CN113913968A - Preparation method of calcium carbonate fiber for improving performance of cement-based composite material - Google Patents
Preparation method of calcium carbonate fiber for improving performance of cement-based composite material Download PDFInfo
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- CN113913968A CN113913968A CN202111203287.4A CN202111203287A CN113913968A CN 113913968 A CN113913968 A CN 113913968A CN 202111203287 A CN202111203287 A CN 202111203287A CN 113913968 A CN113913968 A CN 113913968A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/38—Fibrous materials; Whiskers
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of calcium carbonate fiber for improving the performance of a cement-based composite material, which comprises the following steps: s1: according to the weight ratio of 1: 2, cleaning, filtering and drying the calcium carbonate powder; s2: according to the weight ratio of calcium carbonate to acetic acid of 5: 10, stirring at the speed of 100-120r/min for 20min, uniformly mixing to obtain a mixture, and standing for 2h to obtain a mixture solution A ((CH)3‑COO)2Ca solution); s3: 40 parts by mass of citric acid and the mixture solution A ((CH) was added in a weight ratio of acetic acid to citric acid of 1:13‑COO)2Ca solution) and stirring for 30min at the speed of 100-120r/min to be uniformly mixed, so that the pH value tends to be stable to obtain a mixture B; s4: the mixture B is mechanically stirred for 10min at the temperature of 70 ℃ in a constant-temperature water bath at the speed of 100-120r/min, and then sodium dodecyl benzene sulfonate with the weight ratio of 0.5-1 percent is addedContinuously stirring for 30min to obtain milk white liquid C, and drying in a constant-temperature drying oven at 100 ℃ to obtain dry gel D; s5: and calcining the dried gel D in a muffle furnace at 600 ℃ for 2h to obtain the calcium carbonate fiber.
Description
Technical Field
The invention relates to a preparation method of calcium carbonate fibers for a cement-based composite material, and particularly belongs to the technical field of calcium carbonate preparation.
Background
Common fibers such as asbestos fibers, cellulose fibers, steel fibers, various organic fibers, glass fibers, carbon fibers and the like which are currently used for reinforcing cement-based composite materials restrict the development of fiber cement-based composite materials due to factors such as manufacturability, durability, environmental protection, price and the like.
Calcium carbonate fiber is a whisker-like single crystal which is grown in a fibrous form by artificial control using inexpensive calcium carbonate as a raw material, and has a shape similar to that of short fibers and a size much smaller than that of the short fibers. The strength and modulus of the material are close to the theoretical values of bond strength of a complete crystal material, the material has high strength, high modulus, excellent heat resistance and heat insulation performance, has double composite effects of fiber and mineral fine powder, shows excellent physical and chemical properties and mechanical properties, and becomes an ideal reinforcing material of a cement-based composite material.
The current preparation method of calcium carbonate fiber mainly comprises the following steps: reaction of soluble calcium salt with soluble carbonate, hydrolysis of urea, thermal decomposition of calcium bicarbonate, Ca (OH)2-CO2Gas-liquid reaction synthesis method, hypergravity reaction method, etc. Each of these methods has its advantages, but also has some disadvantages. The reaction method of soluble calcium salt and soluble carbonate usually needs to add various crystal form control agents into a reaction system, and the purity and uniformity of calcium carbonate crystal whiskers are influenced due to the nonuniformity of solution concentration and temperature; the urea hydrolysis method needs to be carried out under the constant high-temperature (110 ℃) and high-pressure condition, and has large energy consumption and high danger; the calcium bicarbonate heating decomposition method needs to be filled with CO2Gas, and the length-diameter ratio of the obtained calcium carbonate crystal whisker is not ideal; ca (OH)2-CO2Most of the gas-liquid reaction synthesis methods need to add seed crystals to induce nucleation, or need to add a crystal form control agent to control the ordered growth of crystals, and the process is complex; the hypergravity field synthesis method is carried out in a specific hypergravity reaction device, and the length-diameter ratio is not ideal. The sol-gel method is a wet chemical preparation method capable of preparing materials from zero dimension to three dimensions, and has many advantages, such as simple process, low equipment price, easy control of reaction process, and uniform product components.
Disclosure of Invention
The technical problem to be solved by the invention is that the development of fiber cement-based composite materials is restricted by common fibers currently used for reinforcing cement-based composite materials due to factors such as manufacturability, durability, environmental protection, price and the like, and the invention aims to provide a preparation method of calcium carbonate fibers for improving the performance of cement-based composite materials and solve the problems.
The invention is realized by the following technical scheme:
a method for preparing calcium carbonate fibers for improving the performance of a cement-based composite material, the method comprising the steps of:
s1: according to the weight ratio of 1: 2, cleaning, filtering and drying the calcium carbonate powder;
s2: according to the weight ratio of calcium carbonate to acetic acid of 5: 10, stirring at the speed of 100-120r/min for 20min, uniformly mixing to obtain a mixture, and standing for 2h to obtain a mixture solution A ((CH)3-COO)2Ca solution);
s3: 40 parts by mass of citric acid and the mixture solution A ((CH) was added in a weight ratio of acetic acid to citric acid of 1:13-COO)2Ca solution) and stirring for 30min at the speed of 100-120r/min to be uniformly mixed so as to lead the pH value to tend to be stable to obtain a mixture B;
s4: mechanically stirring the mixture B in a constant-temperature water bath at 70 ℃ for 10min at 120r/min, adding 0.5-1 wt% of sodium dodecyl benzene sulfonate, continuously stirring for 30min to obtain a milky white liquid C, and drying in a constant-temperature drying oven at 100 ℃ to obtain a dry gel D;
s5: and calcining the dried gel D in a muffle furnace at 600 ℃ for 2h to obtain the calcium carbonate fiber.
The invention provides a preparation method of calcium carbonate fiber for improving a cement-based composite material aiming at the current situation of the research of a modified cement-based composite material fiber material, which concentrates the particle size distribution of the calcium carbonate fiber and has higher dispersibility and fluidity by controlling the particle size of the calcium carbonate fiber and modifying the surface of the calcium carbonate fiber.
The invention relates to a preparation method of calcium carbonate fiber for cement mortar, which comprises the following steps: the calcium carbonate fiber is obtained by adopting a sol-gel method preparation process, and the process flow is shown in figure 1. In addition, because the calcium carbonate fiber has small size, the agglomeration effect is easy to occur, and the agglomeration phenomenon can occur when the calcium carbonate fiber is used with a cement material, so that the negative effect is generated on the performance of the cement material. However, the technology of the application utilizes the dispersing performance of the surfactant, introduces the surfactant in the process of preparing the calcium carbonate fiber to improve the agglomeration defect of the calcium carbonate fiber in the cement-based composite material, improves the dispersing rate of the calcium carbonate whisker in the cement-based composite material, reduces the agglomeration effect, and fully plays the role of a bridge of the whisker, thereby improving the performance of the cement-based composite material.
Furthermore, in the preparation method, the calcium carbonate fiber is prepared by a sol-gel method, the process is simple, the reaction process is easy to control, the components of the product are uniform, and all the used reagents are chemical analysis reagents.
Further, in step S4, sodium dodecyl sulfate with a weight ratio of 0.5% is preferably added and stirring is continued for 30min to obtain milk white liquid C, and drying is performed in a drying oven at a constant temperature of 100 ℃ to obtain dry gel D.
Further, in step S4, preferably, 1% by weight of sodium dodecyl sulfate is added and stirring is continued for 30min to obtain a milk white liquid C, and the milk white liquid C is dried in a drying oven at a constant temperature of 100 ℃ to obtain a dry gel D.
Further, in the step S2, the weight ratio of calcium carbonate to anhydrous acetic acid is 5: 15 and the xerogel D is calcined in step S5 in a muffle furnace at 600 ℃ for 2 h.
Further, in step S1, the calcium carbonate powder is cleaned, filtered, washed, and dried.
Further, the calcium carbonate fiber comprises the following components in percentage by weight: 5-40 parts of calcium carbonate and 5-40 parts of acetic acid; 5-40 parts of citric acid and 1-3 parts of surfactant.
Further, the surfactant is one or a mixture of two of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
Further, the calcium carbonate is 20-100nm of superfine light calcium.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the preparation method of the calcium carbonate fiber for improving the performance of the cement-based composite material has the advantages of simple process for preparing the calcium carbonate fiber by the sol-gel method, low equipment price, easily controlled reaction process and uniform product components.
2. According to the preparation method of the calcium carbonate fiber for improving the performance of the cement-based composite material, two ends of the calcium carbonate fiber are bonded with cement, so that a bridge function is achieved, and a cement-based system is supported. Due to the characteristics of high modulus and high strength of the calcium carbonate whisker, under the action of tensile stress, compressive stress and shear stress, the calcium carbonate whisker absorbs energy transmitted from external load in the processes of stretching, breaking and compressing, so that the damage degree of the cement stone under the action of load is reduced, and the strength of a test piece is improved when the mixing amount of the calcium carbonate whisker is within a certain range;
drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a flow chart of the method of the present invention.
Fig. 2 is a schematic view showing the dispersion of cement particles in water.
Fig. 3 is a schematic diagram of cement particles adsorbed on the surface of calcium carbonate fibers.
Reference numbers and corresponding part names in the drawings:
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
The method comprises the following steps:
step 1, according to calcium carbonate: the weight ratio of the absolute ethyl alcohol is 1: 2, cleaning, filtering and drying the calcium carbonate powder;
step 2, according to calcium carbonate: the weight ratio of acetic acid is 5: 10, stirring at the speed of 100-120r/min for 20min, and uniformly mixing to obtain a mixture. Standing for 2h to obtain a mixture solution A ((CH)3-COO)2Ca solution);
step 3, according to acetic acid: adding 40 parts by mass of citric acid and CH according to the weight ratio of 1:1 of citric acid3-COO)2In the Ca mixed solution, stirring for 30min at the speed of 100-120r/min, and uniformly mixing to ensure that the pH value tends to be stable (the pH value is approximately equal to 3.5) to obtain a mixture B;
and 4, mechanically stirring the mixture B in a constant-temperature water bath at 70 ℃ for 10min at 120r/min, adding 1 wt% of sodium dodecyl benzene sulfonate, continuously stirring for 30min to obtain a milky white liquid C, and drying in a constant-temperature drying oven at 100 ℃ to obtain a dry gel D.
And 5, calcining the dried gel D in a 600 ℃ muffle furnace for 2 hours to obtain the calcium carbonate fiber.
Example 2
The method comprises the following steps:
step 1, according to calcium carbonate: the weight ratio of the absolute ethyl alcohol is 1: 2, cleaning, filtering and drying the calcium carbonate powder;
step 2, according to calcium carbonate: the weight ratio of acetic acid is 5: 10, stirring at the speed of 100-120r/min for 20min, and uniformly mixing to obtain a mixture. Standing for 2h to obtain a mixture solution A ((CH)3-COO)2Ca solution);
step 3, according to acetic acid: adding 40 parts by mass of citric acid and CH according to the weight ratio of 1:1 of citric acid3-COO)2In the Ca mixed solution, the mixture solution A ((CH) was stirred at 100-120r/min3-COO)2Ca solution) for 30min, and the mixture B is obtained by leading the pH value to tend to be stable (pH is approximately equal to 3.5);
and 4, mechanically stirring the mixture B in a constant-temperature water bath at 70 ℃ for 10min at 120r/min, adding 0.5 wt% of sodium dodecyl sulfate, continuously stirring for 30min to obtain a milky liquid C, and drying in a constant-temperature drying oven at 100 ℃ to obtain a dry gel D.
And 5, calcining the dried gel D in a 600 ℃ muffle furnace for 2 hours to obtain the calcium carbonate fiber.
Example 3
The method comprises the following steps:
step 1, according to calcium carbonate: the weight ratio of the absolute ethyl alcohol is 1: 2, cleaning, filtering and drying the calcium carbonate powder;
step 2, according to calcium carbonate: the weight ratio of the anhydrous acetic acid is 5: 15, stirring at the speed of 100-120r/min for 20min, and uniformly mixing to obtain a mixture. Standing for 2h to obtain a mixture solution A ((CH)3-COO)2Ca solution);
step 3, according to anhydrous acetic acid: adding 40 parts by mass of citric acid and CH according to the weight ratio of 1:1 of citric acid3-COO)2In the Ca mixed solution, stirring for 30min at the speed of 100-120r/min, and uniformly mixing to ensure that the pH value tends to be stable (the pH value is approximately equal to 3.5) to obtain a mixture B;
and 4, mechanically stirring the mixture B in a constant-temperature water bath at 70 ℃ for 10min at 120r/min, adding 1 wt% of sodium dodecyl benzene sulfonate, continuously stirring for 30min to obtain a milky white liquid C, and drying in a constant-temperature drying oven at 100 ℃ to obtain a dry gel D.
And 5, calcining the dried gel D in a muffle furnace at 700 ℃ for 2h to obtain the calcium carbonate fiber.
Example 4
The method comprises the following steps:
step 1, according to calcium carbonate: the weight ratio of the absolute ethyl alcohol is 1: 2, cleaning, filtering, washing and drying the calcium carbonate powder;
step 2, according to calcium carbonate: the weight ratio of the anhydrous acetic acid is 5: 15, stirring at the speed of 100-120r/min for 20min, and uniformly mixing to obtain a mixture. Standing for 2h to obtain a mixture solution A ((CH)3-COO)2Ca solution);
step 3, according to anhydrous acetic acid: adding 40 parts by mass of citric acid and CH according to the weight ratio of 1:1 of citric acid3-COO)2In the Ca mixed solution, stirring for 30min at the speed of 100-120r/min, and uniformly mixing to ensure that the pH value tends to be stable (the pH value is approximately equal to 3.5) to obtain a mixture B;
step 4, mechanically stirring the mixture B in a constant-temperature water bath at 70 ℃ for 10min at 120r/min, adding 1 wt% of sodium dodecyl benzene sulfonate, continuously stirring for 30min to obtain a milky white liquid C, and drying in a constant-temperature drying oven at 100 ℃ to obtain a dry gel D;
and 5, calcining the dried gel D in a 600 ℃ muffle furnace for 2 hours to obtain the calcium carbonate fiber.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A preparation method of calcium carbonate fibers for improving the performance of a cement-based composite material is characterized by comprising the following steps:
s1: according to the weight ratio of 1: 2, cleaning, filtering and drying the calcium carbonate powder;
s2: according to the weight ratio of calcium carbonate to acetic acid of 5: 10, stirring at the speed of 100-120r/min for 20min, uniformly mixing to obtain a mixture, and standing for 2h to obtain a mixture A ((CH)3-COO)2Ca solution);
s3: adding 40 parts by mass of citric acid and (CH) according to the weight ratio of acetic acid to citric acid of 1:13-COO)2Stirring the Ca mixed solution for 30min at the speed of 100-120r/min, and uniformly mixing to ensure that the pH value tends to be stable to obtain a mixture B;
s4: mechanically stirring the mixture B in a constant-temperature water bath at 70 ℃ for 10min at 120r/min, adding 0.5-1 wt% of sodium dodecyl benzene sulfonate, continuously stirring for 30min to obtain a milky white liquid C, and drying in a constant-temperature drying oven at 100 ℃ to obtain a dry gel D;
s5: and (3) calcining the white milky white liquid in a 600 ℃ muffle furnace for 2h to obtain the calcium carbonate fiber.
2. The method for preparing calcium carbonate fiber for improving the performance of cement-based composite material according to claim 1, wherein in step S4, sodium dodecyl sulfate with weight ratio of 0.5% is preferably added and stirring is continued for 30min to obtain milk white liquid C, and drying is performed in a drying oven at constant temperature of 100 ℃ to obtain xerogel D.
3. The method for preparing calcium carbonate fiber for improving the performance of cement-based composite material according to claim 1, wherein in step S4, sodium dodecyl sulfate with a weight ratio of 1% is preferably added and the stirring is continued for 30min to obtain milk white liquid C, and the drying is performed in a drying oven at constant temperature of 100 ℃ to obtain xerogel D.
4. The method for preparing calcium carbonate fiber for improving the performance of cement-based composite material as claimed in claim 1, wherein the weight ratio of calcium carbonate and anhydrous acetic acid in step S2 is 5: 15 and the xerogel D is calcined in step S5 in a muffle furnace at 600 ℃ for 2 h.
5. The method of claim 4, wherein in step S1, the calcium carbonate powder is cleaned, filtered, washed, and dried.
6. The method for preparing the calcium carbonate fiber for improving the performance of the cement-based composite material as claimed in claim 1, wherein the calcium carbonate fiber consists of the following components in percentage by weight: 5-40 parts of calcium carbonate and 5-40 parts of acetic acid; 5-40 parts of citric acid and 1-3 parts of surfactant.
7. The method for preparing calcium carbonate fiber for improving the performance of cement-based composite material as claimed in claim 6, wherein the surfactant is one or a mixture of two of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
8. The method for preparing calcium carbonate fiber for improving the performance of cement-based composite material as claimed in claim 1, wherein the calcium carbonate is 20-100nm of ultra-fine light calcium.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102943306A (en) * | 2012-11-27 | 2013-02-27 | 大连理工大学 | Calcium carbonate whisker synthesizing and modified integrating method based on sol-gel method |
| CN103408972A (en) * | 2013-07-03 | 2013-11-27 | 青阳县永诚钙业有限责任公司 | High-glossiness modified calcium carbonate for air conditioner housings and preparation method thereof |
| CN106032287A (en) * | 2016-02-16 | 2016-10-19 | 沈阳建筑大学 | Preparation method of oil-dispersing calcium carbonate ultrafine powder |
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- 2021-10-15 CN CN202111203287.4A patent/CN113913968A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102943306A (en) * | 2012-11-27 | 2013-02-27 | 大连理工大学 | Calcium carbonate whisker synthesizing and modified integrating method based on sol-gel method |
| CN103408972A (en) * | 2013-07-03 | 2013-11-27 | 青阳县永诚钙业有限责任公司 | High-glossiness modified calcium carbonate for air conditioner housings and preparation method thereof |
| CN106032287A (en) * | 2016-02-16 | 2016-10-19 | 沈阳建筑大学 | Preparation method of oil-dispersing calcium carbonate ultrafine powder |
Non-Patent Citations (1)
| Title |
|---|
| 谢元彦;杨海林;阮建明;周忠诚;: "溶胶-凝胶法制备碳酸钙晶须", 粉末冶金材料科学与工程, no. 03, pages 76 - 77 * |
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