CN111943547B - Method for preparing cement-based material carbonization internal curing agent through surface hydrophobic modification - Google Patents
Method for preparing cement-based material carbonization internal curing agent through surface hydrophobic modification Download PDFInfo
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- CN111943547B CN111943547B CN202010860721.5A CN202010860721A CN111943547B CN 111943547 B CN111943547 B CN 111943547B CN 202010860721 A CN202010860721 A CN 202010860721A CN 111943547 B CN111943547 B CN 111943547B
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- cement
- based material
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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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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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
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1051—Organo-metallic compounds; Organo-silicon compounds, e.g. bentone
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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
- C04B40/02—Selection of the hardening environment
- C04B40/0231—Carbon dioxide hardening
Abstract
The invention provides a method for preparing a cement-based material carbonization internal curing agent through surface hydrophobic modification2And adsorbing to obtain the cement-based material carbonized internal curing agent. The carbonization internal curing agent solves the technical defects that the carbonization reaction degree is low, the water-cement ratio of the material is low, the working performance is poor, the field application cannot be realized due to the limitation of high-pressure curing equipment and the like in the carbonization curing process of the existing cement-based material. The invention takes the molecular sieve after the release control treatment as CO2A carrier not only for CO2More of the introduction into the interior of the cement-based material may also control its release behavior. The carbonized internal curing agent can break through the limitation of curing equipment to realize the field application of carbonized curing on cement-based materials under the condition of not reducing the water cement ratio of the cement-based materials.
Description
The patent application of the invention is based on the application number: 202010233016.2, application name: a cement-based material carbonization internal curing agent and a preparation and use method thereof are disclosed in the application date: divisional patent application of the invention patent application on 3/28/2020.
Technical Field
The invention provides a cement-based material carbonization internal curing agent, and a preparation and use method thereof, belonging to the technical field of building materials.
Background
The carbonization and maintenance is to put the cement-based material such as plain concrete or mortar without steel bars into high-pressure CO after forming2Curing in atmosphere, mineral and CO in cement2A chemical reaction occurs, so that the cement-based material is coagulated and hardened in a short time, also known as CO2Curing or accelerated carbonization curing is a method capable of realizing CO2A novel maintenance mode of sealing and storing and utilizing. The cement-based material can obtain higher early strength after carbonization and maintenance, greatly shortens the concrete maintenance time, and has better dimensional stability, reduced porosity and improved mechanical property and durability. CO22In the process, calcium carbonate (CaCO)3) The curing in a stable form in the cement-based material does not have the risk of escaping again, and the CO is realized while the resource utilization is realized2The security of (2) is sealed. Compared with conventional hydration curing and steam curing, the carbonization curing not only accelerates the strength development of the cement-based material, improves the curing efficiency, but also improves the material performance and reduces the curing energy consumption.
However, CO2The diffusion problems in cement-based materials cause their use in cement-based materials to remain with the following problems: (1) the carbonization reaction only takes place in the range of the material surface layer, the whole reaction degree is lower, and the promotion range of the material performance and the solid carbon amount are both limited. The general cement-based material has the working performance requirement, the mixing water quantity is higher than the theoretical water quantity of cement hydration, and CO is2The solubility in pure water is low at normal temperature and pressure, and excessive free water blocks CO2The cement-based material is permeated into the interior of the material, so that the carbonization reaction degree of the cement-based material is greatly reduced. In addition, CaCO formed by preliminary carbonization3Can refine or block partial pores and block CO in later period2Continue to diffuse into the material. (2) The method is generally applied to cement-based materials with low water-cement ratio, dry hardness and compression molding, and has a limited application range. In order to improve the carbonization reaction degree and reduce the barrier effect of free water, the cement-based material for carbonization curing is often very low in water-cement ratio, basically has no fluidity and has the characteristics of dry hardness, and the cement-based material is generally molded in a compression mode, so that the application range is greatly limited. (3) The carbonization and maintenance needs high-pressure maintenance equipment, and the field application of the carbonization and maintenance in the cement-based material cannot be realized. To increase CO2The diffusion depth in cement-based materials is often increased by increasing the CO content2The method for curing pressure ensures that carbonization curing cannot get rid of the limitation of special high-pressure curing equipment and cannot be applied on site.
In chinese patent CN201910036456, an in-situ carbonization method for improving structural properties of carbonized products, bacterial powder is added into the carbonized products, and in the later maintenance process, the bacteria contact with urea nutrient solution to perform ureolysis reaction, and urea is decomposed into carbon dioxide and water by the metabolism of the urea, so that carbonate ions are generated from the inside to achieve the carbonization process from inside to outside. Chinese patent CN 201910059816-preparation method of waterproof and pressure-resistant autoclaved aerated concrete block, modified tetratitanic acid is added when the waterproof and pressure-resistant autoclaved aerated concrete block is prepared, the added nano-silica is modified and the surface of the nano-silica is grafted with amino, when the tetratitanic acid is modified, the aminated nano-silica can enter an interlayer structure of the tetratitanic acid, and the nano-silica modified by the amino has carbon dioxide adsorption property, so that after entering the product along with the modified tetratitanic acid, the carbon dioxide can be released under the action of high temperature and high pressure in the preparation process of the product, and the product has the function of air entraining. Although the air-entraining is performed by a chemical reaction method in the above two patents, the problems in the background art can be solved, but the disadvantages of high cost and complicated preparation steps still exist.
Disclosure of Invention
The invention provides a cement-based material carbonization internal curing agent and a preparation and use method thereof, which solve the technical defects of low carbonization reaction degree, low material water-cement ratio, poor working performance, no on-site application limited by high-pressure curing equipment and the like in the cement-based material carbonization curing process in the background technology2The gas may also control its release behavior inside the material. The carbonized internal curing agent can break through the limitation of curing equipment to realize the field application of carbonized curing on cement-based materials under the condition of not reducing the water cement ratio of the cement-based materials.
The technical scheme adopted for realizing the above purpose of the invention is as follows:
a cement-based material carbonization internal curing agent is prepared by the following method: the molecular sieve is used as a raw material, subjected to surface hydrophobic modification or surface coating release control treatment to have hydrophobic property, and then subjected to CO treatment2And adsorbing to obtain the cement-based material carbonized internal curing agent.
The molecular sieve is rod-shaped particles, spherical particles or powder.
The molecular sieve comprises the following models: more than one of A type, X type, Y type and ZSM type.
The surface coating release control treatment is carried out on the molecular sieves of the rod-shaped particles and the spherical particles, and the specific method comprises the following steps: firstly, placing a granular molecular sieve in a muffle furnace for fully drying; and then, dissolving the silicone in xylene, then placing the mixture in a spraying container, placing the granular molecular sieve in a turntable, spraying a silicone xylene solution while rotating, fully spraying, standing, and solidifying the silicone on the surfaces of the molecular sieve granules to form a breathable and waterproof film coating after the xylene is completely volatilized.
The mass concentration of the silicone in the silicone xylene solution is 30-70%.
For the powdery molecular sieve, surface hydrophobic modification is carried out by the following specific method: firstly, placing a powdery molecular sieve in a muffle furnace for fully drying; and then placing the cooled powdery molecular sieve into a toluene solution of trimethylchlorosilane, fully stirring in a constant-temperature water bath for silanization, washing with a toluene and acetone solution after treatment, and finally fully heating and drying the washed powdery molecular sieve.
The mass concentration of the toluene solution of the trimethylchlorosilane is 1-10%, the solid-to-liquid ratio of the powdery molecular sieve to the toluene solution of the trimethylchlorosilane is 1g: 20-80 mL, and the heating temperature of the thermostatic water bath is 60-80 ℃.
The CO is2The method of adsorption is CO2Pressure adsorption or CO2And (5) gas purging.
A use method of a cement-based material carbonization internal curing agent is characterized in that the cement-based material carbonization internal curing agent is doped into a cement-based material according to the proportion of 5-60% of the mass of cement.
In the invention, the molecular sieve is used as an adsorption carrier, and after surface hydrophobic modification or surface coating release control treatment, the molecular sieve has hydrophobic property and adsorbs CO2CO which is not absorbed in the cement-based material after being mixed with the cement-based material2And (4) escaping. In addition, Ca generated by cement hydrolysis in the pore solution of the cement-based material2+And OH-and the pH rise during hydrolysis become the trigger of CO inside the molecular sieve2Diffusion conditions realize CO inside the molecular sieve2Controlled release of (2). CO22After being released from the interior of the molecular sieve, the molecular sieve can generate carbonization reaction with mineral phases and hydration products in the cement base as follows:
3CaO·SiO2+yH2O+(3-x)CO2→CaO·SiO2·yH2O+(3-x)CaCO3formula (1)
2CaO·SiO2+yH2O+(2-x)CO2→CaO·SiO2·yH2O+(2-x)CaCO3Formula (2)
Ca(OH)2+CO2→CaCO3+H2O type (3)
Compared with the prior art, the invention has the following advantages and remarkable effects:
1. the invention overcomes the defect of CO in the carbonization and maintenance process2Low diffusion depth and low carbonization reaction degree, directly adding CO2Is introduced into the cement-based material.
2. The invention can improve the carbonization reaction degree without reducing the water cement ratio of the cement-based material.
3. The invention can realize the field application of carbonization curing in cement materials without special high-pressure curing equipment.
4. The invention obviously improves the early mechanical property of the cement-based material.
Drawings
Fig. 1 is a schematic diagram of a technical solution provided by the present invention.
Detailed Description
The present invention will be specifically described below with reference to specific examples, but the scope of the present invention is not limited to the following examples.
The cement-based material carbonization internal curing agent provided by the invention is prepared by the method and the reaction principle is shown in figure 1, firstly, rod-shaped particles, spherical particles or powdery molecular sieves are used as raw materials, and the types of the molecular sieves comprise: more than one of A type, X type, Y type and ZSM type.
The surface coating release control treatment is carried out on the molecular sieves of the rod-shaped particles and the spherical particles, and the specific method comprises the following steps: firstly, placing the granular molecular sieve in a muffle furnace for fully drying, preferably drying for 4 hours at 500 ℃; and then dissolving the silicone in xylene, wherein the mass concentration of the silicone in the silicone xylene solution is 30-70% (preferably 50%). And then placing the granular molecular sieve in a spraying container, spraying a silicone xylene solution while rotating, standing after full spraying, and solidifying the silicone on the surfaces of the molecular sieve granules to form a breathable and waterproof film coating after the xylene is completely volatilized.
For the powdery molecular sieve, surface hydrophobic modification is carried out by the following specific method: firstly, putting a powdery molecular sieve into a muffle furnace for fully drying, preferably drying for 4 hours at 500 ℃; and then placing the cooled powdery molecular sieve into a toluene solution of trimethylchlorosilane, wherein the mass concentration of the toluene solution of the trimethylchlorosilane is 1-10% (preferably 5%), and the solid-to-liquid ratio of the powdery molecular sieve to the toluene solution of the trimethylchlorosilane is 1g: 20-80 mL (preferably 1g: 50mL), fully stirring in a constant-temperature water bath for silanization, and heating the mixture in the constant-temperature water bath at the temperature of 60-80 ℃ (preferably 70 ℃). After the treatment, the powder was washed with toluene and acetone solution, and finally the washed powder was dried by heating sufficiently (drying at 50 ℃ C. for 12 hours).
After the surface hydrophobic modification or surface coating release control treatment, the molecular sieve has hydrophobic property, and then the molecular sieve is subjected to CO2Adsorbing to obtain the cement-based material carbonized internal curing agent, wherein the CO is2The method of adsorption is CO2Pressure adsorption or CO2And (5) gas purging.
When the cement-based material carbonization internal curing agent is used, the cement-based material carbonization internal curing agent is doped into the cement-based material according to the proportion of 5-60% of the mass of cement. After surface hydrophobic modification or surface coating release control treatment, the molecular sieve shows hydrophobic property and adsorbs CO2CO which is not absorbed in the cement-based material after being mixed with the cement-based material2And (4) overflowing. In addition, Ca generated by cement hydrolysis in the pore solution of the cement-based material2+And OH-And the rising of the pH value in the hydrolysis process can be used for inducing CO in the molecular sieve2Diffusion conditions realize CO inside the molecular sieve2Controlled release of (2).
Example 1: in the embodiment, the spherical granular 13X molecular sieve is taken as CO2Carrier material, surface-coated by CO2The carbonized internal curing agent prepared by adsorbing CO2 in a gas purging mode is mixed into pure cement slurry with the water cement ratio of 0.38 according to the mass percent of cement, and the 1-day compressive strength of the pure cement slurry is improved by 22 percent compared with pure cement slurry without the internal curing agent.
Example 2: in this example, powdered 5A molecular sieve is used as CO2Support material, surface hydrophobically modified by CO2CO adsorption by means of pressure adsorption2The carbonized internal curing agent is added into cement paste with the water cement ratio of 0.38 according to 30 percent of the mass of the cement, and the 1-day compressive strength of the cement paste is improved by 10 percent compared with pure cement paste without the internal curing agent.
Example 3: in the embodiment, powdered ZSM-5 molecular sieve is used as CO2Support material, surface hydrophobically modified by CO2CO adsorption by means of pressure adsorption2The carbonized internal curing agent is prepared, is mixed into mortar with the water cement ratio of 0.5 and the mortar ratio of 1: 3 according to 30 percent of the mass of the cement, and the 1-day compressive strength of the mortar is improved by 16 percent compared with the mortar without the internal curing agent.
Claims (4)
1. A method for preparing a cement-based material carbonized internal curing agent by surface hydrophobic modification is characterized by comprising the following steps: the method is characterized in that a powdery molecular sieve is used as a raw material, surface hydrophobic modification is carried out to ensure that the molecular sieve has hydrophobic characteristics, and the specific method for the surface hydrophobic modification is as follows: firstly, placing a powdery molecular sieve in a muffle furnace for fully drying; then placing the cooled powdery molecular sieve in a toluene solution of trimethylchlorosilane, fully stirring in a constant-temperature water bath for silanization treatment, washing with a toluene and acetone solution after the treatment is finished, and finally fully heating and drying the washed powdery molecular sieve;
then subjecting it to CO2And adsorbing to obtain the cement-based material carbonized internal curing agent.
2. The method for preparing the cement-based material carbonized internal curing agent by the hydrophobic modification of the surface according to claim 1, wherein the method comprises the following steps: the molecular sieve comprises the following models: more than one of A type, X type, Y type and ZSM type.
3. The method for preparing the cement-based material carbonized internal curing agent by the hydrophobic modification of the surface according to claim 1, wherein the method comprises the following steps: the mass concentration of the toluene solution of the trimethylchlorosilane is 1-10%, the solid-to-liquid ratio of the powdery molecular sieve to the toluene solution of the trimethylchlorosilane is 1g: 20-80 mL, and the heating temperature of the thermostatic water bath is 60-80 ℃.
4. The method for preparing the cement-based material carbonized internal curing agent by the hydrophobic modification of the surface according to claim 1, wherein the method comprises the following steps: the CO is2The method of adsorption is CO2Pressure adsorption or CO2And (5) gas purging.
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| CN114570328A (en) * | 2022-03-30 | 2022-06-03 | 大连理工大学盘锦产业技术研究院 | Hydrophobic modified molecular sieve and preparation method and application thereof |
| CN115124273A (en) * | 2022-07-12 | 2022-09-30 | 山东汉博昱洲新材料有限公司 | Carbonized internal curing agent and preparation method and application thereof |
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| CN111943547A (en) | 2020-11-17 |
| CN111960708A (en) | 2020-11-20 |
| CN111393060B (en) | 2020-10-09 |
| CN111393060A (en) | 2020-07-10 |
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