100-200 parts;
a coupling agent: 200-400 parts;
water: 250-600 parts.
Compared with the prior art, the concrete micro-foaming agent provided by the embodiment of the invention is prepared by carrying out unilateral condensation reaction on a unilateral condensation agent and other components to obtain the concrete micro-foaming agent of a small molecular polymer, and in addition, the concrete micro-foaming agent has the advantages of good bubble stability, small influence of concrete stirring time and storage time, great improvement on the workability, the flowability and the construction performance of concrete, and higher water reduction rate and cost performance.
In some embodiments, the sulfonating agent comprises one or more of sulfite, pyrosulfite and bisulfite, the sulfonic acid group of the sulfonating agent after being dissolved in water is hydrolyzed in an aqueous solution, so that the concrete micro-foaming agent reaction system is alkaline, and the condensation reaction of the components in the concrete micro-foaming agent reaction system is promoted to obtain a small-molecular polymer concrete micro-foaming agent, and the sulfonating agent can also perform sulfonation reaction with a unilateral condensing agent and a cross-linking agent in the concrete micro-foaming agent reaction system to provide hydroxyl and sulfonic acid groups, and further promote the condensation reaction.
Specifically, the sulfonating agent includes one or more of sodium sulfite, sodium metabisulfite and sodium bisulfite to more effectively promote the condensation reaction.
Specifically, the purity of the sodium sulfite is more than or equal to 96 percent, so that the reaction efficiency in the concrete micro-foaming agent reaction system is effectively improved.
Specifically, the purity of the sodium metabisulfite is more than or equal to 96 percent, so that the reaction efficiency in a concrete micro-foaming agent reaction system is effectively improved.
Specifically, the purity of the sodium bisulfite is more than or equal to 96 percent, so as to effectively improve the reaction efficiency in the concrete micro-foaming agent reaction system.
In some embodiments, the one-sided condensation agent comprises butanone or a butanone derivative, or butanone or a butanone derivative, wherein the carbonyl group of butanone or the butanone derivative is flanked on one side by a primary carbon, i.e., three hydrogens on the carbon, and on the other side by no primary carbon, such that the condensation reaction performed with butanone or the butanone derivative is a one-sided condensation reaction, and the resulting concrete micro-foam agent is a small-molecule polymer-based concrete micro-foam agent.
Specifically, the butanone derivatives comprise one or more of methyl isobutyl ketone, 3-hydroxy butanone and 3-mercapto-2-butanone.
In some embodiments, the crosslinking agent includes one or more of formaldehyde and acetaldehyde to effectively adjust the molecular weight of the concrete microfoaming agent to obtain the small molecule polymer-based concrete microfoaming agent of the present invention.
In some embodiments, the concentration of formaldehyde is 37% to more effectively adjust the molecular weight of the concrete micro-foaming agent, and the concentration of formaldehyde of 37% is a concentration capable of adapting to other components in the concrete micro-foaming agent reaction system to obtain the concrete micro-foaming agent with excellent performances, so that the excessive use of formaldehyde is avoided, and the environmental pollution is avoided.
In some embodiments, the concentration of acetaldehyde is 40% to more effectively adjust the molecular weight of the concrete micro-foaming agent, and the acetaldehyde with the concentration of 40% can adapt to other components in the concrete micro-foaming agent reaction system to obtain the concentration of the concrete micro-foaming agent with excellent performance, so that the acetaldehyde is not excessively used, and the energy-saving effect is achieved.
In some embodiments, the alkali agent is one or more of sodium hydroxide and potassium hydroxide, and the alkali agent is used for adjusting the pH value of the concrete micro-foam agent reaction system to 9.0-11.0 to achieve the alkaline environment required by the reaction under the condition that the hydrolysis of the sulfonic acid group in the sulfonating agent in water cannot enable the concrete micro-foam agent reaction system to achieve the alkaline environment required by the reaction.
In some embodiments, the alkaline agent comprises one or more of sodium hydroxide with a concentration of 50% and potassium hydroxide with a concentration of 50% to effectively adjust the pH of the concrete microfoamer reaction system to 9.0-11.0, thereby avoiding the pH of the concrete microfoamer reaction system from being incompatible with the pH required for the reaction.
The invention also provides a preparation method of the concrete micro-foaming agent, which comprises the following steps,
(1) Mixing 100-150 parts of sulfonating agent and 200-400 parts of water, adding 0-100 parts of alkaline agent to adjust the pH value to 9.0-11.0, and fully stirring at 50-65 ℃ until the sulfonating agent and the alkaline agent are completely dissolved in the water to obtain a dissolved solution;
(2) Controlling the temperature in the step (1) to rise to 60-70 ℃, adding 100-200 parts of unilateral condensing agent and 200-400 parts of coupling agent into the dissolved solution, controlling the temperature to be 95-100 ℃, then preserving the heat for 4.0-6.0 h, and supplementing 50-200 parts of water after the heat preservation is finished, thus obtaining the concrete micro-foaming agent.
Compared with the prior art, the embodiment of the invention provides a preparation method of a concrete micro-foaming agent, wherein a sulfonating agent is added into a concrete micro-foaming agent reaction system, the pH value is adjusted to 9.0-11.0 by an alkaline agent, then the mixture is fully stirred at 50-65 ℃ until the sulfonating agent and the alkaline agent are completely dissolved in water to obtain a dissolved solution, so that the concrete micro-foaming agent reaction system is in an alkaline environment to promote the subsequent single-side condensation reaction in the concrete micro-foaming agent reaction system, and a sulfonic acid group generated after the sulfonating agent is dissolved in water and the single-side condensation agent and the cross-linking agent in the concrete micro-foaming agent reaction system are subjected to sulfonation reaction to provide a hydroxyl group and a sulfonic acid group and can also promote the subsequent single-side condensation reaction; meanwhile, under an alkaline environment and under the conditions, the unilateral condensation reaction of the unilateral condensation agent and the coupling agent occurs in the dissolved solution, 50-200 parts of water is supplemented, and the concrete micro-foaming agent after the unilateral condensation reaction is finished is adjusted to be the required ideal concentration, so that the small-molecular polymer concrete micro-foaming agent is obtained, and the concentration is the required ideal concentration for construction.
In some embodiments, in the step (1), the mixture is fully stirred at 50-65 ℃ for 10-30 min until the sulfonating agent and the alkaline agent are completely dissolved in the water, so as to obtain a dissolved solution, so that the sulfonating agent and the alkaline agent are fully dissolved, and the stability of the dissolved solution is increased.
In some embodiments, in the step (2), after the heat preservation is finished, the temperature is reduced to 70-75 ℃, and 50-200 parts of water are supplemented, so that the concrete micro-foaming agent is obtained.
The technical solution of the present invention will be further described with reference to the preferred embodiments.
Example 1:
(1) Mixing 350 parts of water and 130 parts of sodium sulfite, adding 10 parts of 50% sodium hydroxide to adjust the pH to 9.0, and fully stirring for 20min at the temperature of 50-65 ℃ until the sulfonating agent and the alkaline agent are completely dissolved in the water to obtain a dissolved solution;
(2) And (2) controlling the temperature in the step (1) to rise to 65 ℃, adding 150 parts of butanone and 300 parts of formaldehyde into the dissolved solution, controlling the reaction temperature to be 96 ℃, preserving the heat for 4.0 hours, cooling to below 70 ℃ after the heat preservation is finished, and supplementing 100 parts of water to obtain the concrete micro-foaming agent.
Example 2:
(1) Mixing 350 parts of water and 100 parts of sodium metabisulfite, adding 80 parts of 50% sodium hydroxide to adjust the pH value to 10.0, and fully stirring for 20min at the temperature of 50-65 ℃ until the sulfonating agent and the alkaline agent are completely dissolved in the water to obtain a dissolved solution;
(2) And (2) controlling the temperature in the step (1) to rise to 65 ℃, adding 160 parts of 3-hydroxy butanone and 300 parts of formaldehyde into the dissolved solution, controlling the reaction temperature to be 96 ℃, preserving the heat for 4.0 hours, cooling to below 70 ℃ after the heat preservation is finished, and supplementing 50 parts of water to obtain the concrete micro-foaming agent.
Example 3
(1) Mixing 350 parts of water and 110 parts of sodium bisulfite, adding 50 parts of 50% sodium hydroxide to adjust the pH value to 10.0, and fully stirring for 20min at the temperature of 50-65 ℃ until the sulfonating agent and the alkaline agent are completely dissolved in the water to obtain a dissolved solution;
(2) And (2) controlling the temperature in the step (1) to rise to 68 ℃, adding 180 parts of 3-mercapto-2-butanone and 350 parts of acetaldehyde into the dissolved solution, controlling the reaction temperature to be 96 ℃, preserving heat for 5.0 hours, cooling to below 70 ℃ after the heat preservation is finished, and supplementing 120 parts of water to obtain the concrete micro-foaming agent.
Example 4
(1) Mixing 350 parts of water and 130 parts of sodium sulfite, adding 10 parts of 50% sodium hydroxide to adjust the pH to 10.0, and fully stirring for 20min at the temperature of 50-65 ℃ until the sulfonating agent and the alkaline agent are completely dissolved in the water to obtain a dissolved solution;
(2) And (2) controlling the temperature in the step (1) to rise to 68 ℃, adding 100 parts of butanone, 60 parts of 3-hydroxy butanone and 300 parts of formaldehyde into the dissolved solution, controlling the reaction temperature to be 96 ℃, preserving the heat for 4.0h, cooling to below 70 ℃ after the heat preservation is finished, and supplementing 100 parts of water to obtain the concrete micro-foam agent.
Performance evaluation
The performance of the concrete microfoams according to the invention was evaluated in combination with examples 1 to 4, and conventional concrete microfoams on the market.
Firstly, the concrete micro-foam agents obtained in examples 1-4 and the commercially available traditional concrete micro-foam agents are added into concrete of each group, and the concrete added with the concrete micro-foam agents in examples 1-4 and the commercially available traditional concrete micro-foam agents are stored and stirred for 60min, wherein the mixing ratio of the concrete of each group is shown in table 1, the concrete of each group is the same, southern P.O42.5R cement is adopted as the cement, coal ash is II-grade coal ash, mineral powder is S95 mineral powder, fine sand is fine sand with fineness modulus of 1.2, the manufactured sand is manufactured sand with fineness modulus of 3.0, the broken stone is continuous graded broken stone with particle size of 5-25, and the water reducing agent is polycarboxylic acid water reducing agent, wherein the amount of the polycarboxylic acid water reducing agent is 2.0% of the total mass of rubber materials including cement, coal ash, PCE, fine sand, PCE, crushed stone and water (PCE is 0% of the commercially available concrete micro-foam agents in examples 1-4), and the commercially available polycarboxylic acid water reducing agent is 0.0%. According to GB8076-2008 concrete admixture and GBT 50081-2002 common concrete mechanical property experiment method, different performance indexes are detected. The results are shown in Table 2.
TABLE 1 C30 concrete mixing ratio
TABLE 2 Performance testing of different concrete microfoamers
As can be seen from Table 2, the concrete microfoams of examples 1 to 4 of the invention have higher water reducing ratio of concrete and better workability than the conventional concrete microfoams of the market of comparative example 1 at the same mixing amount; secondly, the gas content of the sample in the comparative example 1 is changed from 1.0% to 0.2% within 0-60 min, however, in the invention, the gas content of the sample in the examples 1-4 is not obvious within 0-60 min, and the concrete micro-foaming agent has higher gas content, good bubble stability and small influence of concrete stirring and storage time; in addition, the samples in examples 1 to 4 of the present invention and the samples in comparative example 1 all had superior compressive strength in 7d to 28d, which indicates that the concrete micro-foam of the present invention has no significant effect on the compressive strength of the concrete at different ages and can make the concrete have superior strength, therefore, the concrete added with the concrete micro-foam of the present invention has the advantage of high strength.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.
Claims (5)
1. The concrete micro-foaming agent is characterized by comprising the following components in parts by weight:
sulfonating agent: 100-150 parts;
alkali agent: 0-100 parts;
single-side condensing agent: 100-200 parts;
a coupling agent: 200-400 parts;
water: 250-600 parts;
the unilateral condensing agent comprises one or more of butanone and butanone derivatives; wherein the butanone derivative comprises one or more of methyl isobutyl ketone, 3-hydroxy butanone and 3-mercapto-2-butanone;
the cross-linking agent comprises one or more of formaldehyde and acetaldehyde; wherein the concentration of the formaldehyde is 37 percent, and the concentration of the acetaldehyde is 40 percent;
the preparation method of the concrete micro-foaming agent comprises the following steps:
(1) Mixing 100-150 parts of sulfonating agent and 200-400 parts of water, adding 0-100 parts of alkaline agent to adjust the pH value to 9.0-11.0, and fully stirring at 50-65 ℃ until the sulfonating agent and the alkaline agent are completely dissolved in the water to obtain a dissolved solution;
(2) And (2) controlling the temperature in the step (1) to rise to 60-70 ℃, adding 100-200 parts of unilateral condensation agent and 200-400 parts of coupling agent into the dissolved solution, controlling the temperature to be 95-100 ℃, then preserving heat for 4.0-6.0 h, and supplementing 50-200 parts of water after the heat preservation is finished, thus obtaining the concrete micro-foaming agent.
2. The concrete microfoam agent of claim 1, wherein the sulfonating agent comprises one or more of a sulfite, a metabisulfite, and a bisulfite.
3. The concrete microfoam of claim 2, wherein the sulfonating agent comprises one or more of sodium sulfite, sodium metabisulfite, and sodium bisulfite.
4. The concrete microfoam agent as recited in claim 1, wherein said alkaline agent is one or more of sodium hydroxide and potassium hydroxide.
5. The concrete microfoam agent as claimed in claim 1, wherein in step (1), fully stirring is carried out at 50-65 ℃ for 10-30 min until the sulfonating agent and the alkaline agent are completely dissolved in water, so as to obtain a dissolved solution.
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| CN100415675C (en) * | 2003-12-31 | 2008-09-03 | 吴霖秀 | High efficiency aliphatic sulfonate water reducing agent and method for preparing same |
| JP2009019079A (en) * | 2007-07-10 | 2009-01-29 | Nippon Paper Chemicals Co Ltd | Method for producing water-soluble formaldehyde condensation product having reduced residual formaldehyde content |
| CN101508536B (en) * | 2009-03-20 | 2011-11-30 | 武汉市联合石油化工有限责任公司 | modified aliphatic water reducing agent and preparation method |
| CN101575186B (en) * | 2009-05-11 | 2012-06-20 | 江苏尼高科技有限公司 | Aliphatic concrete water reducing agent and preparation process thereof |
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| CN102276192B (en) * | 2011-05-11 | 2012-11-14 | 马清浩 | Grouting material containing phenol modified aliphatic water reducer and preparation method thereof |
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