CN115650716A - Preparation method of permanent magnetic ferrite wet-pressing magnetic shoe - Google Patents

Preparation method of permanent magnetic ferrite wet-pressing magnetic shoe Download PDF

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CN115650716A
CN115650716A CN202211363715.4A CN202211363715A CN115650716A CN 115650716 A CN115650716 A CN 115650716A CN 202211363715 A CN202211363715 A CN 202211363715A CN 115650716 A CN115650716 A CN 115650716A
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ball milling
magnetic shoe
slurry
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朱永宁
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Sinomag Technology Co ltd
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The invention discloses a preparation method of a permanent magnetic ferrite wet-pressing magnetic shoe, which comprises the following steps of carrying out primary ball milling on raw materials to obtain primary slurry, then filtering and drying the primary slurry to obtain a material, firing the material, and cooling to room temperature to obtain a primary sintered material; crushing the obtained primary sintering material and then sieving; adding a composite additive into the sieved primary sintered material for secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material; the method comprises the steps of carrying out wet pressing forming on the obtained filter material, firing the sample obtained by wet pressing forming to obtain a secondary sintering material sample, and carrying out coarse grinding processing on the secondary sintering material sample to obtain the magnetic shoe.

Description

Preparation method of permanent magnetic ferrite wet-pressing magnetic shoe
Technical Field
The invention relates to the technical field of magnetic shoe manufacturing, in particular to a preparation method of a permanent magnetic ferrite wet-pressing magnetic shoe.
Background
Chinese patent CN114105626B discloses a preparation method of a wet-pressing magnetic tile, which comprises the following specific preparation processes: adding the raw materials into a ball mill for ball milling, filtering and drying, firing the dried materials in a muffle furnace, cooling to room temperature, crushing the obtained primary sintered material, passing through a sieve, adding the crushed material into the ball mill, adding a composite additive into the ball mill, performing secondary ball milling, filtering the obtained secondary slurry, performing wet pressing and molding, and sintering in the muffle furnace to obtain a magnetic shoe;
the permanent magnetic ferrite wet pressing magnetic shoe adopts wet pressing mode magnetic field forming, and drainage in the forming process becomes a key factor for determining the quality of the magnetic shoe blank. There are many factors that affect the "drainage," with the size and consistency of the slurry size having a significant effect on drainage. At present, the grinding slurry in China is generally ground by a single steel ball or two steel balls in a mixing way, the slurry prepared by the method is difficult to drain, and the forming can only ensure sufficient drainage by prolonging the pressing time, so that the forming pressing period is long and the production efficiency is low.
Disclosure of Invention
The invention aims to solve the problems of the background technology and provides a preparation method of a permanent magnetic ferrite wet-pressing magnetic shoe.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a permanent magnetic ferrite wet-pressing magnetic shoe comprises the following steps:
step 1: performing primary ball milling on the raw materials to obtain primary slurry, filtering and drying the primary slurry to obtain a material, firing the material, and cooling to room temperature to obtain a primary sintering material;
step 2: crushing the primary sintered material obtained in the step 1 and then sieving;
and step 3: adding the primary sintered material sieved in the step 2 into a composite additive for secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material;
wherein, the steel ball of the secondary ball milling selects bearing steel balls with phi 9.5mm, phi 6.35mm and phi 4.8mm, and the adding proportion of the bearing steel balls with phi 9.5mm, phi 6.35mm and phi 4.8mm of the secondary ball milling is as follows: 1: (1.5-1.8): (1.2-1.5);
and 4, step 4: and (3) carrying out wet pressing forming on the filter material obtained in the step (3), then firing the sample obtained by the wet pressing forming to obtain a secondary sintered material sample, and then carrying out coarse grinding processing on the secondary sintered material sample to obtain the magnetic shoe.
As a further scheme of the invention: in step 1, the raw materials include ferric oxide and strontium carbonate.
As a further scheme of the invention: the molar ratio of ferric oxide to strontium carbonate is 5.8-6.0:1; the purity of ferric oxide is controlled to be more than 97%, and the purity of strontium carbonate is controlled to be more than 98%.
As a further scheme of the invention: in the step 1, the ball milling time is 1-3h, the firing temperature is 1280-1300 ℃, and the firing time is 1-3h.
As a further scheme of the invention: in step 2, a 60-200 target standard sample sieve is adopted for sieving.
As a further scheme of the invention: in the step 3, the secondary ball milling time is 13h.
As a further scheme of the invention: in step 3, the water content of the filter material is controlled to be 32-35%.
As a further scheme of the invention: in step 3, the raw materials and the composite additive are mixed according to the mass ratio of 91.
As a further scheme of the invention: in step 3, secondary ball grinding: ball: water =1:6-12:1.5-2.5; the rotating speed of the ball mill is controlled to be 90-100 r/min during the secondary ball milling.
As a further scheme of the invention: in the step 4, the sintering temperature is 1190-1250 ℃, and the sintering time is 1-3h.
The invention has the beneficial effects that:
according to the invention, through different proportions of grinding media (steel balls and water), the particle size distribution of the slurry is optimized on the premise of the same average particle size, the grinding efficiency is improved, the slurry which is more beneficial to forming is prepared, the forming efficiency is improved, and the product percent of pass is improved, so that the problems that the single steel ball or two steel balls are commonly adopted for grinding the grinding slurry in China at present and the slurry prepared by the method is difficult to drain, and the forming can only ensure sufficient drainage by prolonging the pressing time, so that the forming pressing period is long, and the production efficiency is low are solved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The invention relates to a preparation method of a permanent magnetic ferrite wet-pressing magnetic shoe, which comprises the following steps:
step 1: performing primary ball milling on the raw materials to obtain primary slurry, filtering and drying the primary slurry to obtain a material, firing the material, and cooling to room temperature to obtain a primary sintering material;
specifically, mixing ferric oxide and strontium carbonate, adding the mixture into a ball mill, carrying out ball milling for 1h, filtering and drying, firing the dried material in a muffle furnace at 1280 ℃ for 1h, and cooling to room temperature to obtain a primary sintered material;
wherein the molar ratio of ferric oxide to strontium carbonate is 5.8:1; the purity of ferric oxide is controlled to be more than 97%, and the purity of strontium carbonate is controlled to be more than 98%;
step 2: crushing the primary sintered material obtained in the step 1 and then sieving;
specifically, the obtained primary sintering material is crushed and then screened by a 60-target standard sample sieve;
and step 3: adding the primary sintered material sieved in the step 2 into a composite additive for secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material;
specifically, adding the primary sintered material crushed in the step 2 into a ball mill, adding a composite additive into the ball mill, performing secondary ball milling for 13 hours, and filtering the obtained secondary slurry to keep the water content of the filter material at 32-35%;
wherein, the raw materials and the composite additive are mixed according to the mass ratio of 91;
the steel balls for the secondary ball milling are selected from bearing steel balls with phi 9.5mm, phi 6.35mm and phi 4.8mm, and the addition proportion of the bearing steel balls with phi 9.5mm, phi 6.35mm and phi 4.8mm for the secondary ball milling is as follows: 1:1.5:1.2;
and secondary ball grinding: ball: water =1:6:1.5; the rotating speed of the ball mill is controlled at 90 revolutions per minute during secondary ball milling;
the composite additive comprises the following components in parts by weight: 0.31 part of aluminum oxide, 0.42 part of calcium carbonate, 0.53 part of boric acid, 0.15 part of cobaltosic oxide, 0.28 part of silicon dioxide and 0.26 part of modified dispersant; wherein the modified dispersant is branched polyacrylic acid ammonium chloride; performing secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material;
and 4, step 4: wet-pressing and molding the filter material obtained in the step 3, then firing a sample obtained by wet-pressing and molding to obtain a secondary sintered material sample, and then carrying out coarse grinding processing on the secondary sintered material sample to obtain the magnetic shoe;
specifically, the filter material prepared in the step 3 is subjected to wet pressing forming, then a formed sample is sintered for 1 hour at the temperature of 1190 ℃ in a roller kiln, and then the obtained sample is subjected to grinding processing to obtain the magnetic tile.
Example 2
The invention relates to a preparation method of a permanent magnetic ferrite wet-pressing magnetic shoe, which comprises the following steps:
step 1: performing primary ball milling on the raw materials to obtain primary slurry, filtering and drying the primary slurry to obtain a material, firing the material, and cooling to room temperature to obtain a primary sintering material;
specifically, mixing ferric oxide and strontium carbonate, adding the mixture into a ball mill, carrying out ball milling for 2 hours, filtering and drying, firing the dried material in a muffle furnace at 1290 ℃ for 2 hours, and cooling to room temperature to obtain a primary sintering material;
wherein the molar ratio of the ferric oxide to the strontium carbonate is 5.9:1; the purity of ferric oxide is controlled to be more than 97%, and the purity of strontium carbonate is controlled to be more than 98%;
step 2: crushing the primary sintering material obtained in the step 1 and then sieving;
specifically, the obtained primary sintering material is crushed and then screened by a 130-target standard sample sieve;
and step 3: adding the primary sintered material sieved in the step 2 into a composite additive for secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material;
specifically, adding the primary sintered material crushed in the step 2 into a ball mill, adding a composite additive into the ball mill, performing secondary ball milling for 13 hours, and filtering the obtained secondary slurry to keep the water content of the filter material at 32-35%;
wherein, the raw materials and the composite additive are mixed according to the mass ratio of 91;
the steel balls for the secondary ball milling are bearing steel balls with the diameters of phi 9.5mm, phi 6.35mm and phi 4.8mm, and the steel balls for the secondary ball milling are bearing steel balls with the diameters of phi 9.5mm, phi 6.35mm and phi 4.8mm in the following proportion: 1:1.7:1.3;
and secondary ball grinding: ball: water =1:9:2.0; the rotating speed of the ball mill is controlled to be 90-100 r/min during secondary ball milling;
the composite additive comprises the following components in parts by weight: 0.32 part of aluminum oxide, 0.45 part of calcium carbonate, 0.56 part of boric acid, 0.155 part of cobaltosic oxide, 0.30 part of silicon dioxide and 0.30 part of modified dispersant; wherein the modified dispersant is branched polyacrylic acid ammonium chloride; performing secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material;
and 4, step 4: wet-pressing and molding the filter material obtained in the step 3, then firing a sample obtained by wet-pressing and molding to obtain a secondary sintered material sample, and then carrying out coarse grinding processing on the secondary sintered material sample to obtain the magnetic shoe;
specifically, the filter material prepared in the step 3 is subjected to wet pressing forming, then a formed sample is sintered for 2 hours in a roller kiln at the temperature of 1210 ℃, and then the obtained sample is subjected to grinding processing to obtain the magnetic tile.
Example 3
The invention relates to a preparation method of a permanent magnetic ferrite wet-pressing magnetic shoe, which comprises the following steps:
step 1: performing primary ball milling on the raw materials to obtain primary slurry, filtering and drying the primary slurry to obtain a material, firing the material, and cooling to room temperature to obtain a primary sintering material;
specifically, mixing ferric oxide and strontium carbonate, adding the mixture into a ball mill, carrying out ball milling for 3 hours, filtering and drying, firing the dried material in a muffle furnace at 1300 ℃ for 3 hours, and cooling to room temperature to obtain a primary sintering material;
wherein the molar ratio of the ferric oxide to the strontium carbonate is 6.0:1; the purity of ferric oxide is controlled to be more than 97%, and the purity of strontium carbonate is controlled to be more than 98%;
step 2: crushing the primary sintered material obtained in the step 1 and then sieving;
specifically, the obtained primary sintering material is crushed and then screened by a 200-target standard sample sieve;
and step 3: adding the primary sintered material sieved in the step 2 into a composite additive for secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material;
specifically, adding the crushed primary sintered material obtained in the step 2 into a ball mill, adding a composite additive into the ball mill, performing secondary ball milling for 13 hours, and filtering the obtained secondary slurry to keep the water content of the filter material at 32-35%;
wherein, the raw materials and the composite additive are mixed according to the mass ratio of 91;
the steel balls for the secondary ball milling are selected from bearing steel balls with phi 9.5mm, phi 6.35mm and phi 4.8mm, and the addition proportion of the bearing steel balls with phi 9.5mm, phi 6.35mm and phi 4.8mm for the secondary ball milling is as follows: 1:1.8:1.5;
and a secondary ball abrasive: ball: water =1:12:2.5; the rotating speed of the ball mill is controlled at 100 revolutions per minute during secondary ball milling;
the composite additive comprises the following components in parts by weight: 0.33 part of aluminum oxide, 0.47 part of calcium carbonate, 0.58 part of boric acid, 0.16 part of cobaltosic oxide, 0.33 part of silicon dioxide and 0.36 part of modified dispersant; wherein the modified dispersant is branched polyacrylic acid ammonium chloride; performing secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material;
and 4, step 4: wet-pressing and molding the filter material obtained in the step 3, then firing a sample obtained by wet-pressing and molding to obtain a secondary sintered material sample, and then carrying out coarse grinding processing on the secondary sintered material sample to obtain the magnetic shoe;
specifically, the filter material prepared in the step 3 is subjected to wet pressing forming, then a formed sample is sintered for 3 hours in a roller kiln at the temperature of 1250 ℃, and then the obtained sample is ground to obtain the magnetic shoe.
Comparative example 1
According to the method of the embodiment 1, the type of the steel ball is changed into a single steel ball with the diameter of 9.5mm, and the proportion of the material balls to the water is the same;
comparative example 1
According to the method of the embodiment 1, the type of the steel ball is changed into a single steel ball with the diameter of 6.35mm, and the proportion of the material balls to the water is the same;
comparative example 2
According to the method of the embodiment 1, the type of the steel ball is changed into a single steel ball with phi 4.8mm, and the proportion of the material balls to the water is the same;
comparative example 3
According to the method of the embodiment 1, the steel ball model is changed into a phi 6.35mm and phi 4.8mm combined steel ball, the proportion is 1:1, the proportion of the material balls to the water is the same.
Performance testing
The filter materials after the secondary ball milling of example 1 and comparative examples 1-3 were subjected to a particle size test, the test results of which are shown in the following table:
Figure BDA0003922957640000071
Figure BDA0003922957640000081
as can be seen from the above table, in the same ball milling time, the average particle size of the filter material after the secondary ball milling in example 1 is 0.85um, and the average particle size of the filter material after the secondary ball milling in comparative examples 1 to 4 is 0.88 to 1.05um, and the comparison shows that the diameter of the filter material generated after the ball milling of a single steel ball is larger than that of the filter material generated after the ball milling of two combined steel balls; in the embodiment 1, the diameter of the filter material generated after the ball milling of the three steel balls with different diameters is smaller than that of the filter material generated after the ball milling of the two combined steel balls; therefore, the invention optimizes the particle size distribution of the slurry on the premise of the same average particle size by different proportions of grinding media (steel balls and water), improves the grinding efficiency, prepares the slurry more favorable for forming, improves the forming efficiency and improves the product percent of pass, thereby effectively solving the problems that the prior domestic grinding slurry generally adopts single steel ball or two steel balls to mix and grind, the slurry prepared by the method is difficult to drain, the forming can only ensure sufficient drainage by prolonging the pressing time, and the forming pressing period is long and the production efficiency is low.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.

Claims (10)

1. A preparation method of a permanent magnetic ferrite wet-pressing magnetic shoe is characterized by comprising the following steps:
step 1: performing primary ball milling on the raw materials to obtain primary slurry, filtering and drying the primary slurry to obtain a material, firing the material, and cooling to room temperature to obtain a primary sintering material;
step 2: crushing the primary sintering material obtained in the step 1 and then sieving;
and step 3: adding the primary sintered material sieved in the step 2 into a composite additive for secondary ball milling to obtain secondary slurry, and filtering the secondary slurry to obtain a filter material;
wherein, the steel ball of the secondary ball milling selects bearing steel balls with phi 9.5mm, phi 6.35mm and phi 4.8mm, and the adding proportion of the bearing steel balls with phi 9.5mm, phi 6.35mm and phi 4.8mm of the secondary ball milling is as follows: 1: (1.5-1.8): (1.2-1.5);
and 4, step 4: and (3) carrying out wet pressing forming on the filter material obtained in the step (3), then firing the sample obtained by the wet pressing forming to obtain a secondary sintered material sample, and then carrying out coarse grinding processing on the secondary sintered material sample to obtain the magnetic shoe.
2. The method for preparing a permanent magnetic ferrite wet compression magnetic shoe as claimed in claim 1, wherein in step 1, the raw materials comprise ferric oxide and strontium carbonate.
3. The method for preparing a permanent magnetic ferrite wet-pressing magnetic shoe according to claim 2, characterized in that the molar ratio of ferric oxide to strontium carbonate is 5.8-6.0:1; the purity of ferric oxide is controlled to be more than 97%, and the purity of strontium carbonate is controlled to be more than 98%.
4. The method for preparing a permanent magnetic ferrite wet pressing magnetic shoe according to claim 3, characterized in that in step 1, the ball milling time is 1-3h, the firing temperature is 1280-1300 ℃, and the firing time is 1-3h.
5. The method for preparing a permanent magnetic ferrite wet pressing magnetic shoe as claimed in claim 1, wherein in step 2, a 60-200 target standard sample sieve is used for sieving.
6. The method for preparing a permanent magnetic ferrite wet pressing magnetic shoe according to claim 5, characterized in that in step 3, the secondary ball milling time is 13h.
7. The method for preparing a permanent magnetic ferrite wet pressing magnetic shoe as claimed in claim 6, characterized in that in step 3, the water content of the filter material is controlled at 32-35%.
8. The method for preparing a permanent magnetic ferrite wet pressing magnetic shoe according to claim 7, characterized in that in step 3, the raw materials and the composite additive are mixed according to the mass ratio of 91.
9. The method for preparing a permanent magnetic ferrite wet pressing magnetic shoe according to claim 8, wherein in step 3, the secondary ball grinding material: ball: water =1:6-12:1.5-2.5; the rotating speed of the ball mill is controlled to be 90-100 r/min during the secondary ball milling.
10. The method for preparing a permanent magnetic ferrite wet pressing magnetic shoe as claimed in claim 1, characterized in that in step 4, the sintering temperature is 1190-1250 ℃ and the sintering time is 1-3h.
CN202211363715.4A 2022-11-02 2022-11-02 Preparation method of permanent magnetic ferrite wet-pressing magnetic shoe Pending CN115650716A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05275227A (en) * 1992-03-27 1993-10-22 Nec Corp Manufacture of oxide magnetic material
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CN108101529A (en) * 2017-12-20 2018-06-01 横店集团东磁股份有限公司 A kind of production method for shrinking smaller permanent magnetic ferrite magnet
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05275227A (en) * 1992-03-27 1993-10-22 Nec Corp Manufacture of oxide magnetic material
CN101860091A (en) * 2010-04-26 2010-10-13 马鞍山市鑫洋永磁有限责任公司 Preparation method for rare earth permanent ferrite magnetic shoe and product
CN108101529A (en) * 2017-12-20 2018-06-01 横店集团东磁股份有限公司 A kind of production method for shrinking smaller permanent magnetic ferrite magnet
CN110372362A (en) * 2019-07-15 2019-10-25 横店集团东磁股份有限公司 A kind of preparation method and permanent-magnet ferrite material of permanent-magnet ferrite material
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