CN107540355B - Preparation method of light refractory material - Google Patents
Preparation method of light refractory material Download PDFInfo
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Abstract
The invention relates to a preparation method of a light refractory material, and belongs to the technical field of materials. Adding polyvinylpyrrolidone, absolute ethyl alcohol, deionized water and styrene into a three-neck flask, introducing nitrogen, and stirring; preparing divinylbenzene, absolute ethyl alcohol and deionized water into a mixed solution, dropwise adding the mixed solution into a three-neck flask, continuing to react after the dropwise adding is finished, and filtering to obtain polystyrene microspheres; ball-milling bauxite and mica to obtain ball-milled powder; placing the ball-milling powder and hydrogen peroxide in a beaker, and filtering after ultrasonic oscillation to obtain modified ball-milling powder; pouring the polystyrene microspheres, ethanol, deionized water and a surfactant into a beaker, stirring, adding the ball-milling powder and a sulfuric acid solution, stirring, filtering, washing and drying to obtain the alumina hollow microspheres; stirring the alumina hollow microspheres, the aluminum silicate, the dispersant, the perlite and the deionized water, filling the prepared stirring slurry into a mold, freeze-drying and sintering to obtain the light refractory material.
Description
Technical Field
The invention relates to a preparation method of a light refractory material, and belongs to the technical field of materials.
Background
In the modern society, energy and environmental problems are receiving more and more attention. The development of energy-saving, environment-friendly and eco-friendly green refractory materials as the base material of high temperature industry is also an important direction for the future development of refractory materials. The light unshaped refractory material has good heat insulation and preservation effects, can effectively reduce the energy loss, can be directly used without high-temperature sintering, and conforms to the idea of green refractory materials. With the development of society and the progress of science and technology, the variety of thermal equipment is more and more, the use requirement on light refractory materials is more and more, and therefore, the high-performance light refractory materials meeting special use environments are in the forefront. The refractory material is an important basic material for high-temperature industries such as steel, cement, ceramics, glass and the like, and has important influence on high-temperature industrial products and processing products. The steel industry is a large consumer of refractory materials, and the consumption of the steel industry accounts for more than half of the total amount of the refractory materials. Therefore, the refractory material is one of the important guarantees for the development and progress of the steel industry, and the quality and performance of the refractory material have important influence on the steel production and processing. Today, the global refractory industry is changing tremendously. With the development and progress of industrial technology, the production process and production equipment are more and more advanced, and the continuous improvement and improvement of the quality and performance of the refractory materials lead the consumption of the refractory materials to be reduced year by year. Along with the increasing of the global economic globalization degree, the competition among the global refractory material enterprises is intensified day by day, and the refractory material enterprises need to improve the product research and development ability continuously, so that the variety of the refractory materials is more and more, the quality and the performance of refractory material products are improved continuously, and the use requirements of users can be met more. Meanwhile, the awareness and the capability of the refractory material enterprises for serving customers are continuously enhanced, so that the enterprises can have stronger competitiveness and occupy a place in intense competition. Under the current market economic situation, a plurality of small-scale small and medium-sized enterprises with low product quality and poor competitiveness are gradually eliminated. At present, the global refractory material enterprises are gradually realizing the optimization and recombination of the enterprises, which is more beneficial to the optimization and utilization of market resources and promotes the development of the refractory material industry. Under the situation of strongly advocating the development of low-carbon economy all over the world, energy conservation and consumption reduction become problems to be solved by high-temperature industry. The refractory material is used as a base material of high-temperature industry, has extremely important significance in developing energy-saving, environment-friendly and eco-friendly green refractory materials, and is related to the sustainable development of the refractory material industry in China currently and in future. The total yield and product types of refractory materials in China are the first in the world. In recent years, the development of Chinese refractory materials is rapid, the variety of products is complete, and the quality is greatly improved, so China becomes one of important refractory material bases in the world. Industrial refractory materials such as steel, nonferrous metal, chemical industry and the like mainly meet domestic requirements, and some higher-grade refractory products are exported to a plurality of developed countries. In addition, China is also an important refractory raw material base in the world and plays an important role in the global refractory industry. However, compared with the developed national refractory material, the development of the national refractory material has a great gap, which is mainly expressed as follows: the average consumption of the refractory materials for the iron and steel industry is far higher than the international advanced level, and the quality and the service life of the refractory materials have certain difference; the high-performance and long-life refractory materials are few, mainly comprise primary products, and have low technical content and high energy consumption; the waste of resources is serious, the consumption speed is too high, the raw material resources are lost, and the resource utilization is unreasonable; environmental pollution and waste recycling. The unused refractory raw materials and the piled refractory materials after use can cause air pollution and land desertification, and the chromium-containing refractory materials can cause harm to the environment and human bodies. The recycling rate of the waste materials and the used refractory materials caused by production is low, and the resource waste is serious. Therefore, the refractory industry in China is developed towards energy conservation, ecology, environmental protection and low waste. "Green refractory" can be summarized as: resource and energy conservation, excellent variety and quality, harmless use process and environment-friendly production process. The green development integrates multiple benefits, and all advanced, scientific and reasonable concepts, management and technologies are beneficial to the development of refractory materials. The light refractory material is one of important components of the refractory material, has good heat insulation and preservation effects, can reduce heat loss of thermal equipment in the using process, reduces energy waste, reduces waste gas generated by energy combustion, and accords with the energy-saving, environment-friendly and eco-friendly concept of green refractory materials.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems of poor uniformity, poor fire resistance and mechanical property and high energy consumption of the traditional refractory material, the preparation method of the refractory material is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) adding 10-20 g of polyvinylpyrrolidone, 8-16 g of absolute ethyl alcohol, 20-30 g of deionized water and 40-50 g of styrene into a three-neck flask, introducing nitrogen, adjusting the temperature, and stirring to obtain a stirring solution;
(2) preparing divinylbenzene, absolute ethyl alcohol and deionized water into a mixed solution according to the mass ratio of 1:1:3, dropwise adding the mixed solution into a three-neck flask, and filtering after reaction to obtain polystyrene microspheres;
(3) ball-milling 50-60 g of bauxite and 5-6 g of mica to obtain ball-milled powder;
(4) placing the ball-milling powder and hydrogen peroxide in a beaker, and filtering after ultrasonic oscillation to obtain modified ball-milling powder;
(5) pouring polystyrene microspheres, 50m L ethanol, 50m L deionized water and 5m L surfactant into a beaker, stirring, adding ball-milling powder and 40-50 m L sulfuric acid solution, stirring, filtering, repeatedly washing with deionized water, and naturally drying to obtain aluminum oxide hollow microspheres;
(6) placing hollow alumina microspheres, 10-20 g of aluminum silicate, 5-8 g of dispersing agent, 15-20 g of perlite and 40-50 g of deionized water in a beaker for stirring, then filling the beaker into a block-shaped mold, placing the mold in a freezing box for freezing for 20-24 h, and then placing the mold in a freeze drier for freeze drying to obtain a solidified material;
(7) and sintering the solidified material in a sintering furnace to obtain the light refractory material.
And (2) introducing nitrogen at a speed of 30-40 m L.
And (3) dropwise adding the mixed solution in the step (2) at a speed of 10m L/min.
The sulfuric acid solution in the step (5) is 25 percent.
And (4) the pressing pressure in the step (6) is 30-40 MPa.
The sintering temperature in the step (7) is 600-800 ℃.
Compared with other methods, the method has the beneficial technical effects that:
(1) in the process of preparing the light refractory material, the alumina hollow microspheres are prepared by taking the alumina as the main raw material, so that the refractory capacity and the mechanical strength of the material are greatly improved, and the prepared material has lower density.
(2) In the process of preparing the light refractory material, the prepared stirring slurry is frozen at low temperature and then dried and sintered, the method can reduce energy consumption to a certain extent, and the method can increase the aperture ratio of the prepared material and reduce the density of the material.
Detailed Description
The preparation method comprises the steps of adding 10-20 g of polyvinylpyrrolidone, 8-16 g of absolute ethyl alcohol, 20-30 g of deionized water and 40-50 g of styrene into a three-neck flask provided with a stirrer, a thermometer and a nitrogen pipe, introducing nitrogen at the speed of 30-40 m L/min for 15-20 min, adjusting the temperature to 55-65 ℃, stirring at the speed of 120-150 r/min for 1-2 h to obtain a stirring liquid, preparing a mixed solution from divinylbenzene, absolute ethyl alcohol and deionized water at the mass ratio of 1:1:3, dropwise adding the mixed solution into the three-neck flask at the speed of 10m L/min, continuing to react for 18-22 h after dropwise addition is completed, filtering to obtain polystyrene microspheres, taking 50-60 g of bauxite and 5-6 g of mica, placing the mixture into a ball milling tank, ball milling at the rotation speed of 200-300 r/min for 1-2 h to obtain a ball milling powder, placing the ball milling powder into a flame-resistant aluminum oxide curing powder which the mass fraction is 20-20 m L% of 20m, placing the flame resistant aluminum oxide curing powder into a beaker, stirring machine, placing the flame resistant aluminum oxide curing agent into a flame retardant curing furnace, stirring machine, placing the flame retardant curing furnace, stirring the flame retardant curing furnace, placing the flame retardant curing furnace, stirring furnace, placing the flame retardant curing furnace, the flame retardant curing furnace, the flame retardant curing furnace, the flame retardant, the.
Example 1
The preparation method comprises the steps of adding 10g of polyvinylpyrrolidone, 8g of absolute ethyl alcohol, 20g of deionized water and 40g of styrene into a three-neck flask provided with a stirrer, a thermometer and a nitrogen pipe, introducing nitrogen at 30m L/min for 15min, adjusting the temperature to 55 ℃, stirring at 120r/min for 1h to obtain a stirring solution, preparing a mixed solution by adding divinylbenzene, absolute ethyl alcohol and deionized water at a mass ratio of 1:1:3, dropwise adding the mixed solution into the three-neck flask at a speed of 10m L/min, continuing to react for 18h after dropwise addition is completed, filtering to obtain polystyrene microspheres, adding 50g of bauxite and 5g of mica into a ball milling tank, carrying out ball milling at a rotating speed of 200r/min for 1h to obtain ball milling powder, placing the ball milling powder into 20% by mass fraction of 500m L in hydrogen peroxide water, placing the hydrogen peroxide into a beaker, placing the hollow beaker into a 180W ultrasonic oscillation instrument, carrying out ultrasonic oscillation for 8h, filtering to obtain modified ball milling powder, placing the polystyrene microspheres into a baking oven, placing the hollow beaker into a baking oven, placing the baking oven, the.
Example 2
Adding 15g of polyvinylpyrrolidone, 12g of absolute ethyl alcohol, 25g of deionized water and 45g of styrene into a three-mouth flask provided with a stirrer, a thermometer and a nitrogen pipe, introducing nitrogen at 35m L/min for 17min, adjusting the temperature to 60 ℃, stirring at 135r/min for 1h to obtain a stirring solution, preparing a mixed solution by adding divinylbenzene, absolute ethyl alcohol and deionized water at a mass ratio of 1:1:3, dropwise adding the mixed solution into the three-mouth flask at a speed of 10m L/min, continuing to react for 20h after the dropwise addition is completed, filtering to obtain polystyrene microspheres, taking 55g of bauxite and 5.5g of mica, placing the bauxite into a pot, performing ball milling at a rotating speed of 250r/min for 1.5h to obtain ball milling powder, placing the ball milling powder into a beaker with 20% by mass fraction of hydrogen peroxide water, placing the beaker into a 200W ultrasonic oscillation instrument, performing ultrasonic oscillation filtration for 8h to obtain modified ball milling powder, placing the polystyrene microspheres into a ball milling tank, placing the beaker into a baking oven, placing the baking oven for 50m L mass fraction of 20% of hydrogen peroxide, placing the baking powder into a baking oven, placing the baking oven at a temperature of 50m of a baking oven, placing the baking oven at a baking oven, placing the baking oven at a temperature of 50m of a baking oven, placing the.
Example 3
The preparation method comprises the steps of adding 20g of polyvinylpyrrolidone, 16g of absolute ethyl alcohol, 30g of deionized water and 50g of styrene into a three-neck flask provided with a stirrer, a thermometer and a nitrogen pipe, introducing nitrogen at 40m L/min for 20min, adjusting the temperature to 65 ℃, stirring at 150r/min for 2h to obtain a stirring liquid, preparing a mixed solution by adding divinylbenzene, absolute ethyl alcohol and deionized water at a mass ratio of 1:1:3, dropwise adding the mixed solution into the three-neck flask at a speed of 10m L/min, continuing to react for 22h after dropwise addition is completed, filtering to obtain polystyrene microspheres, taking 60g of bauxite and 6g of mica, placing the bauxite and mica into a ball milling tank for ball milling for 2h at a rotating speed of 200-300 r/min to obtain ball milling powder, placing the ball milling powder into a 20% by stirring speed of 20% hydrogen peroxide water, placing the ball milling powder into a hollow beaker, placing the hollow beaker into a 220W ultrasonic oscillation instrument, filtering after ultrasonic oscillation for 9h to obtain modified powder, placing the ball milling powder into a ball milling tank, placing the ball milling tank for 50m L% by stirring, stirring at a stirring speed of 20min, placing the ball milling powder into a 20% by stirring machine, placing the ball milling machine for 2h, placing the ball milling powder into a 50-20 min, placing the ball milling machine for 50 h, placing the ball milling machine for 50m of 20min, placing the ball milling machine for 50 min, placing the ball milling machine for 50 h, placing the ball milling machine for drying, placing the ball milling machine for 50 min, placing the ball milling machine for 50 h, placing the ball milling machine for 50 min, placing the baking furnace for 50 min, placing the ball milling machine for.
The prepared light refractory material and the Zibo Zichuan Xinhua refractory material are detected, and the concrete detection is as follows:
(1) measurement of surface elasticity
Vertically placing a die steel needle with the diameter =1.5mm right above the sample, enabling the needle point to face downwards, supporting the bottom of the needle by a thumb, pressing downwards by natural force, measuring the depth of the inserted sample by a vernier caliper, and visually judging the surface elasticity of the sample according to the depth.
(2) Determination of apparent Density
And (3) putting the demoulded sample into an oven at 120 ℃, drying to constant weight, and cooling to room temperature for later use. And (4) grinding the prepared three test pieces respectively, weighing the test pieces, and accurately measuring the test pieces to lg. And sequentially measuring the length and the width of the test piece at the position 20 mm away from the edges and the middle position of the two ends of the test piece by using a steel plate ruler, wherein the length and the width are accurate to lm m, and taking the average value of 3 measurement data. The thickness was measured with a vernier caliper at the 20 mm and middle position from the edge at either end of the specimen and the measurement was repeated on the opposite side to an accuracy of 0.lmm. And taking the average value of 6 measurement data to obtain the mass and the volume of each test piece. The dry density is calculated as follows:
ρ=m /v
in the formula:
rho-dry density/g/cm3M mass/g, v volume/cm of test piece3。
The arithmetic mean of the dry densities of the three test pieces was calculated and the specific test results are shown in table 1.
TABLE 1 characterization of light refractory Properties
As can be seen from Table 1, the light refractory material prepared by the method greatly improves the fire resistance and mechanical strength of the material, and meanwhile, the material has low density. In the process of preparing the light refractory material, the prepared stirring slurry is frozen at low temperature and then dried and sintered, the method can reduce energy consumption to a certain extent, and the method can increase the aperture ratio of the prepared material and reduce the density of the material.
Claims (5)
1. A preparation method of a light refractory material is characterized by comprising the following specific preparation steps:
(1) adding 10-20 g of polyvinylpyrrolidone, 8-16 g of absolute ethyl alcohol, 20-30 g of deionized water and 40-50 g of styrene into a three-neck flask, introducing nitrogen, adjusting the temperature, and stirring to obtain a stirring solution;
(2) preparing divinylbenzene, absolute ethyl alcohol and deionized water into a mixed solution according to the mass ratio of 1:1:3, dropwise adding the mixed solution into a three-neck flask, and filtering after reaction to obtain polystyrene microspheres;
(3) ball-milling 50-60 g of bauxite and 5-6 g of mica to obtain ball-milled powder;
(4) placing the ball-milling powder and hydrogen peroxide in a beaker, and filtering after ultrasonic oscillation to obtain modified ball-milling powder;
(5) pouring polystyrene microspheres, 50m L ethanol, 50m L deionized water and 5m L surfactant into a beaker, stirring, adding ball-milling powder and 40-50 m L sulfuric acid solution, stirring, filtering, repeatedly washing with deionized water, and naturally drying to obtain aluminum oxide hollow microspheres;
(6) placing hollow alumina microspheres, 10-20 g of aluminum silicate, 5-8 g of dispersing agent, 15-20 g of perlite and 40-50 g of deionized water in a beaker, stirring at a rotating speed of 120-150 r/min for 20-30 min, filling the prepared stirring slurry into a block-shaped mold under the pressure of 30-40 MPa, placing the mold in a freezer at-10 to-5 ℃ for 20-24 h, then placing the mold in a freeze dryer, and freeze-drying at-40 to-50 ℃ to obtain a cured material;
(7) and sintering the solidified material in a sintering furnace to obtain the light refractory material.
2. The preparation method of the light refractory material according to claim 1, wherein the nitrogen gas is introduced at a speed of 30-40 m L in the step (1).
3. The method for preparing a lightweight refractory according to claim 1, wherein the dropping speed of the mixed solution in the step (2) is 10m L/min.
4. The method for preparing a lightweight refractory according to claim 1, wherein: the sulfuric acid solution in the step (5) is 25 percent.
5. The method for preparing a lightweight refractory according to claim 1, wherein: the sintering temperature in the step (7) is 600-800 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370136A (en) * | 1999-06-07 | 2002-09-18 | 联合矿物产品公司 | Lightweight dry refractory |
| CN1886350A (en) * | 2003-11-28 | 2006-12-27 | 新型材料莱布尼兹研究所公益性有限责任公司 | Insulation material |
| CN102811973A (en) * | 2010-07-13 | 2012-12-05 | 三井金属矿业株式会社 | Heat insulating refractory and method for producing same |
| CN107021776A (en) * | 2016-01-29 | 2017-08-08 | 阔斯泰公司 | Unsetting refractory body particle |
-
2017
- 2017-09-16 CN CN201710835812.1A patent/CN107540355B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370136A (en) * | 1999-06-07 | 2002-09-18 | 联合矿物产品公司 | Lightweight dry refractory |
| CN1886350A (en) * | 2003-11-28 | 2006-12-27 | 新型材料莱布尼兹研究所公益性有限责任公司 | Insulation material |
| CN102811973A (en) * | 2010-07-13 | 2012-12-05 | 三井金属矿业株式会社 | Heat insulating refractory and method for producing same |
| CN107021776A (en) * | 2016-01-29 | 2017-08-08 | 阔斯泰公司 | Unsetting refractory body particle |
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