CN117886535B - Internally-doped concrete compaction reinforcing agent and preparation method thereof - Google Patents
Internally-doped concrete compaction reinforcing agent and preparation method thereof Download PDFInfo
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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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- 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
- C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
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- 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
- C04B24/2652—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles
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- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/02—Acyclic radicals, not substituted by cyclic structures
- C07H15/04—Acyclic radicals, not substituted by cyclic structures attached to an oxygen atom of the saccharide radical
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- C07H15/02—Acyclic radicals, not substituted by cyclic structures
- C07H15/12—Acyclic radicals, not substituted by cyclic structures attached to a nitrogen atom of the saccharide radical
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
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- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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Abstract
The invention discloses an internal doped concrete compaction reinforcing agent and a preparation method thereof. The internal doped concrete compaction reinforcing agent is prepared from a hydration product growth modifying component, an accelerated cement mineral dissolving component and a crystal growth inhibiting component according to a mass ratio of 1:1:1 through a physical-chemical reaction, wherein the hydration product growth modifying component is alcohol amine, the accelerated cement mineral dissolving component is polyvinyl amine, and the crystal growth inhibiting component is a saccharide water-dispersible solution. The invention adopts a multi-component compounding method to regulate and control the density of early hydration products of cement-based materials, improve the later rate of cement hydration, and realize the compaction of microstructures and the improvement of strength.
Description
Technical Field
The invention belongs to the field of concrete additives, and particularly relates to an internal doped concrete compaction reinforcing agent and a preparation method thereof.
Background
Cement-based materials are the most widely used building materials worldwide and are also an important contributor to the growth of national economy. In the context of the national strategy of traffic, including the planning and construction of numerous infrastructures, such as roads, subways, tunnels, etc., due to the requirements of significant infrastructures for safety and life, the durability of cement-based materials must be considered during the construction phase. The durability problem of cement-based materials mainly relates to the degradation of concrete materials and the corrosion degradation of reinforcing steel bars, and the main process is that after cement serving as a main cementing material is hydrated and hardened, the slurry is in an alkaline environment to cause the formation of a compact oxide film on the surfaces of the reinforcing steel bars, so that the corrosion of the reinforcing steel bars is prevented. After harmful gas and erosion solution enter the concrete, the passivation film on the surface of the steel bar can be damaged by eroding the matrix of the cement-based material or reducing the PH value in the concrete. Thus, the means and methods of improving the durability of concrete by compacting the microstructure of the cement-based material are of paramount importance.
The dense microstructure exhibits enhanced strength and reduced permeability in macroscopic properties. The method for improving the microstructure compactness of the cement-based material by using the additive method has few reports, the retarder can directly improve the microstructure compactness of the cement-based material, the retarder can greatly improve the hydration rate and the hydration degree of the cement-based material in the later stage of cement hydration, the later-stage strength can be obviously improved in macroscopic performance, and the problems of construction and cracking can be brought by adding the retarder. In order to avoid the problem of delayed setting caused by retarder, the setting accelerating technology including alcohol amine and calcium chloride is matched with the water reducing agent to accelerate the early hydration process of cement so as to improve the strength, but the setting accelerating technology is found to reduce the later strength of concrete, and the common setting accelerator contains chlorine components to bring about the negative effects of corrosion of reinforcing steel bars and the like, and aldehyde substances can accelerate the hydration process of cement but have toxicity. Therefore, the chemical additive which can be added into the cement-based material to promote the later hydration of cement, enhance the microstructure compactness of the cement-based material and improve the strength of concrete must not introduce additional gas, cause the problem of corrosion of reinforcing steel bars and have the characteristic of no chemical toxicity to be used in the cement-based material.
The rate of cement hydration is reduced after the peak value is reached, the control mechanism is mainly caused by the influence on the transmission of hydration after the overlap joint of different products, the later reaction of cement hydration is accelerated, the density of hydration products generated in the earlier stage of cement hydration is required to be reduced, and the later hydration rate of cement hydration is improved.
Disclosure of Invention
Aiming at the problems of introducing extra gas into the reinforcing agent and corrosion of the reinforcing steel bars and the application defect of chemical toxicity, the invention provides an internally doped concrete compaction reinforcing agent and a preparation method thereof.
The invention adopts a compounding method to regulate and control the density of early hydration products of cement-based materials, improve the later rate of cement hydration, and realize the compaction of microstructures and the improvement of strength. By adopting the multi-component compounding method, on one hand, high-density hydrated calcium silicate is inhibited and non-static calcium hydroxide is induced to generate, so that the efficiency of water transmission into a non-hydrated area in the later hydration stage is improved, on the other hand, the dissolution rate of cement minerals is increased through chemical components, the number of reactants in the chemical reaction process is increased, the hydration degree of a cement-based material is finally improved, more hydration products are generated in unit time, the stacking and strength of the compact hydration products are improved, and the regulation and control of the microstructure of the cement-based material and the effective improvement of the durability are realized.
In order to achieve the aim, the invention provides an internal doped concrete compaction reinforcing agent, which is prepared from a hydration product growth modifying component, a cement mineral dissolution accelerating component and a crystal growth inhibiting component by a physicochemical reaction according to a mass ratio of 1:1:1;
the hydration product growth modification component is alcohol amine, and the mass of the hydration product growth modification component is 0.01% -0.03% of the mass of cement in concrete;
the accelerating cement mineral dissolution component is polyvinyl amine, and the mass of the accelerating cement mineral dissolution component is 0.01% -0.03% of the mass of cement in concrete;
the crystal growth inhibition component is a saccharide water dispersion solution, and the mass of the crystal growth inhibition component is 0.01% -0.03% of the mass of cement in the concrete;
the mass ratio of the saccharide to the alcohol amine in the saccharide water dispersion solution is 1:1 to 1:10.
Further, the saccharide of the present invention is a hemiacetal hydroxyl group-containing monosaccharide.
Further, the alcohol amine is selected from any one or more of monoethanolamine, diethanolamine and triethanolamine.
Further, the general formula of the polyvinyl amine is shown as follows: - [ CH 2-CH2-NH]x -where X has a value of 1,2 or 3.
Further, the saccharides in the aqueous dispersion solution of saccharides are specifically selected from any one or more of D-glucopyranose, D-galactopyranose, D-mannopyranose, L-rhamnose, L-arabinose, D-allose and D-altrose.
The invention also provides a preparation method of the internal doped concrete compaction reinforcing agent, which comprises the following steps: firstly, saccharide reacts with alcohol amine in a solvent for 24 hours at the temperature of 40-70 ℃, the solvent is removed by a distillation method after the reaction is finished to obtain a primary reactant, and then the primary reactant and the polyvinyl amine are uniformly mixed in an aqueous solution to obtain the internal doped concrete compaction reinforcing agent.
The solvent is one of water, toluene and ethanol solvent;
the mass ratio of the primary reactant to the polyvinyl amine is 1:1 to 1:10.
The reinforcing agent can be added into any He Shuini-based material, including cement concrete, cement mortar pure cement products and the like. The mixing amount of the internal mixing type concrete compaction reinforcing agent is 0.01-1.0% of the mass of the cementing material when the internal mixing type concrete compaction reinforcing agent is mixed into concrete. The invention aims to accelerate the post-reaction rate of cement, promote the generation of hydration products, improve the strength and the compactness of a microstructure, further improve the durability of cement-based materials and prolong the service life of concrete materials and structures.
The dense reinforcing agent obviously enhances the later hydration rate of concrete, improves the strength of the concrete, has no chemical toxicity, does not introduce gas, has nontoxic and easily available synthetic raw materials, and is applicable to industrial production.
Drawings
FIG. 1 shows the effect of varying amounts of reinforcing agent on the hydration level of cement according to the reference group of the present invention and example 1.
FIG. 2 shows the effect of varying amounts of the reinforcing agent of the baseline group of the present invention on the hydration rate of cement according to example 1.
FIG. 3 is a graph showing the nitrogen adsorption of cement 28 days after hydration of cement by different amounts of the reinforcing agent according to the reference group of the present invention than in example 1.
FIG. 4 shows the micropore variation of the cement after 28 days of hydration with different amounts of the reinforcing agent according to the reference group of the present invention than in example 1.
Detailed Description
For better illustration of the invention, examples are set forth below. However, the specific material ratios, process conditions, and results thereof described in the examples are illustrative of the present invention only and should not be construed as limiting the claims in the present invention.
The cement used in the examples of the invention is P.O.42.5 cement from the conch cement plant, and the chemical reagents are all purchased from Aba Ding Shiji company.
Example 1
A preparation method of an internal doped concrete compaction reinforcing agent comprises the following steps: 20g D-galactopyranose is added into a three-necked flask, 80L of water and 50g of monoethanolamine are sequentially added, the mixture is reacted for 24 hours at 50 ℃ under mechanical stirring, the mixture is cooled to room temperature and distilled to obtain a primary product, the primary product is dissolved into 100mL of water, and commercial 20g (HOCH 2CH2)2-NCH2CH2N-(CH2CH2OH)2 and the primary product are stirred and dissolved to obtain the reinforcing agent).
Example 2
A preparation method of an internal doped concrete compaction reinforcing agent comprises the following steps: 20g D-galactopyranose is added into a three-necked bottle, 80L of toluene and 30g of diethanolamine are sequentially added, the mixture is reacted for 22 hours at 60 ℃ under the condition of mechanical stirring, the mixture is cooled to room temperature and distilled to obtain a primary product, the primary product is dissolved into 100mL of water, and commercial 20g (HOCH 2CH2)2-NCH2CH2N-(CH2CH2OH)2 and the primary product are stirred and dissolved to obtain the reinforcing agent).
Example 3
A preparation method of an internal doped concrete compaction reinforcing agent comprises the following steps: 20g D-glucopyranose is added into a three-necked bottle, 80L of ethanol, 20g of monoethanolamine and 10g of triethanolamine are sequentially added, the mixture is reacted for 22 hours at 60 ℃ under mechanical stirring, the mixture is cooled to room temperature and distilled to obtain a primary product, the primary product is dissolved into 100mL of water, and commercial 20g (HOCH 2CH2)2-NCH2CH2N-(CH2CH2OH)2 and the primary product are stirred and dissolved to obtain the reinforcing agent).
Example 4
A preparation method of an internal doped concrete compaction reinforcing agent comprises the following steps: 20g L-arabinopyranose is added into a three-necked bottle, 80L of water and 30g of diethanolamine are sequentially added, the reaction is carried out for 26 hours at 40 ℃ under the condition of mechanical stirring, the primary product is obtained by distillation after cooling to room temperature, the primary product is dissolved into 100mL of water, and commercial 20g (HOCH 2CH2)2-NCH2CH2N-(CH2CH2OH)2 and the primary product are added, and the reinforcing agent is obtained after stirring and dissolving).
Example 5
A preparation method of an internal doped concrete compaction reinforcing agent comprises the following steps: 20g D-mannopyranose is added into a three-necked flask, 80L of water and 20g of diethanolamine are sequentially added, the mixture is reacted for 22 hours at 50 ℃ under the condition of mechanical stirring, the mixture is cooled to room temperature and distilled to obtain a primary product, the primary product is dissolved into 100mL of water, and 30g of commercial (HOCH 2CH2)3-NCH2CH2N-(CH2CH2OH)3 and the primary product are stirred and dissolved to obtain the reinforcing agent.
Example 6
A preparation method of an internal doped concrete compaction reinforcing agent comprises the following steps: 20g D-altopyranose was added to a three-necked flask, followed by the sequential addition of 80L of water and 20g of diethanolamine, reacted at 60℃for 24 hours under mechanical stirring, cooled to room temperature, distilled to give the primary product, dissolved in 100mL of water, and added with 30g of commercial (HOCH 2CH2)3-NCH2CH2N-(CH2CH2OH)3 and the primary product were dissolved under stirring to give the enhancer).
Example 7
A preparation method of an internal doped concrete compaction reinforcing agent comprises the following steps: 30g L-arabinopyranose was added to a three-necked flask, followed by the sequential addition of 80L of water and 40g of diethanolamine, reacted at 40℃for 26 hours under mechanical stirring, cooled to room temperature, distilled to give a primary product, dissolved in 100mL of water, and added with 30g of commercial (HOCH 2CH2)3-NCH2CH2N-(CH2CH2OH)3 and the primary product were dissolved under stirring to give an enhancer).
Comparative example 1
Triethanolamine, a commonly used enhancer, was used as a comparative example.
Application examples
Application example 1
The cement ratio of the concrete test piece is set to be 0.5, and the admixture is 0.02 percent, 0.05 percent and 0.10 percent of reinforcing agents of different types of cementing materials. Concrete test pieces with strength of C30 were prepared using 350kg cement, 1075kg cobble, 777kg sand and 175kg tap water as raw materials. The results of the standard curing of the molded concrete test pieces for 28d are shown in Table 1. No enhancer was present in the baseline group.
TABLE 1 early strength comparison of concrete with reinforcing agent
In table 1, the concrete materials added with different reinforcing agents have slightly enhanced strength for 7 days, but the strength is obviously enhanced with the increase of the doping amount for 28 days, as compared with the experimental results of the examples. Of these, example 1 is most effective. The better comparison result shows that the reinforcing agent has the effect of reinforcing the cement in the later hydration period, and the test result is shown in figure 1.
Application example 2
The effect of varying amounts of the reinforcing agent of example 1 on the degree of hydration of the cement is shown in FIGS. 1 and 2 using a trace thermal test to add 0.02%, 0.05%, 0.10% of the reinforcing agent of example 1. The results of the trace thermal examples in fig. 1 and 2 show that the cement still remains reacted after the deceleration period with increasing amounts of the reinforcing agent, and the results of the cumulative heat release test for cement hydration show that the cement hydration level is significantly higher than that of the reference sample, indicating that the cement maintains a higher hydration rate during the deceleration period and the later hydration period relative to the reference sample.
Application example 3
The pore structure of the cement after 28 days of hydration, to which 0.02%, 0.05%, 0.10% of the reinforcing agent of example 1 was added, was tested using a nitrogen adsorber, as shown in fig. 3 and 4. In order to determine the density of hydration products generated in the hydration process, the results of the nitrogen adsorption test carried out are shown in fig. 3 and 4, and the results show that the pore structure generated by cement hydration is obviously reduced along with the increase of the doping amount of the reinforcing agent, but the pore structure is obviously increased below 60 angstroms, and the increase of the pores of the initial hydration products after the reinforcing agent is added is proved, but the compaction effect on the later hydration products is obviously achieved.
Claims (7)
1. The internal doped concrete compaction reinforcing agent is characterized in that the reinforcing agent is prepared from a hydration product growth modification component, a cement mineral dissolution acceleration component and a crystal growth inhibition component by a physical-chemical reaction according to a mass ratio of 1:1:1;
the hydration product growth modification component is alcohol amine, and the mass of the hydration product growth modification component is 0.01% -0.03% of the mass of cement in concrete;
the accelerating cement mineral dissolution component is polyvinyl amine, and the mass of the accelerating cement mineral dissolution component is 0.01% -0.03% of the mass of cement in concrete;
the crystal growth inhibition component is a saccharide water dispersion solution, and the mass of the crystal growth inhibition component is 0.01% -0.03% of the mass of cement in the concrete;
The mass ratio of the saccharide to the alcohol amine is 1:1 to 1:10; the saccharide is a monosaccharide containing hemiacetal hydroxyl, and is specifically selected from more than one of D-glucopyranose, D-mannopyranose, L-rhamnopyranose, L-arabinopyranose, D-allopyranose and D-altrose;
The preparation method of the reinforcing agent comprises the following steps: firstly, reacting saccharides with alcohol amine in a solvent for 24 hours at the temperature of 40-70 ℃, removing the solvent by a distillation method after the reaction is finished to obtain a primary reactant, and uniformly mixing the primary reactant with polyvinyl amine in an aqueous solution to obtain the internal doped concrete compaction reinforcing agent.
2. The internally doped concrete compaction reinforcing agent according to claim 1, wherein the alcohol amine is selected from any one or more of monoethanolamine, diethanolamine and triethanolamine.
3. The internally doped concrete compaction enhancer of claim 1, wherein the polyvinyl amine has the formula: - [ CH 2-CH2-NH]x -where X has a value of 1, 2 or 3.
4. The internally doped concrete compaction enhancer of claim 1, wherein the mass ratio of the primary reactant to the polyvinylamine is 1:1 to 1:10.
5. The internally doped concrete compaction enhancer of claim 1, wherein the solvent is one of water, toluene, and ethanol.
6. A method of using the internal mix concrete compaction enhancer of any one of claims 1 to 4, wherein the enhancer is used in a cement-based material.
7. The method of claim 6, wherein the amount of the internal mix concrete compaction enhancer added to the concrete is 0.01% -1.0% of the mass of the cementitious material.
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| EP1980541A4 (en) * | 2006-01-26 | 2011-09-07 | Sika Ltd | Cement dispersing agent |
| CN101516801B (en) * | 2006-09-13 | 2012-07-18 | 东邦化学工业株式会社 | Cement dispersant |
| US20110120349A1 (en) * | 2009-11-24 | 2011-05-26 | E. Khashoggi Industries, Llc | Extruded fiber reinforced cementitious products having stone-like properties and methods of making the same |
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