CN113105136A - Preparation method of early-strength regenerated micro powder - Google Patents
Preparation method of early-strength regenerated micro powder Download PDFInfo
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- CN113105136A CN113105136A CN202011144718.XA CN202011144718A CN113105136A CN 113105136 A CN113105136 A CN 113105136A CN 202011144718 A CN202011144718 A CN 202011144718A CN 113105136 A CN113105136 A CN 113105136A
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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
- C04B20/026—Comminuting, e.g. by grinding or breaking; Defibrillating fibres other than asbestos
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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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/16—Waste materials; Refuse from building or ceramic industry
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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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- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Civil Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a preparation method of early-strength regenerated micro powder. The preparation method comprises the following steps: grinding the regenerated micro powder, and screening and selecting the regenerated micro powder with the particle size not more than 5 mu m; placing the ground and sieved regenerated micro powder into water, and uniformly dispersing by ultrasonic to form a suspension A; pouring the suspension A into a modifier solution B, placing the suspension in a reaction kettle after ultrasonic dispersion, and completely reacting by a hydrothermal method to form a mixed solution C; carrying out centrifugal separation, water washing, absolute ethyl alcohol washing and drying on the mixed solution C to obtain early-strength regenerated micro powder; the modifier solution B is microemulsion which is formed by silicon tetrachloride after water reaction and contains hydrochloric acid and silicic acid compounds. The preparation method of the invention better excites the activity of the regenerated micro powder, the prepared early strength type regenerated micro powder can effectively improve the early strength of the mortar, increases the reutilization of the solid waste micro powder, expands the high-end application thereof, and has good promotion effect on protecting the ecological environment and promoting the development of circular economy.
Description
Technical Field
The invention relates to the field of building materials, in particular to a preparation method of early-strength regenerated micro powder.
Background
With the continuous increase of the scale of urban reconstruction and expansion and the continuous updating of urban old buildings, a large amount of waste concrete is generated by the dismantling of a large number of old buildings and structures. At present, the waste concrete of the building is mainly treated by adopting the traditional modes of open-air stacking, landfill and the like, not only occupies a large amount of land, but also causes great harm to the environment and personal safety. In recent years, our country has accelerated the recycling of waste concrete, but the recycling is mainly focused on the use of coarse and fine aggregates, and a large amount of recycled micro powder inevitably appears in the process of forming recycled aggregates. At present, the use of the regenerated micro powder is less, and the regeneration and the utilization of the regenerated micro powder are mainly realized by the following ways from the research on the regenerated micro powder and the prior invention data: (1) grinding the mixture into fine powder to be used as an inert admixture or filler; (2) the unhydrated cement particle components are utilized, and active admixtures such as mineral powder and silica fume are added, so that the production of concrete can be realized by replacing part of cement; (3) grinding into a certain fineness, adding admixture, adjusting the calcium-silicon ratio, sintering at a certain temperature, and grinding into active admixture for use. However, it is known from the current research and patent data that the activity of the recycled micro powder is activated by physical means and high temperature mainly by using unhydrated cement particles and calcium silicon components in the recycled aggregate micro powder of the waste concrete. However, since the recycled fine powder has a large water absorption amount, when cement is replaced with the recycled aggregate fine powder, the strength is lowered to some extent, and the formed concrete is cracked. The technical means of high-temperature sintering has high energy consumption, and because the components of the regenerated micro powder are complex, the sintered admixture is used for replacing cement, and certain difference exists in performance. Therefore, from the current research and the prior patent technical means, the practical value of the recycled micro powder as the cementing material is not fully excavated, and the problems existing in the application of the recycled micro powder of the waste concrete are not completely solved.
Disclosure of Invention
In order to overcome the technical defects of the prior art that the recycled micro powder is not fully utilized, make up the defects of large water absorption capacity, low activity and the like of the recycled micro powder, fully excavate the technical characteristics and potential activity of the recycled micro powder, and realize the maximum activity and the highest utilization efficiency of the recycled micro powder, the components and the characteristics of the recycled micro powder are fully considered, the activity of the recycled micro powder can be better excited, the early strength of the mortar can be effectively improved, and the preparation method of the early-strength recycled micro powder is provided.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a preparation method of early-strength regenerated micro powder comprises the following steps:
(1) firstly, grinding the regenerated micro powder, and then screening and selecting the regenerated micro powder with the particle size of not more than 5 mu m;
(2) putting the regenerated micro powder with the particle size not more than 5 microns obtained after grinding in the step (1) into water, and uniformly dispersing by ultrasonic to form suspension A;
(3) pouring the suspension A prepared in the step (2) into a modifier solution B, ultrasonically dispersing for 3-6 min, placing in a reaction kettle, and completely reacting at 120-150 ℃ by a hydrothermal method to form a mixed solution C;
(4) carrying out centrifugal separation, water washing, absolute ethyl alcohol washing and drying on the mixed solution C prepared in the step (3) to obtain early strength type regenerated micro powder;
the suspension A in the step (2) is formed by placing 5-10 parts by mass of regenerated micro powder into 20-30 parts by mass of water and performing ultrasonic dispersion; the ultrasonic dispersion time is generally 3-5 min.
The modifier solution B in the step (3) is microemulsion generated by silicon tetrachloride water reaction, and mainly is microemulsion which is formed by silicon tetrachloride water reaction and contains hydrochloric acid and silicic acid compounds;
the modifier solution B is formed by mixing and uniformly stirring liquid paraffin, a nonionic surfactant, cetyl trimethyl ammonium bromide, silicon tetrachloride and water and then reacting, and the modifier solution B comprises the following components in parts by weight:
the regenerated micro powder in the step (1) is calcium silicate regenerated micro powder.
The nonionic surfactant is preferably sorbitan monooleate.
The reaction time of the mixed solution of A and B in a hydrothermal method is 8-10 h.
After the regenerated micro powder is ground, the surface area of the regenerated micro powder is increased, the inertia of the hydrated calcium silicate is changed, the activation of the activity of the hydrated calcium silicate is promoted, and suspension is formed after ultrasonic dispersion, so that mutual dispersion among particles can be kept in water, and the particles are not agglomerated. Meanwhile, water, liquid paraffin, a nonionic surfactant and an auxiliary agent cetyl trimethyl ammonium bromide are utilized, and silicon tetrachloride is added to form the microemulsion in which the silicon tetrachloride water reactant is solubilized. The dispersed regenerated micro powder suspension is mixed with the silicon tetrachloride water reactant microemulsion, the silicon tetrachloride water reactant in the microemulsion can react with the regenerated micro powder through hydrothermal reaction under a certain condition and re-nucleate and grow, specifically, the regenerated micro powder reacts with hydrochloric acid in the silicon tetrachloride water reactant and further reacts with silicic acid compounds, and under the condition of the microemulsion, the micro-nano particles of a formed substance can be guaranteed by the water nucleus size, and higher activity is kept. The micro-nano particles are adsorbed on the surfaces of the regenerated micro-powder particles, so that the activity of the regenerated micro-powder is greatly increased, and the water absorption of the regenerated micro-powder is reduced, and the regenerated micro-powder becomes active powder with multiple early strength effects.
The early-strength regenerated micro powder provided by the invention increases the reutilization of solid waste micro powder, expands the high-end application of the solid waste micro powder, and has good promotion effects on protecting ecological environment and promoting the development of circular economy.
Detailed Description
The invention is further described below for a better understanding of the invention, but it should not be understood that the invention is applicable to the following examples, and that the invention is subject to some insubstantial changes and modifications within the scope of the invention as determined by those skilled in the art based on the teachings of the invention.
Example 1
The invention provides a preparation method of early-strength regenerated micro powder, which comprises the following steps:
(1) placing 5 parts by mass of calcium silicate regenerated micro powder with the particle size of not more than 5 mu m into 20 parts by mass of water, and performing ultrasonic dispersion to form a suspension A;
(2) mixing 30 parts by mass of liquid paraffin, 3.5 parts by mass of sorbitan monooleate, 1 part by mass of hexadecyl trimethyl ammonium bromide, 1 part by mass of silicon tetrachloride and 10 parts by mass of water, and uniformly stirring to form a solution B;
(3) pouring the A into the B, placing the A into a reaction kettle after ultrasonic dispersion for 5min, and carrying out hydrothermal reaction at 150 ℃ for 8h to form C;
(4) and (4) carrying out centrifugal separation, water washing, absolute ethyl alcohol washing and drying on the C to obtain the early strength type regenerated micro powder.
The calcium silicate regenerated micro powder obtained in the step (1) is obtained by grinding the regenerated micro powder and then screening and selecting the regenerated micro powder with the particle size not more than 5 mu m.
Example 2
The invention provides a preparation method of early-strength regenerated micro powder, which comprises the following steps:
(1) 10 parts by mass of calcium silicate regenerated micro powder with the particle size of not more than 5 mu m is put into 20 parts by mass of water and is subjected to ultrasonic dispersion to form a suspension A;
(2) mixing 30 parts by mass of liquid paraffin, 2 parts by mass of fatty alcohol-polyoxyethylene ether, 1.5 parts by mass of hexadecyl trimethyl ammonium bromide, 1.5 parts by mass of silicon tetrachloride and 12 parts by mass of water, and uniformly stirring to form a solution B;
(3) pouring the A into the B, placing the A into a reaction kettle after ultrasonic dispersion for 6min, and carrying out a hydrothermal method reaction at 120 ℃ for 10h to form C;
(4) and (4) carrying out centrifugal separation, water washing, absolute ethyl alcohol washing and drying on the C to obtain the early strength type regenerated micro powder.
The calcium silicate regenerated micro powder obtained in the step (1) is obtained by grinding the regenerated micro powder and then screening and selecting the regenerated micro powder with the particle size not more than 5 mu m.
Example 3
The invention provides a preparation method of early-strength regenerated micro powder, which comprises the following steps:
(1) placing 5 parts by mass of calcium silicate regenerated micro powder with the particle size not more than 5 mu m in 30 parts by mass of water, and performing ultrasonic dispersion to form a suspension A;
(2) mixing 30 parts by mass of liquid paraffin, 5 parts by mass of alkylphenol ethoxylates, 0.5 part by mass of hexadecyl trimethyl ammonium bromide, 0.5 part by mass of silicon tetrachloride and 8 parts by mass of water, and uniformly stirring to form a solution B;
(3) pouring the A into the B, placing the A into a reaction kettle after ultrasonic dispersion for 3min, and carrying out hydrothermal reaction at 125 ℃ for 9h to form C;
(4) and (4) carrying out centrifugal separation, water washing, absolute ethyl alcohol washing and drying on the C to obtain the early strength type regenerated micro powder.
The calcium silicate regenerated micro powder obtained in the step (1) is obtained by grinding the regenerated micro powder and then screening and selecting the regenerated micro powder with the particle size not more than 5 mu m.
Example 4
The invention provides a preparation method of early-strength regenerated micro powder, which comprises the following steps:
(1) placing 5 parts by mass of calcium silicate regenerated micro powder with the particle size not more than 5 mu m into 25 parts by mass of water, and performing ultrasonic dispersion to form a suspension A;
(2) mixing 30 parts by mass of liquid paraffin, 3.5 parts by mass of sorbitan monooleate, 0.5 part by mass of hexadecyl trimethyl ammonium bromide, 1.5 parts by mass of silicon tetrachloride and 8 parts by mass of water, and uniformly stirring to form a solution B;
(3) pouring the A into the B, placing the A into a reaction kettle after ultrasonic dispersion for 4min, and carrying out hydrothermal reaction for 10h at 140 ℃ to form C;
(4) and (4) carrying out centrifugal separation, water washing, absolute ethyl alcohol washing and drying on the C to obtain the early strength type regenerated micro powder.
The calcium silicate regenerated micro powder obtained in the step (1) is obtained by grinding the regenerated micro powder and then screening and selecting the regenerated micro powder with the particle size not more than 5 mu m.
Application examples
The reclaimed fine powder and the unmodified reclaimed fine powder obtained in each example were mixed in the proportions shown in Table 1 to prepare mortar.
TABLE 1 base mortar to test mortar component ratios
| Test of | Cement (g) | Early strength type regenerated micro powder (g) | Sand | Water (W) |
| Basic mortar | 450 | —— | 1350 | 180 |
| Contrast mortar | 425 | 25 (unmodified recycled micropowder) | 1350 | 180 |
| Example 1 | 425 | 25 | 1350 | 180 |
| Example 2 | 425 | 25 | 1350 | 180 |
| Example 3 | 425 | 25 | 1350 | 180 |
| Example 4 | 425 | 25 | 1350 | 180 |
The results of testing the strength of the mortar prepared in each example, the base example and the comparative example are shown in table 2.
TABLE 2 mortar Strength test results
As can be seen from Table 2, the early strength of the mortar doped with the early strength type modified recycled micro powder is greatly improved, the 12h compressive strength, the 1d compressive strength and the 3d compressive strength are far higher than those of the comparative mortar, namely the mortar doped with the unmodified recycled micro powder, and simultaneously the early strength of the mortar is higher than that of the basic mortar, and the 28d compressive strength is also higher than that of the comparative mortar and is not lower than that of the basic mortar. The activity of the regenerated micro powder modified by the method is greatly improved, the regenerated micro powder can replace cement, the final strength of the mortar is not reduced, and the early strength of the mortar can be obviously improved.
Claims (6)
1. The preparation method of the early-strength regenerated micro powder is characterized by comprising the following steps:
(1) firstly, grinding the regenerated micro powder, and then screening and selecting the regenerated micro powder with the particle size of not more than 5 mu m;
(2) putting the regenerated micro powder with the particle size not more than 5 microns obtained after grinding in the step (1) into water, and uniformly dispersing by ultrasonic to form suspension A;
(3) pouring the suspension A prepared in the step (2) into a modifier solution B, ultrasonically dispersing for 3-6 min, placing in a reaction kettle, and completely reacting at 120-150 ℃ by a hydrothermal method to form a mixed solution C;
(4) carrying out centrifugal separation, water washing, absolute ethyl alcohol washing and drying on the mixed solution C prepared in the step (3) to obtain early strength type regenerated micro powder;
the suspension A in the step (2) is formed by placing 5-10 parts by mass of regenerated micro powder into 20-30 parts by mass of water and performing ultrasonic dispersion;
the modifier solution B in the step (3) is a microemulsion containing hydrochloric acid and silicic acid compounds formed after silicon tetrachloride is subjected to water reaction;
2. the method for preparing the early strength recycled micropowder according to claim 1, wherein the ultrasonic dispersion time of the suspension A prepared in the step (2) is 3-5 min.
3. The method for preparing the early strength recycled micropowder according to claim 1, wherein the recycled micropowder obtained in the step (1) is a calcium silicate recycled micropowder.
4. The preparation method of the early strength recycled micropowder according to claim 1, wherein the modifier solution B in the step (2) is formed by mixing and uniformly stirring liquid paraffin, a nonionic surfactant, cetyl trimethyl ammonium bromide, silicon tetrachloride and water, and reacting, and the mass parts of the components are as follows:
5. the method of claim 1, wherein the non-ionic surfactant is sorbitan monooleate.
6. The method for preparing the early strength recycled micropowder according to claim 1, wherein the hydrothermal reaction time in the step (3) is 8h to 10 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113788638A (en) * | 2021-10-11 | 2021-12-14 | 台州学院 | High-activity regenerated micro powder and preparation method thereof |
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