CN111393106B - High-mechanical-property iron boride modified cement mortar and preparation method thereof - Google Patents
High-mechanical-property iron boride modified cement mortar and preparation method thereof Download PDFInfo
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- CN111393106B CN111393106B CN202010220129.9A CN202010220129A CN111393106B CN 111393106 B CN111393106 B CN 111393106B CN 202010220129 A CN202010220129 A CN 202010220129A CN 111393106 B CN111393106 B CN 111393106B
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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
- 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
- C04B28/02—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 containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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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
- 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
Abstract
The invention discloses high-mechanical-property iron boride modified cement mortar and a preparation method thereof, wherein the iron boride modified cement mortar comprises the following components in parts by weight: 310-350 parts of Portland cement, 1380-1420 parts of graded sand, 230-270 parts of water and 0.16-0.33 part of an iron boride raw material; the preparation method of the iron boride modified cement mortar comprises the following steps: firstly, preparing iron boride aqueous solution, then uniformly dispersing the iron boride aqueous solution serving as a composite modifier in cement mortar, and preparing the iron boride modified cement mortar through stirring, vibrating, forming and curing processes. The iron boride modified cement mortar prepared by the invention not only greatly improves the mechanical property, but also extracts the raw materials from the construction waste, thereby protecting the environment and saving the resources.
Description
Technical Field
The invention relates to novel cement mortar, in particular to iron boride modified cement mortar with high mechanical property and a preparation method thereof.
Background
In recent years, with the increasing of urbanization process, large-scale old cities are removed and rebuilt, and a large amount of construction waste appears. Therefore, how to treat the construction waste and how to recycle the construction waste become great challenges to various big cities. The construction waste is not waste, and is a renewable resource, and the main components of the construction waste are as follows: dregs, waste steel bars, waste iron wires, scattered mortar, broken bricks, broken concrete blocks and the like. The materials account for about 80% of the total amount of the construction waste, and most of the materials can be reused as renewable resources after being sorted, removed or crushed, so that researches on how to treat the construction waste and how to recycle the construction waste at home and abroad are very much, and particularly the recycled aggregate concrete, the recycled mortar and the like are applied in the field of construction engineering.
With the rapid development of modern engineering techniques, ultrahigh-performance building materials are also rapidly developed, and in particular, cement mortar is used as an important engineering material in the civil engineering field. In modern society, people have higher and higher requirements on buildings, and meanwhile, the requirements on the performance of cement mortar are also increased. Because the traditional cement mortar has the defects of low tensile strength, large brittleness, single function and the like, and the modern production and living requirements are difficult to meet, the modern cement mortar needs to be changed to the direction of high performance and multiple functions. The modified cement mortar is a composite material which is formed by combining Portland cement and sand as matrix materials, various nanoscale fillers as modifiers, chemical additives and water through a specific process flow. The invention can not only conform to the trend of modern engineering, but also solve the problems of construction waste and overcome the defects and limitations of the traditional cement mortar.
Disclosure of Invention
The invention aims to provide iron boride modified cement mortar with high mechanical property and a preparation method thereof, so as to overcome the defects and limitations of the traditional cement mortar, effectively solve the dilemma of domestic construction waste treatment, save resources and protect the environment.
In order to solve the technical problems, the invention provides the following technical scheme:
the iron boride modified cement mortar with high mechanical property is characterized by comprising the following components in parts by weight: 0.16-0.33 parts of iron boride, 310-350 parts of Portland cement, 1380-1420 parts of graded sand and 230-270 parts of water.
Preferably, the weight parts of the components are as follows: 0.25 part of ferric boride, 330 parts of Portland cement, 1400 parts of graded sand and 250 parts of water.
Preferably, the purity of the iron boride is more than 99%, and the particle size is 150-250 nm.
Preferably, the portland cement is P.O-type portland cement with the strength of 42.5; the fineness modulus of the graded sand is 2.6-2.9, and the mud content is less than 5%.
The invention also provides a preparation method of the iron boride modified cement mortar with high mechanical property, which mainly comprises the following steps:
(1) preparing molten iron boride solution:
s1, adding the waste iron powder into dilute nitric acid or 37% concentrated hydrochloric acid to be soaked for 4-8 hours;
s2, taking the supernatant obtained in the step S1, and adding a potassium hydroxide solution until the mixed solution is neutral;
s3, taking the neutral solution obtained in the step S2, and adding a sodium borohydride solution until the solution does not precipitate any more;
s4, performing centrifugal separation on the mixture obtained in the step S3, washing the centrifugal precipitate with distilled water for multiple times, and then washing with absolute ethyl alcohol for multiple times;
s5, drying the precipitate obtained in the step S4 in an oven to obtain long-chain iron boride powder;
s6, firstly, adding the nano iron boride powder into 5% water for mixing, magnetically stirring until no suspended iron boride powder exists on the water surface, and then placing the preliminarily stirred dispersion solution into an ultrasonic instrument for ultrasonic dispersion to prepare an iron boride aqueous solution;
(2) pre-mixing the Portland cement, the graded sand and 40% of water by using a cement mortar mixer;
(3) adding the molten iron boride solution prepared in the step (1) and the residual 55% of water, and uniformly stirring to obtain iron boride modified cement mortar slurry;
(4) filling the slurry prepared in the step (3) into an oiling test mold, vibrating and discharging bubbles on a mortar vibrating table, and wiping off the redundant slurry on the surface of the test mold;
(5) and removing the mold after the iron boride modified cement mortar is formed for one day, and performing standard maintenance for 28 days.
Preferably, the concentration of the dilute nitric acid in the step S1 is 3 mol/L; the concentration of the potassium hydroxide solution in the step S2 is 3-6 mol/L; the concentration of the sodium borohydride solution in the step S3 is 2 mol/L.
Preferably, the centrifugal speed is set to 3000r/min in step S4; in the step S5, setting the temperature of the oven to be 70 ℃, and the drying time to be 12 h; the ultrasonic dispersion time in step S6 was 30 min.
Preferably, the stirring speed in the step (2) is set to be 42r/min, and the stirring time is 60-80 s; in the step (3), the stirring speed is set to be 42r/min, and the stirring time is 100-120 s; and (4) the vibration time in the step (4) is 40-60 s.
Preferably, the step (5) specifically comprises the following steps:
(1) pouring the iron boride modified cement mortar into a mold, compacting, placing the mold in a constant temperature room with the temperature of 20 ℃ and the humidity of 20%, curing for 24 hours, and then removing the mold;
(2) after the mold is removed, the test piece is placed in a standard curing room with the temperature of 20 +/-2 ℃ and the humidity of more than or equal to 95 percent, and cured for 28 days.
The invention has the following effects:
the invention adopts a physical method to disperse iron boride in water, and then adds the uniformly distributed and well combined iron boride aqueous solution as a composite modifier into a cement matrix to obtain the uniformly dispersed iron boride composite material.
The test shows that the compressive strength and the flexural strength of the iron boride modified cement mortar are greatly improved, and compared with the common cement mortar, the compressive strength and the flexural strength of the iron boride modified cement mortar are respectively improved by 50.2 percent and 40.8 percent, so that the iron boride modified cement mortar is beneficial to improving the limitation of the traditional cement mortar.
The cement mortar well disperses the iron boride into the composite modified cement-based material, not only greatly improves the mechanical property, but also can solve the problem of recycling construction waste, saves resources and protects the environment.
Drawings
FIG. 1 is a photograph of a scanned ferroelectric boride mirror used in the present invention;
FIG. 2 is a three-dimensional graph of cement mortar performance as iron boride loading increases;
FIG. 3 is a bar graph of slump comparison of comparative and example cement mortar mixes of the present invention;
FIG. 4 is a graph showing the change in compressive strength of cement mortar test pieces after standard curing for 28 days in comparative example and example of the present invention;
FIG. 5 is a graph showing the change in flexural strength of cement mortar test pieces after standard curing for comparative example and example 28 days in accordance with the present invention; and
FIG. 6 is a schematic view of a cement mortar test piece of example 1 of the present invention.
Detailed Description
Hereinafter, embodiments of the present invention will be described with reference to the drawings.
The iron boride modified cement mortar with high mechanical property comprises the following components in parts by weight: 0.16-0.33 parts of iron boride, 310-350 parts of Portland cement, 1380-1420 parts of graded sand and 230-270 parts of water.
Preferably, the weight parts of the components are as follows: 0.25 part of ferric boride, 330 parts of Portland cement, 1400 parts of graded sand and 250 parts of water.
Wherein the purity of the iron boride is more than 99 percent, and the particle size is 150-250 nm; the Portland cement is P.O type Portland cement with the strength of 42.5; the fineness modulus of the graded sand is 2.6-2.9, and the mud content is less than 5%.
A preparation method of iron boride modified cement mortar with high mechanical property mainly comprises the following steps:
(1) preparing molten iron boride solution:
s1, weighing 1-3 g of waste iron powder, adding the waste iron powder into 60-100 mL of dilute nitric acid with the concentration of 3mol/L or 37% concentrated hydrochloric acid, and soaking for 4-8 hours;
s2, taking the supernatant obtained in the step S1, and adding a potassium hydroxide solution with the concentration of 3-6mol/L until the mixed solution is neutral;
s3, adding a sodium borohydride solution with the concentration of 2mol/L into the neutral solution in the step S2 until the solution does not generate precipitate any more;
s4, performing centrifugal separation on the mixture obtained in the step S3 at the rotating speed of 3000r/min, and repeatedly washing the centrifugal precipitate with distilled water and absolute ethyl alcohol for multiple times respectively;
s5, drying the precipitate obtained in the step S4 in an oven at 70 ℃ for 12 hours to obtain long-chain nano iron boride powder;
s6, firstly, adding the required amount of nano iron boride powder into 5% water for mixing, magnetically stirring until no suspended iron boride powder exists on the surface of the water surface, and then placing the preliminarily stirred dispersion solution into an ultrasonic instrument for 30min for ultrasonic dispersion to prepare the iron boride aqueous solution.
(2) Pre-mixing the Portland cement, the graded sand and 40% of water in the required proportion for 60-80 s by using a cement mortar mixer at a rotating speed of 42 r/min;
(3) adding the iron boride aqueous solution prepared in the step (1) and the residual 55% of water, stirring for 100-120 s at a rotating speed of 42r/min, and ensuring that all components are uniformly distributed to obtain iron boride modified cement mortar slurry;
(4) filling the slurry prepared in the step (3) into an oil coating test mold, compacting and discharging bubbles by using a mortar compacting table, and wiping off the redundant slurry on the surface of the test mold after vibrating for 40-60 s to ensure that the upper surface of the test piece is flat;
(5) removing the mold after the test piece is molded for one day and naturally curing for 28 days: pouring the iron boride modified cement mortar into a mold, compacting, placing the mold in a constant temperature room with the temperature of 20 ℃ and the humidity of 20%, curing for 24 hours, and then removing the mold; after the mold is removed, the test piece is placed in a standard curing room with the temperature of 20 +/-2 ℃ and the humidity of more than or equal to 95 percent, and cured for 28 days.
In order to better embody the effect of the iron boride modifier on cement mortar, experiments were conducted by adjusting the weight parts of iron boride using a fixed weight part of portland cement, graded sand, and water in the present example and comparative example.
Example 1:
weighing 1g of waste iron powder, adding the waste iron powder into 60mL of dilute nitric acid with the concentration of 3mol/L, soaking for 8 hours, taking the obtained supernatant, adding a potassium hydroxide solution with the concentration of 6mol/L until the mixed solution is neutral, then adding a sodium borohydride solution with the concentration of 2mol/L into the solution until the solution does not produce any precipitate any more, carrying out centrifugal separation on the obtained mixture at the rotating speed of 3000r/min, then respectively washing the centrifugal precipitate with distilled water and absolute ethyl alcohol repeatedly for multiple times, and drying the obtained precipitate in an oven at 70 ℃ for 12 hours to obtain long-chain nano iron boride powder for later use.
Firstly, slowly adding 0.16 part of nano iron boride into 12.5 parts of water for mixing, magnetically stirring until no suspended nano iron boride powder exists on the surface of the water surface, and then placing the preliminarily stirred dispersion solution into an ultrasonic instrument for ultrasonic dispersion for 30min to prepare an iron boride aqueous solution for later use; then sequentially putting 330 parts of Portland cement, 1400 parts of graded sand and 100 parts of water into a stirrer, and uniformly stirring for 70s at the rotating speed of 42 r/min; then adding the prepared iron boride aqueous solution and 137.5 parts of water, uniformly stirring for 110s at a constant rotating speed, and discharging to obtain iron boride modified cement mortar slurry; pouring the slurry into an oiling test mold, placing the oiling test mold on a mortar vibrating table for vibrating for 50s, removing the mold after the cement mortar is formed, and then carrying out standard maintenance for 28 days. The concrete sample of the resulting cement mortar was as shown in FIG. 6, and other examples and comparative examples were similar thereto.
Example 2:
weighing 3g of waste iron powder, adding the waste iron powder into 100mL of dilute nitric acid with the concentration of 3mol/L, soaking for 4 hours, taking the obtained supernatant, adding a potassium hydroxide solution with the concentration of 3mol/L until the mixed solution is neutral, then adding a sodium borohydride solution with the concentration of 2mol/L into the solution until the solution does not produce any precipitate any more, carrying out centrifugal separation on the obtained mixture at the rotating speed of 3000r/min, then respectively washing the centrifugal precipitate with distilled water and absolute ethyl alcohol repeatedly for multiple times, and drying the obtained precipitate in an oven at 70 ℃ for 12 hours to obtain long-chain nano iron boride powder for later use.
Firstly, slowly adding 0.25 part of nano iron boride into 12.5 parts of water for mixing, magnetically stirring until no suspended nano iron boride powder exists on the surface of the water surface, and then placing the preliminarily stirred dispersion solution into an ultrasonic instrument for ultrasonic dispersion for 30min to prepare an iron boride aqueous solution for later use; then sequentially putting 330 parts of Portland cement, 1400 parts of graded sand and 100 parts of water into a stirrer, and uniformly stirring for 70s at the rotating speed of 42 r/min; then adding the prepared iron boride aqueous solution and 137.5 parts of water, uniformly stirring for 110s at a constant rotating speed, and discharging to obtain iron boride modified cement mortar slurry; pouring the slurry into an oiling test mold, placing the oiling test mold on a mortar vibrating table for vibrating for 50s, removing the mold after the cement mortar is formed, and then carrying out standard maintenance for 28 days.
Example 3:
weighing 2g of waste iron powder, adding the waste iron powder into 80mL of dilute nitric acid with the concentration of 3mol/L, soaking for 6 hours, taking the obtained supernatant, adding a potassium hydroxide solution with the concentration of 5mol/L until the mixed solution is neutral, then adding a sodium borohydride solution with the concentration of 2mol/L into the solution until the solution does not produce any precipitate any more, carrying out centrifugal separation on the obtained mixture at the rotating speed of 3000r/min, then respectively washing the centrifugal precipitate with distilled water and absolute ethyl alcohol repeatedly for multiple times, and drying the obtained precipitate in an oven at 70 ℃ for 12 hours to obtain long-chain nano iron boride powder for later use.
Firstly, slowly adding 0.33 part of nano iron boride into 12.5 parts of water for mixing, magnetically stirring until no suspended nano iron boride powder exists on the surface of the water surface, and then placing the preliminarily stirred dispersion solution into an ultrasonic instrument for ultrasonic dispersion for 30min to prepare an iron boride aqueous solution for later use; then sequentially putting 330 parts of Portland cement, 1400 parts of graded sand and 100 parts of water into a stirrer, and uniformly stirring for 70s at the rotating speed of 42 r/min; then adding the prepared iron boride aqueous solution and 137.5 parts of water, uniformly stirring for 110s at a constant rotating speed, and discharging to obtain iron boride modified cement mortar slurry; pouring the slurry into an oiling test mold, placing the oiling test mold on a mortar vibrating table for vibrating for 50s, removing the mold after the cement mortar is formed, and then carrying out standard maintenance for 28 days.
Comparative example 1:
sequentially putting 330 parts of Portland cement, 1400 parts of graded sand and 100 parts of water into a stirrer, and uniformly stirring for 70s at the rotating speed of 42 r/min; then adding 150 parts of water, uniformly stirring for 110s at a constant rotating speed, and discharging to obtain common cement mortar; pouring common cement mortar into a mold, placing the mold on a mortar jolt ramming table, vibrating for 50s, removing the mold after the cement mortar is molded, and then performing standard maintenance for 28 days.
Through tests, the slump of the iron boride modified cement mortar mixture prepared by the invention and the 28d basic mechanical property of cement mortar are shown in table 1, and the change curve of the performance of the iron boride modified cement mortar along with the addition of iron boride is shown in fig. 2-5.
| Slump (mm) | Compressive strength (Mpa) | Breaking strength (Mpa) | |
| Comparative example 1 | 74 | 15.3 | 3.98 |
| Example 1 | 58 | 20.2 | 4.85 |
| Example 2 | 50 | 22.98 | 5.60 |
| Example 3 | 44 | 18.5 | 4.43 |
TABLE 1
As can be seen from Table 1, the mechanical properties of the iron boride modified cement mortar prepared by the invention are obviously superior to those of common cement mortar, the average compressive strength of the iron boride modified cement mortar is enhanced by 50.2 percent compared with that of the common cement mortar, and the average flexural strength of the iron boride modified cement mortar is enhanced by 40.8 percent. As can be seen from FIGS. 2 to 5, the amount of 0.25 part of iron boride is the optimal choice for the case of 330 parts of portland cement, 1400 parts of graded sand, and 250 parts of water in this example, and in the actual production process, the properties of the cement mortar can be improved within the control range by properly adjusting the weight parts of portland cement, graded sand, water, and iron boride.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention shall fall within the protection scope defined by the claims of the present invention.
Claims (9)
1. The preparation method of the high-mechanical-property iron boride modified cement mortar is characterized in that the cement mortar is composed of the following components in parts by weight: 0.16 to 0.33 parts of iron boride, 310 to 350 parts of Portland cement, 1380 to 1420 parts of graded sand and 230 to 270 parts of water,
the method mainly comprises the following steps:
(1) preparing molten iron boride solution:
s1, adding the waste iron powder into dilute nitric acid or 37% concentrated hydrochloric acid to be soaked for 4-8 hours;
s2, taking the supernatant obtained in the step S1, and adding a potassium hydroxide solution until the mixed solution is neutral;
s3, taking the neutral solution obtained in the step S2, and adding a sodium borohydride solution until the solution does not precipitate any more;
s4, performing centrifugal separation on the mixture obtained in the step S3, washing the centrifugal precipitate with distilled water for multiple times, and then washing with absolute ethyl alcohol for multiple times;
s5, drying the precipitate obtained in the step S4 in an oven to obtain long-chain iron boride powder;
s6, firstly, adding the nano iron boride powder into 5% water for mixing, magnetically stirring until no suspended iron boride powder exists on the water surface, and then placing the preliminarily stirred dispersion solution into an ultrasonic instrument for ultrasonic dispersion to prepare an iron boride aqueous solution;
(2) pre-mixing the Portland cement, the graded sand and 40% of water by using a cement mortar mixer;
(3) adding the molten iron boride solution prepared in the step (1) and the residual 55% of water, and uniformly stirring to obtain iron boride modified cement mortar slurry;
(4) filling the slurry prepared in the step (3) into an oiling test mold, vibrating and discharging bubbles on a mortar vibrating table, and wiping off the redundant slurry on the surface of the test mold;
(5) and removing the mold after the iron boride modified cement mortar is formed for one day, and performing standard maintenance for 28 days.
2. The method for preparing high mechanical properties iron boride modified cement mortar as claimed in claim 1, wherein the concentration of the dilute nitric acid in step S1 is 3 mol/L; the concentration of the potassium hydroxide solution in the step S2 is 3-6 mol/L; the concentration of the sodium borohydride solution in the step S3 is 2 mol/L.
3. The method for preparing high mechanical properties iron boride modified cement mortar as claimed in claim 1, wherein the centrifugal rotational speed is set to 3000r/min in step S4; in the step S5, setting the temperature of the oven to be 70 ℃, and the drying time to be 12 h; the ultrasonic dispersion time in step S6 was 30 min.
4. The preparation method of the high-mechanical-property iron boride modified cement mortar as claimed in claim 1, wherein the stirring speed in the step (2) is set to 42r/min, and the stirring time is 60-80 s; in the step (3), the stirring speed is set to be 42r/min, and the stirring time is 100-120 s; and (4) the vibration time in the step (4) is 40-60 s.
5. The method for preparing high mechanical properties iron boride modified cement mortar as claimed in claim 1, wherein the step (5) specifically comprises the steps of:
(1) pouring the iron boride modified cement mortar into a mold, compacting, placing the mold in a constant temperature room with the temperature of 20 ℃ and the humidity of 20%, curing for 24 hours, and then removing the mold;
(2) after the mold is removed, the test piece is placed in a standard curing room with the temperature of 20 +/-2 ℃ and the humidity of more than or equal to 95 percent, and cured for 28 days.
6. A cement mortar prepared by the method for preparing the high mechanical property iron boride modified cement mortar of claim 1.
7. The cement mortar of claim 6, wherein the weight parts of the components are as follows: 0.25 part of ferric boride, 330 parts of Portland cement, 1400 parts of graded sand and 250 parts of water.
8. The cement mortar of claim 7, wherein the iron boride has a purity of more than 99% and a particle size of 150 to 250 nm.
9. The cement mortar of claim 6, wherein the portland cement is type P.O portland cement with a strength of 42.5; the fineness modulus of the graded sand is 2.6-2.9, and the mud content is less than 5%.
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