CN112457006A - Preparation process of zirconium silicate ball filler - Google Patents

Preparation process of zirconium silicate ball filler Download PDF

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Publication number
CN112457006A
CN112457006A CN202011512804.1A CN202011512804A CN112457006A CN 112457006 A CN112457006 A CN 112457006A CN 202011512804 A CN202011512804 A CN 202011512804A CN 112457006 A CN112457006 A CN 112457006A
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zirconium silicate
mixture
meshes
ball filler
silicate ball
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鲁新辉
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Changsha Xinguang Special Ceramic Co ltd
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Changsha Xinguang Special Ceramic Co ltd
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Abstract

The invention discloses a preparation process of a zirconium silicate ball filler, which comprises the following steps: step 1: adding zircon sand, alumina powder, fluxing agent and charcoal powder into the aqueous solution to mix to form a mixture; step 2: introducing argon into the hearth for atmosphere protection, gradually adding the mixture into the hearth, and heating the mixture to a molten state; forming a molten mixture; and step 3: pouring out the mixture in a molten state from the hearth, blowing the molten mixture flowing out from a launder of the hearth by using compressed air, blowing the molten mixture into balls, cooling, solidifying and preserving heat to obtain the zirconium silicate ball filler with different granularities. The zirconium silicate ball filler has the compression strength of more than 30MPa, acid corrosion resistance, strong impact toughness and micron-sized through apparent porosity of 25-40 percent, and is suitable for chemical industry, water treatment filtration and inorganic salt adsorption.

Description

Preparation process of zirconium silicate ball filler
Technical Field
The invention relates to the field of chemical industry, in particular to a preparation process of a zirconium silicate ball filler.
Background
Alumina packing balls are commonly used in the chemical industry, and have the advantages of wear resistance and corrosion resistance, but the alumina has low impact toughness, so that the alumina packing balls are easy to crack in transportation and feeding operation, the service life of the packing is shortened, and the adsorption effect of the packing is influenced.
Therefore, there is an urgent need to develop an inorganic ceramic ball with good fluidity, wear resistance, corrosion resistance, and sufficient porosity and good comprehensive properties.
Disclosure of Invention
In view of the above, the present invention provides a preparation process of a zirconium silicate ball filler, which can be used for adsorption filtration of catalyst carriers and impurities.
In one aspect, the invention provides a preparation process of a zirconium silicate ball filler, which comprises the following steps:
step 1: adding zircon sand, alumina powder, fluxing agent and charcoal powder into the aqueous solution to mix to form a mixture;
step 2: introducing argon into the hearth for atmosphere protection, gradually adding the mixture into the hearth, and heating the mixture to a molten state; forming a molten mixture;
and step 3: pouring out the mixture in a molten state from the hearth, blowing the molten mixture flowing out from a launder of the hearth by using compressed air, blowing the molten mixture into balls, cooling, solidifying and preserving heat to obtain the zirconium silicate ball filler with different granularities.
Further, step 1 specifically includes: 75-80 parts of zircon sand, 5-8 parts of alumina powder, 1-3 parts of fluxing agent, 2-3 parts of deionized water and 10-20 parts of charcoal powder are mixed to form a mixture.
Further, step 3 specifically includes: collecting the cooled and solidified spherulites, and putting the spherulites into a tube furnace to preserve heat for 5 hours at 900 ℃; and after cooling, screening and grading the spherulites by using a vibrating screen to obtain zirconium silicate ball fillers with different particle sizes.
Further, zircon sand main component: the zirconia content is 55-65%, the SiO2 content is 30-35%, the Fe2O3 content is less than 0.02%, the Na2O content is less than 0.1%, the TiO2 content is less than 0.02%, and the particle size is 200-325 meshes.
Further, the alumina powder has the main components: the content of alumina is more than 99 percent, the content of Na2O is less than 0.1 percent, the content of Fe2O3 is less than 0.02 percent, the content of MgO is less than 0.1 percent, and the granularity is 200-325 meshes.
Furthermore, the fluxing agent is one or a combination of more of ammonium fluoride, boric acid, borax and aluminum fluoride.
Further, in step 3, the pressure of compressed air injection is 0.3-0.8MPa, and the injection angle is 30-60 ℃.
Further, in the step 3, a furnace tube of the tube furnace is made of high-purity corundum, air or oxygen is introduced during heating, and the flow rate is 50-200 mL/min.
Further, in step 3, the mesh number of the vibrating screen includes 40 mesh, 60 mesh, 80 mesh, 120 mesh, 200 mesh, 250 mesh, and 325 mesh.
Aiming at the defect of poor impact toughness of the traditional alumina ceramic filler ball, the invention combines the advantages of strong toughness and high density of zirconium silicate and the requirement of improving the adsorption and filtration effect in chemical reaction, and adopts a method of combining a fusion injection ball forming process and a pore-forming agent adding process to prepare the porous zirconium silicate ball filler, and has the following characteristics:
1. the pores in the zirconium silicate balls are micron-sized through pores, have the apparent porosity of 25-40 percent, and have better adsorption and filtration effects on large-particle iron rust sediment impurities.
2. The relative density of the parts of the zirconium silicate ball except the through holes reaches more than 98 percent, so that the zirconium silicate ball still has higher strength and toughness on the basis of keeping the porous structure.
3. The sphericity of the prepared porous zirconium silicate ball is higher than 0.8% by adopting a fusion jet balling process.
4. The filler balls can be screened into different particle size distributions. The particle size is adjustable from 40-60 microns to 1.5-2 mm.
5. The zirconium silicate ball produced by the preparation process has the compression strength of more than 30MPa, acid corrosion resistance (insolubility in hydrochloric acid and sulfuric acid), strong impact toughness (the fragmentation rate of free fall from 1m is less than 0.5 percent), and micron-sized through apparent porosity of 25-40 percent, and is suitable for chemical industry, water treatment filtration and inorganic salt adsorption.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
The invention preferably selects the following preparation process examples of zirconium silicate ball fillers, which are as follows:
example 1:
firstly, 75-80 parts of zircon sand (the zirconia content in the zircon sand is 65% and the granularity is 325 meshes), 5-8 parts of alumina powder (the MgO content is 0.08% and the granularity is 325 meshes), 1 part of fluxing agent (the fluxing agent is boric acid and the purity is more than 99%), 3 parts of deionized water and 10 parts of charcoal powder (the charcoal powder is needle-crumbed coal-like charcoal and the granularity is 325 meshes) are mixed in a V-shaped mixer for 2 hours (the rotating speed of the V-shaped mixer is 30 rpm) and poured out. Introducing Ar gas into the electric arc furnace for atmosphere protection, gradually adding the mixture into a three-phase alternating current electric arc furnace, and continuously heating the mixture to a molten state by starting an arc through a graphite electrode. After the mixture is completely added and the melting and refining are completed, pouring the hearth, blowing the molten mixture flowing out from the launder by using compressed air (the pressure of the compressed air is 0.7MPa, and the blowing angle is 30 ℃) at the water outlet of the hearth, and blowing the molten zirconium silicate microspheres into balls. The cooled and solidified pellets are collected and placed into a corundum tube furnace to be kept at 900 ℃ for 5 hours (oxygen is introduced, and the oxygen flow is 60 mL/min). After cooling, the spherulites are screened and classified by a vibrating screen (40 meshes, 60 meshes, 80 meshes, 120 meshes, 200 meshes, 250 meshes and 325 meshes), and are sorted by a vibrating spherical sorting machine to obtain the porous electrofused zirconium silicate ball fillers with different particle sizes.
Example 2:
firstly, 75-80 parts of zircon sand (the zirconia content in the zircon sand is 65% and the granularity is 325 meshes), 5-8 parts of alumina powder (the MgO content is 0.08% and the granularity is 325 meshes), 1 part of fluxing agent (the fluxing agent is boric acid and the purity is more than 99%), 3 parts of deionized water and 15 parts of charcoal powder (the charcoal powder is needle-crumbed coal-like charcoal and the granularity is 325 meshes) are mixed in a V-shaped mixer for 2 hours (the rotating speed of the V-shaped mixer is 30 rpm) and poured out. Introducing Ar gas into the electric arc furnace for atmosphere protection, gradually adding the mixture into a three-phase alternating current electric arc furnace, and continuously heating the mixture to a molten state by starting an arc through a graphite electrode. After the mixture is completely added and the melting and refining are completed, pouring the hearth, blowing the melted mixture flowing out of the launder by using compressed air (the pressure of the compressed air is 0.7MPa, and the blowing angle is 30 ℃) at the water outlet of the hearth, and blowing the melted zirconium silicate microspheres into balls. The cooled and solidified pellets are collected and placed into a corundum tube furnace to be kept at 900 ℃ for 5 hours (oxygen is introduced, and the oxygen flow is 60 mL/min). After cooling, the spherulites are screened and classified by a vibrating screen (40 meshes, 60 meshes, 80 meshes, 120 meshes, 200 meshes, 250 meshes and 325 meshes), and are sorted by a vibrating spherical sorting machine to obtain the porous electrofused zirconium silicate ball fillers with different particle sizes.
Example 3:
firstly, 75-80 parts of zircon sand (the zirconia content in the zircon sand is 65% and the granularity is 325 meshes), 5-8 parts of alumina powder (the MgO content is 0.08% and the granularity is 325 meshes), 1 part of fluxing agent (the fluxing agent is boric acid and the purity is more than 99%), 3 parts of deionized water and 20 parts of charcoal powder (the charcoal powder is needle-crumbed coal and the granularity is 325 meshes) are mixed in a V-shaped mixer for 2 hours (the rotating speed of the V-shaped mixer is 30 rpm) and poured out. Introducing Ar gas into the electric arc furnace for atmosphere protection, gradually adding the mixture into a three-phase alternating current electric arc furnace, and continuously heating the mixture to a molten state by starting an arc through a graphite electrode. After the mixture is completely added and the melting and refining are completed, pouring the hearth, blowing the melted mixture flowing out of the launder by using compressed air (the pressure of the compressed air is 0.7MPa, and the blowing angle is 30 ℃) at the water outlet of the hearth, and blowing the melted zirconium silicate microspheres into balls. The cooled and solidified pellets are collected and placed into a corundum tube furnace to be kept at 900 ℃ for 5 hours (oxygen is introduced, and the oxygen flow is 60 mL/min). After cooling, the spherulites are screened and classified by a vibrating screen (40 meshes, 60 meshes, 80 meshes, 120 meshes, 200 meshes, 250 meshes and 325 meshes), and are sorted by a vibrating spherical sorting machine to obtain the porous electrofused zirconium silicate ball fillers with different particle sizes.
The electrofused zirconium silicate ball filler is taken, a spherical porous zirconium silicate sample between 40-60 meshes of screens is selected for detection, the impact toughness (1 m high free fall fragmentation rate) is detected, the apparent porosity of the sample is tested by an Archimedes drainage method, the crushing strength (stress required by uniform speed drop test at a drop rate of 0.5 mm/min) is tested by a universal material testing machine, and the average pore diameter of the sample is tested by a mercury intrusion tester (AUTOPORE 9500).
Examples Charcoal content (%) Percent fracture (%) Apparent porosity (%) Crush load (N/grain) Average pore diameter (micron)
Example-1 10% 0.25% 19.65% 189 12.3
Example-2 15% 0.32% 26.87% 135 17.7
Example 3 20% 0.48% 38.25% 120 22.5
As can be seen from the above table, when the content of the added charcoal is 20%, the obtained apparent porosity can reach the maximum, and the fracture rate can still be kept below 0.5%, and the sample has good comprehensive properties such as crushing strength and pore size.
The techniques not described above are common general knowledge of the skilled person. All numbers less than or greater than the stated ranges are inclusive. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1. The preparation process of the zirconium silicate ball filler is characterized by comprising the following steps of:
step 1: adding zircon sand, alumina powder, fluxing agent and charcoal powder into the aqueous solution to mix to form a mixture;
step 2: introducing argon into the hearth for atmosphere protection, gradually adding the mixture into the hearth, and heating the mixture to a molten state; forming a molten mixture;
and step 3: pouring out the mixture in a molten state from the hearth, blowing the molten mixture flowing out from a launder of the hearth by using compressed air, blowing the molten mixture into balls, cooling, solidifying and preserving heat to obtain the zirconium silicate ball filler with different granularities.
2. The preparation process of the zirconium silicate ball filler according to claim 1, wherein the step 1 specifically comprises: 75-80 parts of zircon sand, 5-8 parts of alumina powder, 1-3 parts of fluxing agent, 2-3 parts of deionized water and 10-20 parts of charcoal powder are mixed to form a mixture.
3. The preparation process of the zirconium silicate ball filler according to claim 1, wherein the step 3 specifically comprises: collecting the cooled and solidified spherulites, and putting the spherulites into a tube furnace to preserve heat for 5 hours at 900 ℃; and after cooling, screening and grading the spherulites by using a vibrating screen to obtain zirconium silicate ball fillers with different particle sizes.
4. The process for preparing a zirconium silicate ball filler according to claim 1, wherein the zircon sand mainly comprises: the zirconia content is 55-65%, the SiO2 content is 30-35%, the Fe2O3 content is less than 0.02%, the Na2O content is less than 0.1%, the TiO2 content is less than 0.02%, and the particle size is 200-325 meshes.
5. The process for preparing a zirconium silicate ball filler according to claim 1, wherein the alumina powder comprises the following main components: the content of alumina is more than 99 percent, the content of Na2O is less than 0.1 percent, the content of Fe2O3 is less than 0.02 percent, the content of MgO is less than 0.1 percent, and the granularity is 200-325 meshes.
6. The preparation process of the zirconium silicate ball filler according to claim 1, wherein the fluxing agent is one or a combination of ammonium fluoride, boric acid, borax and aluminum fluoride.
7. The process for preparing a zirconium silicate ball filler according to claim 1, wherein in step 3, compressed air is blown at a pressure of 0.3 to 0.8MPa and a blowing angle of 30 to 60 ℃.
8. The preparation process of the zirconium silicate ball filler according to claim 3, wherein in the step 3, a furnace tube of the tube furnace is made of high-purity corundum, and air or oxygen is introduced during heating, wherein the flow rate is 50-200 mL/min.
9. The process for preparing a zirconium silicate ball filler according to claim 3, wherein in step 3, the number of meshes of the vibrating screen is 40 meshes, 60 meshes, 80 meshes, 120 meshes, 200 meshes, 250 meshes or 325 meshes.
CN202011512804.1A 2020-12-20 2020-12-20 Preparation process of zirconium silicate ball filler Pending CN112457006A (en)

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