CN113754335A - Preparation method of silicon carbide whisker dispersion liquid applied to cement-based material - Google Patents
Preparation method of silicon carbide whisker dispersion liquid applied to cement-based material Download PDFInfo
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- CN113754335A CN113754335A CN202110926136.5A CN202110926136A CN113754335A CN 113754335 A CN113754335 A CN 113754335A CN 202110926136 A CN202110926136 A CN 202110926136A CN 113754335 A CN113754335 A CN 113754335A
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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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Abstract
The invention provides a preparation method of silicon carbide whisker dispersion liquid with stable dispersion and applied to cement-based materials, which comprises the steps of adding silicon carbide whisker and a polycarboxylic acid water reducing agent into a calcium hydroxide aqueous solution with the pH value of 9-11, and sequentially carrying out magnetic stirring and ultrasonic dispersion to obtain the silicon carbide whisker dispersion liquid applied to the cement-based materials; the mass of the silicon carbide whisker is 0.2-0.6% of that of the calcium hydroxide solution; the mass of the polycarboxylate superplasticizer is 0.2-0.5% of that of the calcium hydroxide solution. The invention utilizes the calcium hydroxide contained in the cement to adjust the pH of the silicon carbide whisker dispersion liquid, thereby improving the stability and the dispersity of the silicon carbide whiskers in the dispersion liquid and leading the silicon carbide whiskers to be dispersed more uniformly in the cement slurry.
Description
Technical Field
The invention relates to a preparation method of silicon carbide whisker dispersion liquid applied to a cement-based material.
Background
Silicon Carbide Whiskers (SiCw) are a material with high strength and high elastic modulus, have good high-temperature resistance and corrosion resistance, and are mostly applied to modification of ceramic substrates and metal-based materials. But the application of the silicon carbide whisker in the cement-based material is almost not.
The cement-based material belongs to quasi-brittle materials, the compressive strength of the cement-based material is higher than the tensile strength, and the defect of brittleness and easy cracking exists generally. Expert scholars have adopted many research schemes to solve the above problems, and the modification of cement-based materials by adding various fibers, carbon nanomaterials and whiskers is currently adopted in several methods. The whiskers are micro-nano short fibers grown from single crystals, and calcium carbonate whiskers and calcium sulfate whiskers are common in cement-based materials, but the strength and hardness of the whiskers are far lower than those of silicon carbide whiskers. If the silicon carbide whisker can be applied to the cement-based material by a new technical means, the constructed new composite material can provide a new idea for solving the brittleness problem of the cement-based material.
Because of the nanometer size of the silicon carbide crystal whisker needle rod shape and the large specific surface area, the aggregation of the silicon carbide crystal whisker is caused by the large van der Waals force between the crystal whisker and the crystal whisker, so that the dispersion of the silicon carbide crystal whisker is difficult, and the application of the silicon carbide crystal whisker in cement-based materials is hindered. The stable silicon carbide whisker dispersion liquid can ensure that the silicon carbide whiskers are dispersed in the cement slurry more uniformly, so that the positive effect of the silicon carbide whisker dispersion liquid on the performance of the cement-based material can be better exerted. However, the existing dispersing method of the nano material mainly adopts mechanical stirring, the obtained dispersing liquid is not stable enough, and can be layered and precipitated after a certain time, and particles can be agglomerated again. Chinese patent CN202011392151 discloses a method for dispersing silicon carbide whiskers in the application of preparing wear-resistant toughened anti-cracking cement-based materials, wherein the method directly uses a hydrated polycarboxylic acid water reducing agent to disperse the silicon carbide whiskers, but the problem that the prepared silicon carbide whisker dispersion liquid is unstable and easy to separate layers exists, which can adversely affect the dispersion of the silicon carbide whiskers in the cement-based materials. Therefore, how to prepare stable silicon carbide whisker dispersion liquid for application in cement-based materials still remains a problem to be solved urgently.
Disclosure of Invention
In order to overcome the defect that the silicon carbide whisker dispersion liquid in the prior art is not stable enough, the invention provides a preparation method of the silicon carbide whisker dispersion liquid which is stably dispersed and applied to a cement-based material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of silicon carbide whisker dispersion liquid applied to a cement-based material, which comprises the following steps: adding silicon carbide whiskers and a polycarboxylic acid water reducing agent into a calcium hydroxide aqueous solution with the pH value of 9-11, and sequentially carrying out magnetic stirring and ultrasonic dispersion to obtain the silicon carbide whisker dispersion liquid applied to the cement-based material; the mass of the silicon carbide whisker is 0.2-0.6% (preferably 0.4%) of the calcium hydroxide solution; the mass of the polycarboxylate superplasticizer is 0.2-0.5% (preferably 0.3%) of the calcium hydroxide solution.
Preferably, the pH of the aqueous calcium hydroxide solution is 11.
The polycarboxylate superplasticizer is an additive commonly used for cement-based materials, and can be used as a dispersing agent of silicon carbide whiskers to prevent the cement-based materials from being deteriorated in strength due to the addition of the dispersing agent. The dispersing mechanism is that the polycarboxylate superplasticizer presents a tooth-shaped adsorption form on the surface of silicon carbide whiskers, the polycarboxylate superplasticizer molecules present a comb-shaped structure, a main chain is connected with a branched chain and a substituent group, such as-COOH, -OH and the like, and a side chain contains a plurality of ether bonds-C-O-C. The reaction of the oxygen of the ether bond with water molecules in the aqueous solution can form strong hydrogen bonds, and when the polycarboxylic acid-based polymer is adsorbed on the surface of the silicon carbide whisker, a strongly dispersible hydrophilic steric protective film is formed, thereby dispersing the agglomerated silicon carbide whisker.
The magnetic stirrer and the ultrasonic dispersion method preferably adopt the sequence of firstly using the magnetic stirrer and then using the ultrasonic dispersion. The magnetic stirrer drives the stirrer to rotate through a rotating magnetic field, and is matched with a polycarboxylic acid water reducing agent to carry out preliminary dispersion on the silicon carbide crystal whiskers. The agglomerated silicon carbide whiskers are further dispersed by ultrasonic dispersion under the action of a polycarboxylate water reducing agent at a higher energy density, and the crystal straightening rate of the silicon carbide whiskers is damaged by overlong ultrasonic dispersion time, so that the modification effect of the silicon carbide whiskers on the cement-based material is influenced.
Further, the magnetic stirring conditions are as follows: the rotating speed is 600-1000 rpm, the power is 40W, and the stirring time is 10-20 min. Preferably, the rotation speed is 800 rpm, the power is 40W, and the stirring time is 15 min.
Further, the conditions of the ultrasonic dispersion are as follows: the dispersing power is 50-80W, the dispersing time is 4-10min, and the temperature is 35-40 ℃. Preferably, the dispersing power is 60W, the dispersing time is 4min and the temperature is 40 ℃. The invention recommends that the silicon carbide whisker dispersion liquid is placed in ice bath for ultrasonic treatment, so as to avoid overheating in the ultrasonic treatment process.
The invention particularly recommends that the method is: adding silicon carbide whiskers and a polycarboxylic acid water reducing agent into a calcium hydroxide aqueous solution with the pH value of 11, and sequentially carrying out magnetic stirring and ultrasonic dispersion to obtain the silicon carbide whisker dispersion liquid applied to the cement-based material; the mass of the silicon carbide whisker is 0.4 percent of that of the calcium hydroxide solution; the mass of the polycarboxylic acid water reducing agent is 0.3 percent of that of the calcium hydroxide solution; the magnetic stirring conditions are that the rotating speed is 800 rpm, the power is 40W, and the stirring time is 15 min; the conditions of ultrasonic dispersion are as follows: the dispersing power is 60W, the dispersing time is 4min, and the temperature is 40 ℃.
Compared with the prior art, the invention has the beneficial effects that: the pH value of the silicon carbide whisker dispersion liquid is adjusted by utilizing calcium hydroxide which is a component contained in the cement, so that the stability and the dispersity of the silicon carbide whiskers in the dispersion liquid are improved, the silicon carbide whiskers are dispersed in the cement slurry more uniformly, and the positive effect of the silicon carbide whiskers on the performance of the cement-based material is better exerted.
Drawings
FIG. 1 is a microscopic morphology of silicon carbide whiskers in a silicon carbide whisker dispersion liquid applied to a cement-based material according to the present invention;
FIG. 2 is a flow chart of a method of preparing a silicon carbide whisker dispersion for use in cement-based materials in accordance with the present invention;
FIG. 3 is a graph showing the effect of pH on zeta potential on the surface of silicon carbide whiskers in a silicon carbide whisker dispersion of the present invention applied to a cement-based material;
FIG. 4 is a graph showing the effect of pH on the absorbance of a silicon carbide whisker dispersion according to the invention in a silicon carbide whisker dispersion applied to a cement-based material;
FIG. 5 is a graph showing the influence of the amount of a polycarboxylic acid water reducing agent incorporated in a silicon carbide whisker dispersion liquid applied to a cement-based material on the zeta potential on the surface of a silicon carbide whisker according to the present invention;
FIG. 6 is a graph showing the effect of the amount of a polycarboxylic acid water reducing agent incorporated in a silicon carbide whisker dispersion liquid applied to a cement-based material on the absorbance of the silicon carbide whisker dispersion liquid.
FIG. 7 is a graph showing the effect of pH on the dispersion rate of a silicon carbide whisker dispersion in a silicon carbide whisker dispersion applied to a cement-based material according to the present invention
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
the room temperature of the embodiment of the invention is 22 +/-1 ℃.
Reagents and apparatus in the following examples: calcium hydroxide powder (purchased from Baishi chemical Co., Ltd., Tianjin, analytical purity), a magnetic stirrer (purchased from photosynthetic DF-101S, model number, Ministry of technology, Ministry of Hunan), and an ultrasonic disperser (purchased from FS-750T, model number, Ministry of technology, Ministry of Hunan).
Example 1
0.16g of silicon carbide crystal whisker (purchased from Beijing Huawei Ruiki chemical Co., Ltd.) and 0.12g of dispersant polycarboxylate superplasticizer (purchased from Wulong New materials Co., Ltd., model ZWL-PG-VI polycarboxylate superplasticizer, Zhejiang) are taken into a beaker, and 40g of calcium hydroxide solution with the pH values of 7, 8, 9, 10, 11 and 12 are added into the beaker. Dispersing the mixed solution by a heat collection type magnetic stirrer (the magnetic stirrer is purchased from Hunan leading edge science and technology Limited company, and the model is photosynthetic DF-101S), wherein the rotating speed is 800 r/m, the power is 40W, and the stirring time is 15 min; immediately performing ultrasonic ice-bath dispersion (an ultrasonic dispersion instrument is purchased from Shannan frontier science and technology Co., Ltd., FS-750T type) after magnetic stirring dispersion, wherein the dispersion power is 60W, the dispersion time is 4min, and the limited temperature is 40 ℃;
placing the silicon carbide whisker dispersion liquid in a Marvens nanometer particle size analyzer Nano ZS90 to measure the zeta potential of the silicon carbide whisker surface, wherein the influence of the pH value on the zeta potential of the silicon carbide whisker is shown in FIG. 3;
as can be seen from FIG. 3, when the pH was 9 to 11, the zeta potential was large in absolute value, and the silicon carbide dispersion was stable.
Example 2
0.16g of silicon carbide whisker and 0.12g of dispersant polycarboxylate superplasticizer (purchased from Wulong, New materials, Inc. of Zhejiang, model number ZWL-PG-VI) are taken to be put in a beaker, and 40g of calcium hydroxide solution with the pH values of 7, 8, 9, 10, 11 and 12 are added in the beaker. Dispersing the mixed solution by a heat collection type magnetic stirrer (the magnetic stirrer is purchased from Hunan leading edge science and technology Limited company, and the model is photosynthetic DF-101S), wherein the rotating speed is 800 r/m, the power is 40W, and the stirring time is 15 min; immediately performing ultrasonic ice-bath dispersion (an ultrasonic dispersion instrument is purchased from Shannan frontier science and technology Co., Ltd., FS-750T type) after magnetic stirring dispersion, wherein the dispersion power is 60W, the dispersion time is 4min, and the limited temperature is 40 ℃;
standing the silicon carbide whisker dispersion liquid for 24h, taking the supernatant, and placing the supernatant in an ultraviolet spectrophotometer to measure the absorbance of the dispersion liquid, wherein the influence of the pH value on the absorbance of the silicon carbide whisker dispersion liquid is shown in figure 4;
as can be seen from fig. 4, the absorbance was the highest when the pH was 11 to 12, indicating that the supernatant of the sample also contained a large amount of silicon carbide whiskers, and the silicon carbide whisker dispersion was stable.
Example 3
0.16g of silicon carbide crystal whisker is taken in a beaker, and then dispersant polycarboxylate superplasticizer (purchased from Wulong, New materials, Inc. of Zhejiang, model number ZWL-PG-VI) is added, the mixing amounts are 0%, 0.2%, 0.3%, 0.4% and 0.5% respectively. 40g of calcium hydroxide solution having a pH of 11 were added to the beaker. Dispersing the mixed solution by a heat collection type magnetic stirrer (the magnetic stirrer is purchased from Hunan leading edge science and technology Limited company, and the model is photosynthetic DF-101S), wherein the rotating speed is 800 r/m, the power is 40W, and the stirring time is 15 min; immediately performing ultrasonic ice-bath dispersion (an ultrasonic dispersion instrument is purchased from Shannan frontier science and technology Co., Ltd., FS-750T type) after magnetic stirring dispersion, wherein the dispersion power is 60W, the dispersion time is 4min, and the limited temperature is 40 ℃;
placing the silicon carbide whisker dispersion liquid in a Marvens nanometer particle size analyzer Nano ZS90 to measure the zeta potential of the silicon carbide whisker surface, wherein the influence of the water reducing agent doping amount on the zeta potential of the silicon carbide whisker is shown in FIG. 5;
as can be seen from FIG. 5, when the amount of the water reducing agent is 0.2 to 0.5%, the zeta potential absolute value is large, and the silicon carbide dispersion liquid is stable.
Example 4
0.16g of silicon carbide crystal whisker is taken in a beaker, and then dispersant polycarboxylate superplasticizer (purchased from Wulong, New materials, Inc. of Zhejiang, model number ZWL-PG-VI) is added, the mixing amounts are 0%, 0.2%, 0.3%, 0.4% and 0.5% respectively. 40g of calcium hydroxide solution having a pH of 11 were added to the beaker. Dispersing the mixed solution by a heat collection type magnetic stirrer (the magnetic stirrer is purchased from Hunan leading edge science and technology Limited company, and the model is photosynthetic DF-101S), wherein the rotating speed is 800 r/m, the power is 40W, and the stirring time is 15 min; immediately performing ultrasonic ice-bath dispersion (an ultrasonic dispersion instrument is purchased from Shannan frontier science and technology Co., Ltd., FS-750T type) after magnetic stirring dispersion, wherein the dispersion power is 60W, the dispersion time is 4min, and the limited temperature is 40 ℃;
standing the silicon carbide whisker dispersion liquid for 24h, taking the supernatant, placing the supernatant into an ultraviolet spectrophotometer, and measuring the absorbance of the dispersion liquid, wherein the influence of the mixing amount of the water reducing agent on the absorbance of the silicon carbide whisker dispersion liquid is shown in FIG. 6;
as can be seen from FIG. 6, when the water reducing agent is added in an amount of 0.2 to 0.5%, the absorbance is relatively high, which indicates that the supernatant of the sample also contains a lot of silicon carbide whiskers, and the silicon carbide whisker dispersion is relatively stable.
Example 5
0.16g of silicon carbide whisker and 0.12g of dispersant polycarboxylate superplasticizer (purchased from Jilong chemical building materials Co., Ltd.) were put in a beaker, and 40g of calcium hydroxide solution having pH values of 7, 8, 9, 10, 11 and 12, respectively, were added in the beaker. Dispersing the mixed solution by a heat collection type magnetic stirrer (the magnetic stirrer is purchased from Hunan leading edge science and technology Limited company, and the model is photosynthetic DF-101S), wherein the rotating speed is 800 r/m, the power is 40W, and the stirring time is 15 min; immediately performing ultrasonic ice-bath dispersion (an ultrasonic dispersion instrument is purchased from Shannan frontier science and technology Co., Ltd., FS-750T type) after magnetic stirring dispersion, wherein the dispersion power is 60W, the dispersion time is 4min, and the limited temperature is 40 ℃;
the dispersion was left to stand, and the dispersion ratios at different times were measured, and the influence of the pH value on the dispersion ratio of the silicon carbide whisker dispersion is shown in fig. 7;
as can be seen from fig. 7, when the pH was 11 to 12, the silicon carbide whisker dispersion rate decreased less after the standing for a long time, indicating that the silicon carbide whisker dispersion liquid was stable.
Example 6
Magnetic stirring time and stirring speedThe influence of the four factors of the sound wave dispersion time, the pH value of the solution and the doping amount of the polycarboxylate superplasticizer on the dispersion effect of the silicon carbide crystal whisker is preliminarily explored, four-factor and three-level orthogonal tests are designed, and the factors and the levels thereof are shown in table 1. Selecting L9(34) In the orthogonal table, the results of quantitative analysis of 9 test groups using the silicon carbide whisker dispersion ratio as an index are shown in table 2. The mixing amount of each group of silicon carbide whiskers is 0.4 percent. After 40ml of the silicon carbide whisker dispersion was dispersed, it was immediately poured into a test tube, and the height H of the initial dispersion was measured0Standing for the same time, and measuring the boundary height Hl，Hl/H0That is, the dispersion rate is as high as possible. The analysis of test results shows that the main and secondary sequence of the influence on the dispersion of the silicon carbide whiskers is as follows: the pH value of the solution is more than the mixing amount of the water reducing agent, the magnetic stirring time is more than the ultrasonic dispersion time. The experiment shows that the solution with the pH value of 11 and the water reducing agent mixing amount of 0.3 percent is most beneficial to the dispersion of the silicon carbide crystal whiskers, and the optimal treatment mode of the suspension is that the suspension is stirred magnetically for 15min and then stirred ultrasonically for 4 min. The examples were carried out on the basis of this preliminary exploration.
TABLE 1 factors and levels of orthogonal experiments
TABLE 2 analysis of orthogonal test results
Claims (9)
1. A preparation method of silicon carbide whisker dispersion liquid applied to cement-based materials is characterized by comprising the following steps: adding silicon carbide whiskers and a polycarboxylic acid water reducing agent into a calcium hydroxide aqueous solution with the pH value of 9-11, and sequentially carrying out magnetic stirring and ultrasonic dispersion to obtain the silicon carbide whisker dispersion liquid applied to the cement-based material; the mass of the silicon carbide whisker is 0.2-0.6% of that of the calcium hydroxide solution; the mass of the polycarboxylate superplasticizer is 0.2-0.5% of that of the calcium hydroxide solution.
2. The method for preparing silicon carbide whisker dispersion liquid for cement-based materials according to claim 1, wherein: the pH of the aqueous calcium hydroxide solution was 11.
3. The method for preparing silicon carbide whisker dispersion liquid for cement-based materials according to claim 1, wherein: the mass of the silicon carbide whisker is 0.4 percent of that of the calcium hydroxide solution.
4. The method for preparing silicon carbide whisker dispersion liquid for cement-based materials according to claim 1, wherein: the mass of the polycarboxylate superplasticizer is 0.3 percent of the calcium hydroxide solution.
5. The method for preparing silicon carbide whisker dispersion for cement-based materials according to claim 1, wherein the magnetic stirring conditions are: the rotating speed is 600-1000 rpm, the power is 40W, and the stirring time is 10-20 min.
6. The method for preparing silicon carbide whisker dispersion for cement-based materials according to claim 5, wherein the magnetic stirring conditions are: the rotating speed is 800 rpm, the power is 40W, and the stirring time is 15 min.
7. The method for preparing silicon carbide whisker dispersion liquid for cement-based materials according to claim 1, wherein the ultrasonic dispersion conditions are as follows: the dispersing power is 50-80W, the dispersing time is 4-10min, and the temperature is 35-40 ℃.
8. The method for preparing silicon carbide whisker dispersion liquid for cement-based materials according to claim 1, wherein the ultrasonic dispersion conditions are as follows: the dispersing power is 60W, the dispersing time is 4min, and the temperature is 40 ℃.
9. The method for preparing silicon carbide whisker dispersion for cement-based materials according to claim 1, wherein the method comprises: adding silicon carbide whiskers and a polycarboxylic acid water reducing agent into a calcium hydroxide aqueous solution with the pH value of 11, and sequentially carrying out magnetic stirring and ultrasonic dispersion to obtain the silicon carbide whisker dispersion liquid applied to the cement-based material; the mass of the silicon carbide whisker is 0.4 percent of that of the calcium hydroxide solution; the mass of the polycarboxylic acid water reducing agent is 0.3 percent of that of the calcium hydroxide solution; the magnetic stirring conditions are that the rotating speed is 800 rpm, the power is 40W, and the stirring time is 15 min; the conditions of ultrasonic dispersion are as follows: the dispersing power is 60W, the dispersing time is 4min, and the temperature is 40 ℃.
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| CN112456906A (en) * | 2020-12-01 | 2021-03-09 | 浙江工业大学 | Application of silicon carbide whiskers in preparation of wear-resistant toughened anti-crack cement-based material |
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| YINGJIA LAN等: ""Preliminary investigation on silicon carbide whisker-modified cement-based composites"", 《OPEN CERAMICS》 * |
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Application publication date: 20211207 |