KR100353520B1 - A Manufacturing method of porous composite particles in dry planetary ball milling of quartz powders - Google Patents

Abstract

The present invention is a method for preparing a functional inorganic filler using silica, and prepared a high functional porous composite particles by dry grinding method using a planetary mill, a kind of high energy mill, this method is a porous catalyst carrier in various catalyst industries In addition to performing the role smoothly, it is to prepare a material that can improve the flowability and mixing properties when used with various fillers.

In the present invention, the high-energy planetary mill type was used as the grinding machine, and the porous composite particles were produced by performing dry grinding by adjusting the loading amount of the grinding media ball, adjusting the sample filling rate, and controlling the grinding time.

Description

A manufacturing method of porous composite particles in dry planetary ball milling of quartz powders}

The present invention relates to the development of resource technology as part of the high purity of non-metallic minerals and the value-added improvement, and more specifically, by controlling the particle quality according to the interpulverization characteristics according to the surface activity increase using dry planetary mill of silica It relates to the production of the resulting porous composite particles.

In general, in order to make porous silica using silica, porous silica which gives porosity in the process of synthesizing silica is currently used in various fields of the industry. In particular, the catalyst carrier should have a high specific surface area and pore volume, and it is an inorganic carrier that plays an important role in determining the performance of the catalyst because it serves to stably disperse the active site of the catalyst to increase the activity of the catalyst.

In the production of the porous carrier, the synthesis method has a problem in that a lot of processes and time are required to make a large amount of energy consumption and resynthesis through pretreatment, melting, and the like for high purity of raw materials.

The present invention has been made in order to solve the above problems, the object of which is to purify the middle and lower grade quartz, which is infinitely buried in the country by physical screening and pulverization without supply of heat source from the outside using high energy type planetary mill In the process to control the surface properties of the pulverized product to produce a composite of high functional porous silica, it is to provide a manufacturing method by a single batch process.

In addition, the mechanochemistry effect, which is the core of the present invention, is conventionally not recognized in the manufacture of powder fine particles by mechanical grinding, which is an essential step for high value-adding inorganic materials and using metal / nonmetallic materials as industrial raw materials. It is to create a composite particle by utilizing the poor powder physical property change.

In terms of technology development, by utilizing the surface activity characteristics of materials, which are mechanical and chemical effects, on the physical properties of various powder products such as resource utilization, mineral treatment, metals, materials, etc., supplying heat sources from the outside for energy saving and eco-friendly, high value-added production Without this, it is possible to simplify the process by improving the reaction efficiency in the process.

In addition, when using a dry high-energy planetary mill, higher energy than the conventional mill is added to increase the surface activity of the powder particles, thereby rapidly increasing the change in the mechanical and chemical properties of the particles. In this process, the pulverized particles are pulverized to small nanometer size particles depending on the pulverization conditions. According to this production mechanism, each of the crushed particles is represented as a sintering connection phenomenon between the crushed particles in a state in which no heat source is supplied from the outside, and is used as a support for supporting a high functional catalyst because it forms a porous composite particle by supporting each of them. This is possible.

The present invention is achieved by providing a porous multiparticulate product using a dry planetary mill of silica due to appropriate combination of modulators of the planetary mill used to achieve the above object.

1 is a manufacturing flow chart for manufacturing the present invention

2 is an exemplary view showing a planetary dense structure of the present invention

Figure 3 is a magnified view of the porous composite particles produced by the present invention under a microscope

4 is a photograph showing the interior of the resulting composite particles of FIG.

5 is an exemplary view showing an embodiment according to the present invention.

Hereinafter, the configuration and operation of the present invention with reference to the accompanying drawings.

Figure 1 shows the manufacturing flow chart for manufacturing the present invention, by grinding and heavy chain by using a jaw crusher and a roll crusher of the silica ore as a general crushing machine to collect the silica powder through the particle size separation and to control the purity of the collected product In order to produce a high-purity refined silica powder by performing specific gravity and magnetic screening, as a raw product of dry planetary mill, grinding is performed by planetary mill to produce porous composite particles as shown in FIGS. 3 and 4.

In order to prepare porous composite particles, raw composite products are prepared by adjusting the size and loading of ball median balls, controlling the sample filling rate, and controlling the grinding time, for each catalyst carrier and industrial filler.

Various inorganic raw materials in the industrial application of grinding are subjected to a processing step in the form of fine powder. The preparation method of the fine powder is roughly divided into a wet process using a medium as a solvent and a dry process using no inorganic material or a medium. However, the wet process consumes a lot of time and energy for post-treatment such as dehydration and filtration after grinding.

In the present invention, the grinding method used a dry process at an economical efficiency, and prepared porous composite particles by controlling the surface properties of the particles during the grinding and mixing process. This is because the ore of the low and medium grade silica is made into a sample that is highly purified through a mineral treatment process and is suitable for use as a high functional filler. The high-energy planetary mill used in the present invention adjusts the revolving speed of the mill body, adjusts the size and filling amount of the ball media, and adjusts the sample filling rate and grinding time to dry the pulverized silica sample for the purpose. Generated.

Figure 2 shows an exemplary view showing the structure of the planetary mill of the present invention, the planetary mill is a high-energy mill based on the centrifugal force as the main action of the grinding, the production of the porous composite particle product using the same has not yet been carried out The present invention is the first process to produce porous composite particles to be used in the fine chemicals and catalyst industry using planetary mills to improve the added value of non-metallic minerals.

When modeling the porous composite particles according to the present invention with reference to Figure 5, look at the arbitrary contact particle group as follows.

Looking at one particle in the fluid particle group, the main particle receives the force of impact contact from surrounding contact particles. Thus, if it is possible to know from time to time the contact force received from the surrounding particles, the motion of the main particles can be represented by Newton's equation of motion. The impact force between particles that are continuously acting activates the surface of the particles, so that the surface of the particles is mechanochemistry and the porous composite particles are formed by the sintered necking of the particles without supply of heat source from the outside. Will generate

Mechanochemistry in pulverization does not only mean that the solid is subdivided, but some energy in the pulverization process accumulates energy in the particles themselves in addition to the energy for producing the pulverized product. This not only reduces the size of the sample particles but also disrupts the crystal structure of the particles. Since the disturbance of the crystal structure directly affects the activity of the particles, it is very important to understand the change, and these change factors appear during the grinding process.

This accumulated energy produces energy-saving and environmentally friendly treatment effects by expressing phenomena that are very important when applying secondary processes throughout the industry such as resource utilization, mineral processing, metals, chemicals, and materials. Here, in general, the pulverization machine acting by the crushing force by gravity generates less than about 2% crushing efficiency, the planetary mill used in this study is the centrifugal force is added to the grinding efficiency of the ball mill with the crushing force by the general gravity It is a high energy efficient grinding machine. Using such a high-energy planetary mill, the porous composite particles for each application by controlling the idle speed of the mill body, the size and filling of the ball media, the sample filling rate, and the grinding time by dry grinding the silica sample Was generated.

An embodiment according to the present invention will be described.

Example 1

The smaller the sample filling rate in the limited container, the faster the particle size decreases as the amount of grinding energy per unit time increases. However, if the sample is overcharged, the space in which the particles and the ball in the mill can move is limited, so the grinding efficiency is low. If the sample is too small, the wear of the ball media is severe. Therefore, in the present invention, the sample filling rate was set to 0.3 to 1.5.

Example 2

As the filling rate of the ball increases in a limited container, the number of impacts increases, so the grinding efficiency increases. However, since the ball filling rate has the milling machine rotational speed as a dependent variable in the case of the ball mill, the maximum grinding effect depends on the change of the rotational speed. That is, when the filling amount of the ball is small, the grinding speed increases as the mill rotation speed (rpm) increases, but in the case of the ball mill, the maximum grinding effect is obtained at the filling ratio of 0.45. However, in the case of planetary mill, the rotational speed does not become a dependent variable of the filling amount because the ball movement is more complicated than the ball mill. Therefore, in this invention, the ball filling rate was set to 0.3-0.7.

Example 3

The size of the ball is an important influence on the final particle size. The smaller the ball size, the smaller the final particle size tends to be. However, if the size of the ball is small, since the collision energy between the particles and the ball is small, the grinding force of the initial feed may be extremely small, so that the appropriate grinding force may not be applied. That is, there is a disadvantage that the initial grinding time takes a long time. This means that the particle size of the final multiparticulate product is also related to the size of the grinding balls. Therefore, in the present invention, the size of the final composite particles by adjusting the size of the ball can be prepared according to the use.

Example 4

In the case of ball mill, there is a critical rotational speed to generate cateracting motion by gravity. However, in the case of planetary mills, the grinding force mixed with the centrifugal force was found to be caused. do.

Therefore, in the present invention, when the distance (r1) of the central axis and the container is more than twice the rotation radius of the container (r2), it is considered that the efficiency is gradually increased in the production of the composite particles. In the present invention, all the regions after the generation of the composite particles generated after the crushing limit point during the generation of the composite particles according to the conditions of each setting element are to be set as the time control elements.

The present invention is not limited to the above-described specific preferred embodiments, and various modifications can be made by any person having ordinary skill in the art without departing from the gist of the present invention claimed in the claims. Of course, such changes will fall within the scope of the claims.

The present invention is a very useful invention that can improve the added value of the non-metallic minerals by producing a porous composite particle product using a high-energy planetary mill, and can be pulverized without supplying a heat source from the outside to save energy sources will be.

Claims (2)

The crude ore is crushed and heavy chained using a jaw crusher and a roll crusher to collect the product through particle size separation, and in order to control the purity of the collected product, specific gravity and magnetic screening are performed to calculate high purity refined silica and dry oil type. A method for producing porous composite particles using a dry oily mill of silica, characterized in that grinding is carried out by a high energy planetary mill as a raw material of wheat. The method of claim 1, In performing grinding by planetary mill, sample filling rate is set to 0.3 ~ 1.5, ball filling rate is set to 0.3 ~ 0.7, and the size of the ball can be converted into a range that can be converted according to each use of the produced composite particles. The grinding speed is set to the distance between the central axis and the container is more than twice the radius of the rotation, and the grinding time is expressed by the mechanochemical effect acting from below the grinding limit point of particle size Method for producing porous composite particles using a dry oil mill of silica, characterized in that the production of products for the use of.