CN114620739B - Nanometer lamellar pyrophyllite powder and preparation method thereof - Google Patents
Nanometer lamellar pyrophyllite powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano lamellar pyrophyllite powder and a preparation method thereof, wherein pyrophyllite raw ore is used as a main raw material, water with a medium-low temperature structure is removed, then saturated adsorption is carried out on high-temperature expandable solution, then rapid freezing is carried out to cause expansion cracking of partial pyrophyllite lamellar, then rapid heat treatment within the range of 200-700 ℃ is carried out, water adsorbed in the pyrophyllite is rapidly vaporized, expandable solvent is rapidly expanded and decomposed to generate a large amount of gas, and the expansion cracking of the pyrophyllite lamellar structure is generated, so that the nano lamellar pyrophyllite is formed. In order to better obtain uniform nano lamellar pyrophyllite powder, the expanded pyrophyllite raw material is assisted to separate and strip by ultrasonic or ball mill, and the thickness of the obtained nano lamellar is about 50-500 nanometers. The nano lamellar pyrophyllite powder prepared by the invention has hot spots of large specific surface area, good activity and the like, and can be widely used in the industries of paint, plastics and catalysts.
Description
Technical Field
The invention relates to a preparation method of pyrophyllite powder, in particular to nano lamellar pyrophyllite powder and a preparation method thereof.
Background
The nano lamellar material not only can play a role in reinforcing and toughening in the material due to the special structure and size effect, but also can be used for compositely loading objects with optical, electric, magnetic, catalytic and other characteristics to obtain a composite material with excellent comprehensive performance, can be applied to various fields of aviation, aerospace, daily production of people and life, and is a hot spot for the current material science research.
Pyrophyllite [ Si ] 4 Al 2 O 10 (OH) 2 ]Is a typical water-containing layered aluminosilicate mineral, and has an aluminum hydroxide octahedral layer sandwiched between two silica layersThe tetrahedral layers form a 2:1 layered structure, and can be widely applied to the fields of ceramics, paint, plastics, rubber, pressure medium, refractory materials, water pollution treatment and the like. At present, compared with the foreign fields, the pyrophyllite industrial application in China has a considerable gap, and mainly shows two aspects: the first is that the application area is narrow. And secondly, the application grade is lower. The pyrophyllite ore has a considerable amount of outlets every year in China, but almost all the pyrophyllite ore is raw ore, and deep processing products such as various filler grades, coating grades and the like still cannot reach the ideal mature products such as light calcium, titanium white and the like due to the granularity, whiteness and reinforcing effect, so that the production is not scaled up to date. In a word, the phenomenon of extensive application exists in the current application of pyrophyllite mineral resources, the mineral price is low (about 300 yuan/ton of 325 mesh powder price), the additional value is low, the application range is limited, and the economic benefit is not obvious.
The pyrophyllite powder used in the current market is mainly obtained by mechanical ball milling and crushing, the granularity is of micron grade, and the processing equipment of the pyrophyllite powder product (generally, the product for glass fiber is smaller than 1250 meshes) for industrial application mainly depends on a Raymond mill and a grading system thereof; and the superfine grinding product is processed mainly by adopting an air flow grinder or a medium stirring mill and the like. But the method of mechanical ball milling only can hardly realize the mass production of nano-scale powder. At present, research on ultrafine pyrophyllite powder at home and abroad is mainly focused on crushing in mechanical or air flow ball milling and other modes, the granularity of the obtained powder is mainly focused on micron level, and part of nano-sheets obtained in the method can be distorted and agglomerated in the ball milling process, so that a series of excellent performances such as large specific surface area, reinforcement, toughening and the like of the nano-powder with a sheet structure cannot be achieved.
The invention provides a preparation method of nano lamellar pyrophyllite powder, which aims at the defects of the existing pyrophyllite powder raw materials. The nano lamellar pyrophyllite prepared by utilizing the structure of the pyrophyllite has an important effect on improving the usability of the pyrophyllite.
Disclosure of Invention
In order to solve the problems of narrow application field, common application performance and the like of the traditional pyrophyllite raw materials, the invention adopts middle-low temperature de-structured water, then carries out saturated adsorption on high-temperature expandable solution, then carries out quick freezing to cause the expansion of partial pyrophyllite sheet layers, then carries out quick heat treatment within the range of 200-700 ℃, and causes the water adsorbed in the pyrophyllite to be quickly vaporized and the expandable solvent to be quickly expanded and decomposed to generate a large amount of gas to cause the expansion and the expansion of the pyrophyllite sheet layer structure, thereby forming the nano-sheet pyrophyllite.
The invention aims at realizing the following technical scheme: the preparation method of the nano lamellar pyrophyllite powder comprises the following steps:
step 1: crushing a pyrophyllite raw material to a granularity below 1mm, and calcining at 600-700 ℃ for 0.5-2 hours to remove part of structural water in the pyrophyllite structure and generate part of pores in the pyrophyllite raw structure;
step 2: adding a high-temperature expandable solution into the calcined pyrophyllite raw material powder, and uniformly mixing the high-temperature expandable solution and the pyrophyllite raw material powder, wherein the mass ratio of the addition of the high-temperature expandable solution to the calcined pyrophyllite raw material powder is 5-20%;
step 3: placing the pyrophyllite raw material powder uniformly mixed in the step 2 into a vacuum-pumping container, and pumping vacuum for 30 minutes to enable the high-temperature expandable solution adsorbed on the surface of the pyrophyllite to be adsorbed into the interlayer and internal pores of the pyrophyllite; then aging the pyrophyllite raw material subjected to vacuum pumping in a container to enable the pyrophyllite raw material to reach full saturated adsorption;
step 4: freezing pyrophyllite raw material powder which is saturated and adsorbed with high-temperature expandable solution by liquid nitrogen, and rapidly freezing by utilizing water in the expandable solution to generate instant volume expansion so as to promote the expansion loosening or peeling of part of pyrophyllite lamellar structure;
step 5: the frozen pyrophyllite raw material powder is quickly added into a heat treatment furnace with the furnace temperature of 200-500 ℃ for expansion treatment, so that moisture in the pyrophyllite lamellar structure is quickly vaporized and removed, and high-temperature expandable substances are expanded and decomposed, so that the pyrophyllite lamellar structure is expanded, and nano lamellar pyrophyllite powder is obtained.
Further, the high-temperature expandable solution is prepared by mixing one or more of urea, dimethyl sulfoxide, starch, sucrose, ethylene glycol or glycerol according to any proportion.
Further, the mass ratio of the addition of the high-temperature expandable solution to the calcined pyrophyllite raw material powder is 5-20%.
Further, the optimized addition range of the high-temperature expandable solution is 10% -15%.
Further, in the step 2, the high-temperature expandable solution and pyrophyllite raw material powder are uniformly mixed by a mechanical stirring method.
Further, the frozen pyrophyllite raw material powder is quickly added into a heat treatment furnace with the furnace temperature of 200-500 ℃ for expansion treatment, and the heat treatment time is 1-30 minutes.
Further, part of the lamellar structure of the pyrophyllite powder obtained after the treatment in the steps 1-5 is in submicron and nanometer scale thickness, part of lamellar layers are in sliding, dislocation connection or agglomeration together, and mechanical ball milling or ultrasonic dispersion treatment is adopted to fully strip and disperse the nano lamellar layers, so that nano powder with uniform lamellar layers is better obtained.
On the other hand, the invention also provides nano lamellar pyrophyllite powder, and the lamellar thickness of the nano lamellar pyrophyllite powder is 50-500 nanometers.
The beneficial effects of the invention are as follows: the invention skillfully utilizes the expansion stripping thought, and utilizes partial free water or adsorbed water in the pyrophyllite structure and other substances capable of expanding at high temperature or low temperature to generate instant explosive volume expansion so as to strip pyrophyllite sheets to prepare nano-sheet pyrophyllite powder. The invention has the advantages of scientific and reasonable design, simple operation process, low production cost and easy mass production, and can reduce the agglomeration of superfine pyrophyllite powder particles, the prepared nano lamellar pyrophyllite powder has excellent dimensional benefit, and the powder has 100m 2 The specific surface area of about/g has the advantages of high activity and large specific surface area, and has good dispersibility and brushing performance when being applied to the paint. Can also be used as a carrier of materials such as biological medicines and the like, and has excellent adsorption and catalytic performances. Improved application in plastic and rubber productsBreaking strength and fracture toughness functions. The addition to the lubricating oil can improve the lubricating performance.
Drawings
FIG. 1 is an SEM photograph (2000 times) of the morphology of an initial pyrophyllite feedstock particle;
FIGS. 2, 3 and 4 are SEM photographs of nano-lamellar pyrophyllite powder prepared in example 1 at various magnifications (2000, 10000 and 2000);
fig. 5 and fig. 6 are SEM photographs of the morphology of nano lamellar pyrophyllite powder prepared in example 2 and example 3, respectively;
Detailed Description
The present invention will be described in further detail with reference to the following examples and drawings.
Example 1
The pyrophyllite raw ore is crushed to a grain size of 200 meshes to be used as a starting material, and then the pyrophyllite powder is placed in a heating furnace to be calcined at 600 ℃ for 2 hours and then taken out for standby. Adding water to prepare a high-temperature expandable solution (containing 25% of urea and 5% of water-soluble starch) with the mass concentration of 30%, adding the high-temperature expandable solution into the calcined pyrophyllite powder with the addition of 10% of the mass of the powder, and stirring for 15 minutes by using a stirrer to enable the high-temperature expandable solution to be fully mixed and contacted with the powder. And then placing the mixture in a vacuum device, vacuumizing for 30 minutes, discharging the gas in the pores of the pyrophyllite, and adsorbing the high-temperature expandable solution adsorbed on the surface of the pyrophyllite into the interlayer and internal pores of the pyrophyllite. And (3) vacuumizing, packaging the mixture with a container with a cover, standing and homogenizing for 24 hours, so that the pores and layers of pyrophyllite reach full saturated adsorption. The pyrophyllite raw material powder of saturated adsorption high-temperature expandable solution is filled into a metallic open container, then the container is placed into liquid nitrogen to quickly freeze the pyrophyllite raw material, and then the metallic container is placed into a heat treatment furnace at 500 ℃ by a shovel to be subjected to expansion heat treatment for 1 minute. Taking out the metal container after 1 minute, naturally cooling to room temperature, and taking out nano lamellar pyrophyllite powder. The nano lamellar pyrophyllite powder obtained after the expansion heat treatment has a part of lamellar structure still with the thickness of submicron or micron scale, and part of lamellar layers are connected in a sliding way or clustered together in a dislocation way, so that the nano lamellar layers are fully stripped and dispersed, and the nano lamellar pyrophyllite powder with uniform thickness is prepared by adopting a powder ball mill for ball milling for 1 hour. And (3) carrying out scanning electron microscope observation on the pyrophyllite original particles and the prepared powder particles, wherein the microscopic morphology of the pyrophyllite original particles is shown in fig. 1 and fig. 2-4. Fig. 1 shows morphology SEM pictures of the nano lamellar pyrophyllite powder prepared by starting denser pyrophyllite raw material particles under different magnification, and fig. 2-4 show that the thickness of a single lamellar is about 50 nanometers, partial lamellar is combined together, and the maximum lamellar thickness is about 500 nanometers.
Example 2
The pyrophyllite raw ore is crushed to 600 meshes of grain size to be used as a starting raw material, and then the pyrophyllite powder is placed in a heating furnace to be calcined at 700 ℃ for 0.5 hour and then taken out for standby. Adding water to prepare a high-temperature expandable solution (containing 5% of dimethyl sulfoxide and 5% of sucrose) with the mass concentration of 10%, adding the high-temperature expandable solution into the calcined pyrophyllite powder with the addition of 20% of the mass of the powder, and stirring for 15 minutes by using a stirrer to ensure that the high-temperature expandable solution and the powder are fully mixed and contacted. And then placing the mixture in a vacuum device, vacuumizing for 30 minutes, discharging the gas in the pores of the pyrophyllite, and adsorbing the high-temperature expandable solution adsorbed on the surface of the pyrophyllite into the interlayer and internal pores of the pyrophyllite. And (3) vacuumizing, packaging the mixture with a container with a cover, standing and homogenizing for 24 hours, so that the pores and layers of pyrophyllite reach full saturated adsorption. The pyrophyllite raw material powder saturated and adsorbed with the high-temperature expandable solution is filled into a metallic open container, then the container is placed in liquid nitrogen to rapidly freeze the pyrophyllite raw material, and then the metallic container is placed into a heat treatment furnace at 200 ℃ by a shovel to be subjected to expansion heat treatment for 30 minutes. Taking out the metal container after 30 minutes, naturally cooling to room temperature, and taking out nano lamellar pyrophyllite powder. The nano lamellar pyrophyllite powder obtained after the expansion heat treatment has a part of lamellar structure still in submicron or micron-scale thickness, and part of lamellar layers are in sliding connection or are clustered together, so that the nano lamellar layers are fully stripped and dispersed, and the pyrophyllite powder is added into a powder ball mill for ball milling for 1 hour, so that the nano lamellar pyrophyllite powder with uniform thickness is obtained. And (3) carrying out scanning electron microscope observation on the pyrophyllite original particles and the prepared powder particles, wherein the microscopic morphology is shown in figure 5, the thickness of a single lamellar layer is about 50 nanometers, part lamellar layers are combined together, and the maximum lamellar layer thickness is about 500 nanometers.
Example 3
The pyrophyllite raw ore is crushed to a grain size of 200 meshes to be used as a starting material, and then the pyrophyllite powder is placed in a heating furnace to be calcined at 650 ℃ for 1 hour and then taken out for standby. Adding water to prepare a high-temperature expandable solution (containing 25% of ethylene glycol, 10% of water-soluble starch and 15% of urea) with the mass concentration of 50%, adding the high-temperature expandable solution into the calcined pyrophyllite powder with the addition amount of 5% of the mass of the powder, and stirring for 10 minutes by using a stirrer to enable the high-temperature expandable solution to be fully mixed and contacted with the powder. And then placing the mixture in a vacuum device, vacuumizing for 30 minutes, discharging the gas in the pores of the pyrophyllite, and adsorbing the high-temperature expandable solution adsorbed on the surface of the pyrophyllite into the interlayer and internal pores of the pyrophyllite. And (3) vacuumizing, packaging the mixture with a container with a cover, standing and homogenizing for 24 hours, so that the pores and layers of pyrophyllite reach full saturated adsorption. The pyrophyllite raw material powder saturated and adsorbed with the high-temperature expandable solution is filled into a metallic open container, then the container is placed in liquid nitrogen to quickly freeze the pyrophyllite raw material, and then the metallic container is placed into a heat treatment furnace at 450 ℃ by a shovel to be subjected to expansion heat treatment for 10 minutes. Taking out the metal container after 10 minutes, naturally cooling to room temperature, and taking out nano lamellar pyrophyllite powder. The nano lamellar pyrophyllite powder obtained after the expansion heat treatment has a part of lamellar structure still with the thickness of submicron or micron scale, and part of lamellar layers are connected in a sliding way or clustered together in a staggered way, so that the nano lamellar layers are fully stripped and dispersed, and the nano lamellar pyrophyllite powder with uniform thickness is prepared by adopting a powder ball mill for ball milling for 1 hour. And (3) carrying out scanning electron microscope observation on the pyrophyllite original particles and the prepared powder particles, wherein the microscopic morphology is shown in figure 6, the thickness of a single lamellar layer is about 50 nanometers, part lamellar layers are combined together, and the maximum lamellar layer thickness is about 500 nanometers.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (5)
1. The preparation method of the nano lamellar pyrophyllite powder is characterized by comprising the following steps of:
step 1: crushing a pyrophyllite raw material to a granularity below 1mm, and calcining at 600-700 ℃ for 0.5-2 hours to remove part of structural water in the pyrophyllite structure and generate part of pores in the pyrophyllite raw structure;
step 2: adding a high-temperature expandable solution into the calcined pyrophyllite raw material powder, and uniformly mixing the high-temperature expandable solution and the pyrophyllite raw material powder, wherein the mass ratio of the addition of the high-temperature expandable solution to the calcined pyrophyllite raw material powder is 5-20%; the high-temperature expandable solution is prepared by mixing one or more of urea, dimethyl sulfoxide, starch, sucrose, ethylene glycol or glycerol according to any proportion;
step 3: placing the pyrophyllite raw material powder uniformly mixed in the step 2 into a vacuum-pumping container, and pumping vacuum for 30 minutes to enable the high-temperature expandable solution adsorbed on the surface of the pyrophyllite to be adsorbed into the interlayer and internal pores of the pyrophyllite; then aging the pyrophyllite raw material subjected to vacuum pumping in a container to enable the pyrophyllite raw material to reach full saturated adsorption;
step 4: freezing pyrophyllite raw material powder which is saturated and adsorbed with high-temperature expandable solution by liquid nitrogen, and rapidly freezing by utilizing water in the expandable solution to generate instant volume expansion so as to promote the expansion loosening or peeling of part of pyrophyllite lamellar structure;
step 5: rapidly adding the frozen pyrophyllite raw material powder into a heat treatment furnace with the furnace temperature of 200-500 ℃ for expansion treatment, so that moisture in the pyrophyllite lamellar structure is rapidly vaporized and removed, and high-temperature expandable substances are expanded and decomposed, thereby expanding the pyrophyllite lamellar structure and obtaining nano lamellar pyrophyllite powder;
step 6: and (3) the part of the lamellar structure of the pyrophyllite powder obtained after the treatment in the steps 1-5 is in submicron and nanoscale thickness, and part of lamellar layers are in sliding connection or are clustered together, so that the nano lamellar layers are fully peeled and dispersed, and mechanical ball milling or ultrasonic dispersion treatment is adopted, so that the nano powder with uniform lamellar layers is better obtained.
2. The method for preparing nano lamellar pyrophyllite powder according to claim 1, wherein the optimized addition amount interval of the high-temperature expandable solution is 10% -15%.
3. The method for preparing nano lamellar pyrophyllite powder according to claim 1, wherein the high-temperature expandable solution and the pyrophyllite raw material powder are uniformly mixed by a mechanical stirring method in the step 2.
4. The method for preparing nano lamellar pyrophyllite powder according to claim 1, wherein the frozen pyrophyllite raw material powder is rapidly added into a heat treatment furnace with the furnace temperature of 200-500 ℃ for expansion treatment, and the heat treatment time is 1-30 minutes.
5. A nano lamellar pyrophyllite powder prepared based on the preparation method of any one of claims 1-4, characterized in that the lamellar thickness of the nano lamellar pyrophyllite powder is 50-500 nm.
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