CN111495513B - Grinding aid for dry grinding of active alpha-alumina micropowder and application thereof - Google Patents

Grinding aid for dry grinding of active alpha-alumina micropowder and application thereof Download PDF

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CN111495513B
CN111495513B CN202010175254.2A CN202010175254A CN111495513B CN 111495513 B CN111495513 B CN 111495513B CN 202010175254 A CN202010175254 A CN 202010175254A CN 111495513 B CN111495513 B CN 111495513B
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grinding
alumina
grinding aid
propylene glycol
light
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CN111495513A (en
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张举
张兰银
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Suzhou Shengmante New Material Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/06—Selection or use of additives to aid disintegrating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18—Details
    • B02C17/20—Disintegrating members
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron

Abstract

The invention discloses a grinding aid for grinding active alpha-alumina micropowder by a dry method, wherein the grinding aid is a composite grinding aid prepared from propylene glycol and light-burned magnesia powder according to a mass ratio of 0.01-0.25: 0.01-0.1. The invention also discloses a method for preparing the active alpha-alumina micropowder by dry grinding, which comprises the following steps: the grinding aid is mixed with calcined alumina raw powder for grinding. According to the invention, a small amount of composite grinding aid is added in the dry grinding of the active alpha-alumina micropowder, so that compared with the method without the grinding aid or by using propylene glycol or light-burned magnesium oxide, the grinding time of the active alumina micropowder can be greatly shortened by 5-30%, the energy consumption is greatly reduced, and the method has a good industrial application value. Meanwhile, the light-burned magnesia is uniformly distributed in the alpha-alumina micro powder, and can inhibit the growth of alumina crystals in the high-temperature sintering process.

Description

Grinding aid for dry grinding of active alpha-alumina micropowder and application thereof
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to a grinding aid for grinding active alpha-alumina micropowder by a dry method, and application of the grinding aid in the production of the active alpha-alumina micropowder in the fields of refractory materials and ceramics.
Background
Grinding aids are additives that increase grinding efficiency, are generally surface active substances, and have the effect of reducing specific surface energy and "wedging" into particle cracks. In the process of fine grinding of the material, the particles are gradually thinned, the specific surface area is increased, the surfaces of the particles are charged due to bond breakage, the particles are mutually adsorbed and agglomerated, and the grinding efficiency is reduced. A small amount of grinding aid is added, so that the agglomeration of particles can be prevented, the material fluidity is improved, the ball milling efficiency is improved, and the grinding time is shortened.
At present, the production of alumina micropowder generally adopts a dry ball milling process, and only depends on mechanical grinding between grinding balls and alumina under the condition of no grinding aid. The dry ball milling process has the advantages of low grinding efficiency and high energy consumption. Meanwhile, due to the problem of grinding efficiency, insufficient grinding sometimes occurs, and aggregates of calcined alumina cannot be completely opened, so that the technical problems of water addition amount increase, fluidity reduction and the like occur in the later use process of the refractory castable. Some production enterprises also use for reference the grinding in the cement industry, and common alcohol grinding aids such as methanol, ethanol and the like are introduced in the grinding process, so that although certain grinding efficiency can be improved properly, the effect is still not very obvious.
Disclosure of Invention
The inventor carries out research comparison on the basis of a great amount of experiments and practices to find that: in the grinding process of calcining the alumina micropowder, the grinding efficiency can be greatly improved and the grinding energy consumption can be obviously reduced by adopting the propylene glycol and light-burned magnesia powder composite grinding aid.
The purpose of the invention is realized by the following technical scheme:
a grinding aid for grinding active alpha-alumina micropowder by a dry method is a composite grinding aid prepared from propylene glycol and light-burned magnesia powder according to a mass ratio of 0.01-0.25: 0.01-0.1.
Preferably, the mass ratio of the propylene glycol to the light-burned magnesia powder is 0.05-0.1: 0.04-0.06.
The index requirements of the grinding aid of the invention are shown in Table 1:
table 1: index requirements for grinding aids
Raw materials Chemical purity (%) Particle size Appearance of the product
Propylene glycol ≥95 Finer than 50 meshes Powder or granules
Light-burned magnesium oxide ≥96 Finer than 1000 meshes Powder of
The propylene glycol is selected from 1, 2-propylene glycol and 1, 3-propylene glycol.
The invention also aims to provide application of the grinding aid in preparing active alpha-alumina micropowder by dry grinding.
A method for preparing active alpha-alumina micropowder by dry grinding comprises the following steps: the grinding aid is mixed with calcined alumina raw powder for grinding.
The method for preparing the active alpha-alumina micropowder by dry grinding comprises the following steps:
weighing and mixing calcined alumina raw powder, propylene glycol and light-burned magnesia powder according to the mass ratio of 100: 0.01-0.25: 0.01-0.1 to prepare a mixture;
and (2) pouring the mixture into a ball mill for mechanical grinding.
In the step (1), the mass ratio of the calcined alumina raw powder to the propylene glycol to the light-burned magnesia powder is 100: 0.05-0.1: 0.04-0.06.
In the step (2), the mass ratio of the total amount of the alumina raw powder, the propylene glycol and the light-burned magnesia powder to the grinding balls is 1: 5.
The invention has the beneficial effects that:
the grinding aid has the advantages of wide raw material source, low cost and no influence on the performance of the product.
According to the invention, a small amount of composite grinding aid is added in the dry grinding of the active alpha-alumina micropowder, so that compared with the method without the grinding aid or by using propylene glycol or light-burned magnesium oxide, the grinding time of the active alumina micropowder can be greatly shortened by 5-30%, the energy consumption is greatly reduced, and the method has a good industrial application value.
According to the invention, a small amount of propylene glycol is added into the active alpha-alumina micro powder ground by the dry method, the propylene glycol hardly influences the ground product, and the product volatilizes at high temperature. The light-burned magnesia is uniformly distributed in the alpha-alumina micro powder, can inhibit the growth of alumina crystals in the high-temperature sintering process, and is beneficial to maintaining the volume stability of functional ceramic sintering.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
Calcined alumina raw powder (primary crystal size D)501.8 μm) with 1, 2-propylene glycol (96.5%, 65 mesh, small granules) and light-burned magnesia powder (97.8%, 1200 mesh) in a mass ratio of 100:0.05:0.04, and the mixture was poured into a ball mill for grinding, the mass ratio of the grinding balls to the mixture being 5: 1. And (3) taking the ethanol grinding aid with equal mass and without the grinding aid as a comparative example, and testing the comparative grinding effect.
The results obtained for the milling protocol of this example are shown in table 2.
TABLE 2
Figure BDA0002410603460000021
Figure BDA0002410603460000031
As can be seen from Table 2, by adopting the composite grinding aid of the embodiment, compared with the scheme without the grinding aid, the grinding time is shortened by 0.9 hour, compared with the traditional ethanol grinding aid, the grinding time is shortened by 0.6 hour, the effect of the composite grinding aid is obviously better than that of a single grinding aid, and the grinding time of the activated alumina is obviously improved.
Comparing the crystal size condition of the alumina product ground by the composite grinding aid and the single propylene glycol grinding aid after sintering at 1650 ℃, and specifically operating: introducing 2% deionized water into the alumina powder, mixing, tabletting with a press (50MP pressure, standing for 30 s), drying at 110 deg.C, sintering at 1650 deg.C for 5 hr, naturally cooling, and polishing the ceramic surface
TABLE 3
Propylene glycol grinding aid Propylene glycol and light-burned magnesia powder
Crystal size distribution of alumina after 1650 ℃ firing 3～25μm 3～15μm
As can be seen from Table 3, in the high-temperature sintering process, the alumina product obtained by grinding with the grinding aid of the embodiment can effectively inhibit the growth of alumina crystals, and is beneficial to maintaining the volume stability of functional ceramic sintering.
Example 2
Calcined alumina raw powder (primary crystal size D)501.8 μm) was mixed with 1, 2-propanediol (same as in example 1) and soft-burned magnesia powder (same as in example 1) at a mass ratio of 100:0.07:0.04, and the mixture was poured into a ball mill and ground at a mass ratio of 5: 1. And (3) taking the ethanol grinding aid with equal mass and without the grinding aid as a comparative example, and testing the comparative grinding effect.
The results obtained for the milling protocol of this example are shown in table 4.
TABLE 4
Figure BDA0002410603460000032
As can be seen from Table 4, by adopting the composite grinding aid of the embodiment, compared with the scheme without the grinding aid, the grinding time is shortened by 1.1 hours, compared with the traditional ethanol grinding aid, the grinding time is shortened by 0.8 hour, the effect of the composite grinding aid is obviously better than that of a single grinding aid, and the grinding time of the activated alumina is obviously improved.
Example 3
Calcined alumina raw powder (primary crystal size D) 501.8 μm) was mixed with 1, 2-propylene glycol (same as example 1) and soft-burned magnesia powder (same as example 1) in a mass ratio of 100:0.07:0.06, and the mixture was poured into a ball mill for grinding, wherein the mass ratio of grinding balls to mixture was 5:1, and a comparative grinding effect was tested by using a grinding aid not added and an ethanol grinding aid of equal mass as comparative examples.
The results obtained for the milling protocol of this example are shown in table 5.
TABLE 5
Figure BDA0002410603460000041
As can be seen from Table 5, by adopting the composite grinding aid of the embodiment, compared with the scheme without the grinding aid, the grinding time is shortened by 1.4 hours, compared with the traditional ethanol grinding aid, the grinding time is shortened by 1.1 hours, the effect of the composite grinding aid is obviously better than that of a single grinding aid, and the grinding time of the activated alumina is obviously improved.

Claims (5)

1. A grinding aid for grinding active alpha-alumina micropowder by a dry method is characterized in that the grinding aid is a composite grinding aid prepared from propylene glycol and light-burned magnesia powder according to a mass ratio of 0.01-0.25: 0.01-0.1;
the index requirements for propylene glycol are: the chemical purity is more than or equal to 95 percent, the granularity is smaller than 50 meshes, and the appearance is powder or small particles;
index requirements of light-burned magnesium oxide: the chemical purity is more than or equal to 96 percent, the granularity is smaller than 1000 meshes, and the appearance is powder.
2. The grinding aid for dry grinding of the active alpha-alumina micropowder according to claim 1, characterized in that the mass ratio of the propylene glycol to the light-burned magnesia powder is 0.05-0.1: 0.04-0.06.
3. A method for preparing active alpha-alumina micropowder by dry grinding, which is characterized in that the grinding aid of claim 1 or 2 is mixed with calcined alumina raw powder for grinding.
4. The method for preparing active alpha-alumina micropowder by dry milling according to claim 3, characterized by comprising the steps of:
weighing and mixing calcined alumina raw powder, propylene glycol and light-burned magnesia powder according to the mass ratio of 100: 0.01-0.25: 0.01-0.1 to prepare a mixture;
and (2) pouring the mixture into a ball mill for mechanical grinding.
5. The method for preparing active alpha-alumina micropowder by dry grinding according to claim 4, wherein in the step (1), the mass ratio of the calcined alumina raw powder, the propylene glycol and the light-burned magnesia powder is 100: 0.05-0.1: 0.04-0.06.
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CN113045298B (en) * 2021-03-24 2022-12-13 苏州盛曼特新材料有限公司 Alumina-based coagulant for refractory castable and preparation method and application thereof
TWI760226B (en) * 2021-05-19 2022-04-01 釔銪鑫應用材料有限公司 Treatment method of metal oxide slag
CN114988885A (en) * 2022-05-25 2022-09-02 河南机电职业学院 Alumina ceramic powder slurry and preparation method thereof
CN117164345B (en) * 2023-09-05 2024-02-13 山东磐石刚玉有限公司 Low-cost preparation method of sintered microcrystalline corundum sand raw material

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CN104446390A (en) * 2014-11-26 2015-03-25 江苏晶鑫新材料股份有限公司 Preparation method for magnetism-containing modified corundum composite material
CN105294138A (en) * 2015-12-08 2016-02-03 武汉科技大学 Doublet aluminum oxide micropowder and preparation method thereof
CN105502450A (en) * 2015-12-25 2016-04-20 山东恒嘉高纯耐火原料股份有限公司 Preparing method and application of subspheroidal alpha-alumina micro powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104108923A (en) * 2014-05-19 2014-10-22 江苏新时高温材料有限公司 Active calcined alumina micro-powder and processing technology thereof
CN104446390A (en) * 2014-11-26 2015-03-25 江苏晶鑫新材料股份有限公司 Preparation method for magnetism-containing modified corundum composite material
CN105294138A (en) * 2015-12-08 2016-02-03 武汉科技大学 Doublet aluminum oxide micropowder and preparation method thereof
CN105502450A (en) * 2015-12-25 2016-04-20 山东恒嘉高纯耐火原料股份有限公司 Preparing method and application of subspheroidal alpha-alumina micro powder

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