CN109678499A - A method of using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads - Google Patents
A method of using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads Download PDFInfo
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- CN109678499A CN109678499A CN201811645452.XA CN201811645452A CN109678499A CN 109678499 A CN109678499 A CN 109678499A CN 201811645452 A CN201811645452 A CN 201811645452A CN 109678499 A CN109678499 A CN 109678499A
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- clout
- zirconium silicate
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- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000011325 microbead Substances 0.000 title claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 90
- 239000000843 powder Substances 0.000 claims abstract description 80
- 239000002994 raw material Substances 0.000 claims abstract description 48
- 239000003595 mist Substances 0.000 claims abstract description 39
- 238000000465 moulding Methods 0.000 claims abstract description 34
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 238000005453 pelletization Methods 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 238000005498 polishing Methods 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 12
- 229920005610 lignin Polymers 0.000 claims abstract description 12
- 239000004615 ingredient Substances 0.000 claims abstract description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract 4
- 238000001035 drying Methods 0.000 claims abstract 3
- 238000004140 cleaning Methods 0.000 claims abstract 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 27
- 238000010792 warming Methods 0.000 claims description 19
- 238000005245 sintering Methods 0.000 claims description 18
- 229920003081 Povidone K 30 Polymers 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000009495 sugar coating Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 2
- 239000011859 microparticle Substances 0.000 claims 1
- 239000000047 product Substances 0.000 description 60
- 239000011265 semifinished product Substances 0.000 description 54
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 11
- 229910052726 zirconium Inorganic materials 0.000 description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 10
- 235000012239 silicon dioxide Nutrition 0.000 description 10
- 239000002270 dispersing agent Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 9
- 241001504664 Crossocheilus latius Species 0.000 description 8
- 238000007605 air drying Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000000227 grinding Methods 0.000 description 7
- 238000000462 isostatic pressing Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000007500 overflow downdraw method Methods 0.000 description 2
- 238000009700 powder processing Methods 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- UUNNUENETDBNPB-HKBOAZHASA-N (2s)-2-[[(2s,3r)-3-amino-2-hydroxy-4-(4-phenylmethoxyphenyl)butanoyl]amino]-4-methylpentanoic acid Chemical compound C1=CC(C[C@@H](N)[C@H](O)C(=O)N[C@@H](CC(C)C)C(O)=O)=CC=C1OCC1=CC=CC=C1 UUNNUENETDBNPB-HKBOAZHASA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/481—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing silicon, e.g. zircon
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The present invention relates to microballon preparation fields, it is especially a kind of using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, composition of raw materials is by mass percentage are as follows: prepares zirconium silicate micro mist clout 48%-88% of the D50 less than 7 μm abandoned during zirconium silicate Polishing Powder, prepare aluminium oxide powder clout 9%-49% of the D50 less than 7 μm abandoned during aluminum oxide Polishing Powder, lignin 3%；Preparation step are as follows: ingredient → dry-mixed → tide is mixed → ageing mixture → encryption compacting → broken → screening → pelletizing → moulding encrypts → choose shuttles → drying → screen → be sintered → selected → polishing → cleaning → drying；The microballon partial size prepared is 63-600 μm, density 3.8-4.0g/cm3, sphericity is greater than 95%.For the present invention using industrial clout, at low cost, product purpose is wide, simple process, is the innovation in terms of zirconium silicate compounded microbeads preparation method.
Description
Technical field
It is more specifically a kind of multiple using density high-strength multipurpose zirconium silicate in clout preparation the present invention relates to microballon preparation field
The method for closing microballon.
Technical background
The rapid development of superfine powder processing industry has driven the research and development and production of abrasive media.Develop high quality and
The high-quality abrasive media of high grinding efficiency can have positive contribution to powder processing industry, and create great economic benefit.It grinds
Mill pearl is a kind of important abrasive media, can be widely applied to cement, mineral, ceramics, electronic material, magnetic material and coating,
The grinding and processing of the industries raw material such as paint, are a kind of good abrasive medias.With superfine powder answering in various industries
With and development, fineness, grain shape and quality of powder etc. constrain science and technology development and productivity raising, in this case,
Hardness with higher, lesser abrasion, corrosion-resistant, resistance to oxidation and the high Zirconium silicate grinding integument of cost performance are more and more given birth to
Producer is produced to be used.
In industrial production, during preparing Polishing Powder using zirconium silicate or aluminum oxide, D50 is micro- less than 7 μm
Powder is abandoned generally as industrial clout, is unfavorable for energy-saving and emission-reduction.
The production technology of the existing zirconium silicate pearl as abrasive media is substantially high-temperature melting method and two kinds of sintering process.
The shortcomings that fusion method is defect easy to form and energy consumption is high, does not meet the national policy of energy-saving and emission-reduction.Zirconium silicate pearl is in high temperature
It is formed under molten condition, if a certain critical technical parameter is not controlled, prepared product will form defective fragile
Broken pearl, bubble pearl, tail pearl and flat pearl, yield rate are generally 60% or less.Sintering process prepares zirconium silicate pearl, ball green body
Molding is usually rolled, partial size is small, the high ball low with wearing valve of hardness the disadvantage is that being difficult to prepare；Isostatic pressing cost
High and partial size is big, acts on extra-fine grinding limited.
The application field of complex silicate zirconium pearl is extensive compared with zirconium oxide microballon, it is suitable for the dispersion and grinding of granular materials,
It is also widely used for polishing and surface sand-blasting process etc., the advantage for there are other abrasive materials incomparable.
Chinese patent CN101786867A discloses a kind of preparation method of zirconium silicate ball, using mist projection granulating, etc. it is quiet
Molded and high temperature sintering preparation method.Wherein use " isostatic pressing " technique, known in the industry, " isostatic pressing "
Ultra-fine micro mist can not be ground in the ball that diameter 3mm or more can only be produced at present, and the sphericity of microballon is poor, following process
Complexity, production efficiency is low, at high cost.
Chinese patent CN103664152B discloses a kind of Wear-resistant zirconium silicate medium ball and preparation method thereof, is first to make by spraying
Grain prepares bulb and the method for rolling sintering is recycled to prepare zirconium silicate media ball.It is told about for the 0024th section in the license text
" production that can be used in the Wear-resistant zirconium silicate medium ball that partial size is 0.5-10.0mm ", specifies the final of preparation method production
The zirconium silicate media ball that partial size is less than 0.5mm can not be made in the particle size range of product, this method.
In conclusion sintering process prepares zirconium silicate ball medium there are the following problems: 1. utilization not yet in effect in the prior art
The industrial clout abandoned after industrial production zirconium silicate or aluminum oxide Polishing Powder, high production cost；2. the silicic acid prepared
Zirconium pearl application range is small, can only be used as abrasive media mostly, and cost performance is low；3. product cut size is big, it is difficult to be ground and is less than
The microballon of 0.5mm；4. needing using " isostatic pressing " or " mist projection granulating " process, complex process；5. the density of finished product microballon is small,
Sphericity is poor；6. there are the pollution problems such as soda acid in preparation process.
Summary of the invention
The purpose of the present invention is to solve the deficiency of the prior art, a kind of of offer utilizes density high-strength in clout preparation
The method of multipurpose zirconium silicate compounded microbeads, adopts the following technical scheme that
A method of using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads, preparation process is as follows:
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate micro mist clout 48%- are carried out in proportion
88%, aluminium oxide powder clout 9%-49%, lignin 3%.
The zirconium silicate micro mist clout refers to prepare zirconium silicate Polishing Powder during, as industrial clout abandon
Micro mist of the D50 less than 7 μm is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent difference
It is 3%, 80%, 17%.
The aluminium oxide powder clout refers to prepare zirconium silicate Polishing Powder during, as industrial clout abandon
Micro mist of the D50 less than 7 μm, be made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent
Respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 1-3h in 3 D stereo batch mixer, is sufficiently mixed raw material
It is even.
(3) tide is mixed: mixing mixed in (2) being added to the deionized water of mass percent 7%, then in planetary wet stone roller
It is mixed that tide is carried out in machine.
(4) ageing mixture: the mixed raw material of tide in (3) is removed into planetary edge runner-wet mill, stands 48h.
(5) raw material being stranded in (4) encryption compacting: is pressed into strip and block, pressure 500-600MPa with press.
(6) it is crushed: the strip and block product in (5) is crushed with pulverizer, air-dry.
(7) it sieves: the material after air-drying in (6) is sieved, choose particle of the partial size no more than 75 μm and carry out (8)
Step, the particle greater than 75 μm return again to carry out (6) step.
(8) pelletizing: by the particle obtained in (7) no more than 75 μm as ball, D50 is less than 7 μm by mass percentage
Aluminium oxide powder clout 10%-50% of zirconium silicate micro mist clout 50%-90%, the D50 less than 7 μm ratio be added it is mixed
Close uniform industrial micro mist clout, add the deionized water of mass percent 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90,
The pelletizing in double dynamical strong granulating machine.
(9) moulding encrypts: by the sphere made in (8), in the formula sugar coating machine that topples, (operating angle can be between 0-180 °
Any adjustment) in moulding encryption, heated in moulding ciphering process, 70-85 DEG C of temperature, soaking time 2-3h, balling-up partial size
It is 63-600 μm.
(10) it chooses shuttles: semi-finished product obtained in (9) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(11) it dries: semi-finished product obtained in (10) is dried into 1-3h at 80-120 DEG C.
(12) it screens: semi-finished product obtained in (11) is sieved, the semi-finished product of partial size needed for choosing.
(13) it is sintered: semi-finished product obtained in (12) being sintered in kiln, sintering curve are as follows: with 60 in kiln
DEG C/speed of h from room temperature rises to 300 DEG C, 0.5h is kept the temperature, is then warming up to 1100 DEG C with the speed of 120 DEG C/h, then with 90 DEG C/h
Speed be warming up to 1400-1500 DEG C of heat preservation 2h, be cooled to room temperature, kiln discharge.
(14) selected, finished product obtained in (13) is carried out to selected, finished product of the selection sphericity greater than 95%.
(15) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (14), (partial size is not more than 20 to carbide fine powder
μm) be polished directly.
(16) it cleans, finished product obtained in (15) is cleaned with deionized water.
(17) it dries: finished product obtained in (16) is dried into 1-2h at 80-120 DEG C.
The present invention is different using the partial size of industrial clout, and mutual disperse in preparation process, gradation is reasonable, then is carried out with press
Compacting encryption, effectively improves its intensity and density, and using ball pelletizing, effect is good, and sphericity is high；Glycerol plays the role of moulding,
Conducive to raising sphericity；Be heated to 70-85 DEG C in moulding ciphering process, be conducive to drainage exhaust, increase semi-finished product density and
Sphericity；Using the methods of addition lignin, reticular structure is increased, toughness of products is improved.
The beneficial effects of the present invention are:
1. preparing silicic acid using the industrial clout after industrial production zirconium silicate Polishing Powder or aluminum oxide Polishing Powder
Zirconium compounded microbeads, production cost is 40% or so of normal fusion method, good in economic efficiency；
2. the zirconium silicate pearl prepared has wide range of applications, suitable for the dispersion and grinding of granular materials, other materials
Polishing and sandblasting etc., cost performance are high；
3. the minimum grain size of product reaches 63 μm, it is suitble to extra-fine grinding, the microballon less than 0.5mm can be ground；
4. not needed in preparation process using " isostatic pressing " and " mist projection granulating " process, simple process, production efficiency
It is high；
5. using " moulding encryption " process in production stage, finished product bead density is made to reach 3.8-4.0g/cm3, sphericity
Greater than 95%, industrial needs are met；
6. it is polluted in whole preparation process without soda acid etc., it is environmentally protective.
Detailed description of the invention:
Fig. 1 is the scanning electron microscopic picture for the zirconium silicate compounded microbeads that the present invention prepares.
Specific embodiment
Principles and features of the present invention are described with reference to embodiments, listed give an actual example is served only for explaining this hair
It is bright, not limit the scope of the invention.
Embodiment 1:
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate of the D50 less than 7 μm is micro- are carried out in proportion
Powder clout 60%, aluminium oxide powder clout 37% of the D50 less than 7 μm, lignin 3%；Wherein silicic acid of the D50 less than 7 μm
Zirconium micro mist clout is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%, aluminium oxide powder clout of 17%, the D50 less than 7 μm is by partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm
Powder composition, mass percent is respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 1.2h in 3 D stereo batch mixer, is sufficiently mixed raw material
It is even.
(3) tide is mixed: mixing mixed in (2) being added to the deionized water of mass percent 7%, then in planetary wet stone roller
It is mixed that tide is carried out in machine.
(4) ageing mixture: the mixed raw material of tide in (3) is removed into planetary edge runner-wet mill, stands 48h.
(5) raw material being stranded in (4) encryption compacting: is pressed into strip and block, pressure 540MPa with press.
(6) it is crushed: the strip and block product in (5) is crushed with pulverizer, air-dry.
(7) it sieves: the material after air-drying in (6) is sieved, choose particle of the partial size no more than 75 μm and carry out (8)
Step, the particle greater than 75 μm return again to carry out (6) step.
(8) pelletizing: by the particle obtained in (7) no more than 75 μm as ball, D50 is less than 7 μm by mass percentage
The ratio of the aluminium oxide powder clout 40% of zirconium silicate micro mist clout 60%, D50 less than 7 μm uniformly mixed work is added
Industry micro mist clout, add the deionized water of mass percent 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90, double dynamical strong
Pelletizing in power pelletizer.
(9) moulding encrypts: by the sphere made in (8), moulding is encrypted in the formula sugar coating machine that topples, in moulding ciphering process
It is heated, is kept for 80 DEG C of temperature, time 2h, balling-up partial size is 63-600 μm.
(10) it chooses shuttles: semi-finished product obtained in (9) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(11) it dries: semi-finished product obtained in (10) is dried into 2h at 100 DEG C.
(12) it screens: semi-finished product obtained in (11) being sieved, the semi-finished product of required partial size are obtained.
(13) it is sintered: semi-finished product obtained in (12) being sintered in kiln, sintering curve are as follows: with 60 in kiln
DEG C/speed of h from room temperature rises to 300 DEG C, 0.5h is kept the temperature, then 1100 DEG C are warming up to the speed of 120 DEG C/h, then again with 90
DEG C/speed of h is warming up to 1450 DEG C of heat preservation 2h, it is cooled to room temperature, kiln discharge.
(14) selected, finished product obtained in (13) is carried out to selected, finished product of the selection sphericity greater than 95%.
(15) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (14), (partial size is not more than 20 to carbide fine powder
μm) be polished directly.
(16) it cleans, finished product obtained in (15) is cleaned with deionized water.
(17) it dries: finished product obtained in (16) is dried into 1h at 120 DEG C.
Embodiment 2:
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate of the D50 less than 7 μm is micro- are carried out in proportion
Powder clout 70%, aluminium oxide powder clout 27% of the D50 less than 7 μm, lignin 3%；Wherein silicic acid of the D50 less than 7 μm
Zirconium micro mist clout is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%, aluminium oxide powder clout of 17%, the D50 less than 7 μm is by partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm
Powder composition, mass percent is respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 1.5h in 3 D stereo batch mixer, is sufficiently mixed raw material
It is even.
(3) tide is mixed: mixing mixed in (2) being added to the deionized water of mass percent 7%, then in planetary wet stone roller
It is mixed that tide is carried out in machine.
(4) ageing mixture: the mixed raw material of tide in (3) is removed into planetary edge runner-wet mill, stands 48h.
(5) raw material being stranded in (4) encryption compacting: is pressed into strip and block, pressure 540MPa with press.
(6) it is crushed: the strip and block product in (5) is crushed with pulverizer, air-dry.
(7) it sieves: the material after air-drying in (6) is sieved, choose particle of the partial size no more than 75 μm and carry out (8)
Step, the particle greater than 75 μm return again to carry out (6) step.
(8) pelletizing: by the particle obtained in (7) no more than 75 μm as ball, D50 is less than 7 μm by mass percentage
The ratio of the aluminium oxide powder clout 30% of zirconium silicate micro mist clout 70%, D50 less than 7 μm uniformly mixed work is added
Industry micro mist clout, add the deionized water of mass percent 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90, double dynamical strong
Pelletizing in power pelletizer.
(9) moulding encrypts: by the sphere made in (8), moulding is encrypted in the formula sugar coating machine that topples, in moulding ciphering process
It is heated, is kept for 75 DEG C of temperature, time 2.5h, balling-up partial size is 63-600 μm.
(10) it chooses shuttles: semi-finished product obtained in (9) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(11) it dries: semi-finished product obtained in (10) is dried into 1.8h at 105 DEG C.
(12) it screens: semi-finished product obtained in (11) being sieved, the semi-finished product of required partial size are obtained.
(13) it is sintered: semi-finished product obtained in (12) being sintered in kiln, sintering curve are as follows: with 60 in kiln
DEG C/speed of h from room temperature rises to 300 DEG C, 0.5h is kept the temperature, then 1100 DEG C are warming up to the speed of 120 DEG C/h, then again with 90
DEG C/speed of h is warming up to 1420 DEG C of heat preservation 2h, it is cooled to room temperature, kiln discharge.
(14) selected, finished product obtained in (13) is carried out to selected, finished product of the selection sphericity greater than 95%.
(15) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (14), (partial size is not more than 20 to carbide fine powder
μm) be polished directly.
(16) it cleans, finished product obtained in (15) is cleaned with deionized water.
(17) it dries: finished product obtained in (16) is dried into 1.2h at 100 DEG C.
Embodiment 3:
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate of the D50 less than 7 μm is micro- are carried out in proportion
Powder clout 81%, aluminium oxide powder clout 16% of the D50 less than 7 μm, lignin 3%；Wherein silicic acid of the D50 less than 7 μm
Zirconium micro mist clout is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%, aluminium oxide powder clout of 17%, the D50 less than 7 μm is by partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm
Powder composition, mass percent is respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 1.6h in 3 D stereo batch mixer, is sufficiently mixed raw material
It is even.
(3) tide is mixed: mixing mixed in (2) being added to the deionized water of mass percent 7%, then in planetary wet stone roller
It is mixed that tide is carried out in machine.
(4) ageing mixture: the mixed raw material of tide in (3) is removed into planetary edge runner-wet mill, stands 48h.
(5) raw material being stranded in (4) encryption compacting: is pressed into strip and block, pressure 550MPa with press.
(6) it is crushed: the strip and block product in (5) is crushed with pulverizer, air-dry.
(7) it sieves: the material after air-drying is sieved, choose particle of the partial size no more than 75 μm and carry out (8) step, greatly
Carry out (6) step is returned again in 75 μm of particles.
(8) pelletizing: by the particle obtained in (7) no more than 75 μm as ball, D50 is less than 7 μm by mass percentage
The ratio of the aluminium oxide powder clout 19% of zirconium silicate micro mist clout 81%, D50 less than 7 μm uniformly mixed work is added
Industry micro mist clout, add the deionized water of mass percent 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90, double dynamical strong
Pelletizing in power pelletizer.
(9) moulding encrypts: by the sphere made in (8), moulding is encrypted in the formula sugar coating machine that topples, in moulding ciphering process
It is heated, is kept for 80 DEG C of temperature, time 2.2h, balling-up partial size is 63-600 semi-finished product.
(10) it chooses shuttles: semi-finished product obtained in (9) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(11) it dries: semi-finished product obtained in (10) is dried into 2h at 105 DEG C.
(12) it screens: semi-finished product obtained in (11) being sieved, the semi-finished product of required partial size are obtained.
(13) it is sintered: semi-finished product obtained in (12) being sintered in kiln, sintering curve are as follows: with 60 in kiln
DEG C/speed of h from room temperature rises to 300 DEG C, 0.5h is kept the temperature, then 1100 DEG C are warming up to the speed of 120 DEG C/h, then again with 90
DEG C/speed of h is warming up to 1480 DEG C of heat preservation 2h, it is cooled to room temperature, kiln discharge.
(14) selected, finished product obtained in (13) is carried out to selected, finished product of the selection sphericity greater than 95%.
(15) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (14), (partial size is not more than 20 to carbide fine powder
μm) be polished directly.
(16) it cleans, finished product obtained in (15) is cleaned with deionized water.
(17) it dries: finished product obtained in (16) is dried into 1.5h at 105 DEG C.
Embodiment 4:
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate of the D50 less than 7 μm is micro- are carried out in proportion
Powder clout 65%, aluminium oxide powder clout 32% of the D50 less than 7 μm, lignin 3%；Wherein silicic acid of the D50 less than 7 μm
Zirconium micro mist clout is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%, aluminium oxide powder clout of 17%, the D50 less than 7 μm is by partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm
Powder composition, mass percent is respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 2.2h in 3 D stereo batch mixer, is uniformly mixed raw material.
(3) tide is mixed: mixing mixed in (2) being added to the deionized water of mass percent 7%, then in planetary wet stone roller
It is mixed that tide is carried out in machine.
(4) ageing mixture: the mixed raw material of tide in (3) is removed into planetary edge runner-wet mill, stands 48h.
(5) raw material being stranded in (4) encryption compacting: is pressed into strip and block, pressure 520MPa with press.
(6) it is crushed: the strip and block product in (5) is crushed with pulverizer, air-dry.
(7) it sieves: the material after air-drying in (6) is sieved, choose particle of the partial size no more than 75 μm and carry out (8)
Step, the particle greater than 75 μm return again to carry out (6) step.
(8) pelletizing: by the particle obtained in (7) no more than 75 μm as ball, D50 is less than 7 μm by mass percentage
The ratio of the aluminium oxide powder clout 35% of zirconium silicate micro mist clout 65%, D50 less than 7 μm uniformly mixed work is added
Industry micro mist clout, add the deionized water of mass percent 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90, double dynamical strong
Pelletizing in power pelletizer.
(9) moulding encrypt: will in (8) by the sphere made in the formula sugar coating machine that topples moulding encryption, moulding ciphering process
In heated, keep 75 DEG C of temperature, time 2.5h, balling-up partial size be 63-600 μm.
(10) it chooses shuttles: semi-finished product obtained in (9) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(11) it dries: semi-finished product obtained in (10) is dried into 2h at 108 DEG C.
(12) it screens: semi-finished product obtained in (11) being sieved, the semi-finished product of required partial size are obtained.
(13) it is sintered: semi-finished product obtained in (12) being sintered in kiln, sintering curve are as follows: with 60 in kiln
DEG C/speed of h from room temperature rises to 300 DEG C, 0.5h is kept the temperature, then 1100 DEG C are warming up to the speed of 120 DEG C/h, then again with 90
DEG C/speed of h is warming up to 1460 DEG C of heat preservation 2h, it is cooled to room temperature, kiln discharge.
(14) selected, finished product obtained in (13) is carried out to selected, finished product of the selection sphericity greater than 95%.
(15) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (14), (partial size is not more than 20 to carbide fine powder
μm) be polished directly.
(16) it cleans, finished product obtained in (15) is cleaned with deionized water.
(17) it dries: finished product obtained in (16) is dried into 1.8h at 110 DEG C.
Embodiment 5:
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate of the D50 less than 7 μm is micro- are carried out in proportion
Powder clout 75%, aluminium oxide powder clout 22% of the D50 less than 7 μm, lignin 3%；Wherein silicic acid of the D50 less than 7 μm
Zirconium micro mist clout is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%, aluminium oxide powder clout of 17%, the D50 less than 7 μm is by partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm
Powder composition, mass percent is respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 2.5h in 3 D stereo batch mixer, is sufficiently mixed raw material
It is even.
(3) tide is mixed: mixing mixed in (2) being added to the deionized water of mass percent 7%, then in planetary wet stone roller
It is mixed that tide is carried out in machine.
(4) ageing mixture: the mixed raw material of tide in (3) is removed into planetary edge runner-wet mill, stands 48h.
(5) raw material being stranded in (4) encryption compacting: is pressed into strip and block, pressure 580MPa with press.
(6) it is crushed: the strip and block product in (5) is crushed with pulverizer, air-dry.
(7) it sieves: the material after air-drying in (6) is sieved, choose particle of the partial size no more than 75 μm and carry out (8)
Step, the particle greater than 75 μm return again to carry out (6) step.
(8) pelletizing: by the particle obtained in (7) no more than 75 μm as ball, D50 is less than 7 μm by mass percentage
The ratio of the aluminium oxide powder clout 25% of zirconium silicate micro mist clout 75%, D50 less than 7 μm uniformly mixed work is added
Industry micro mist clout, add the deionized water of mass percent 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90, double dynamical strong
Pelletizing in power pelletizer.
(9) moulding encrypts: by the sphere made in (8), moulding is encrypted in the formula sugar coating machine that topples, in moulding ciphering process
It is heated, is kept for 75 DEG C of temperature, time 2-3h, balling-up partial size is 63-600 μm.
(10) it chooses shuttles: semi-finished product obtained in (9) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(11) it dries: semi-finished product obtained in (10) is dried into 1.5h at 115 DEG C.
(12) it screens: semi-finished product obtained in (11) being sieved, the semi-finished product of required partial size are obtained.
(13) it is sintered: semi-finished product obtained in (12) being sintered in kiln, sintering curve are as follows: with 60 in kiln
DEG C/speed of h from room temperature rises to 300 DEG C, 0.5h is kept the temperature, then 1100 DEG C are warming up to the speed of 120 DEG C/h, then again with 90
DEG C/speed of h is warming up to 1490 DEG C of heat preservation 2h, it is cooled to room temperature, kiln discharge.
(14) selected, finished product obtained in (13) is carried out to selected, finished product of the selection sphericity greater than 95%.
(15) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (14), (partial size is not more than 20 to carbide fine powder
μm) be polished directly.
(16) it cleans, finished product obtained in (15) is cleaned with deionized water.
(17) it dries: finished product obtained in (16) is dried into 1.2h at 90 DEG C.
Comparative example 1
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate of the D50 less than 7 μm is micro- are carried out in proportion
Powder clout 75%, aluminium oxide powder clout 22% of the D50 less than 7 μm, lignin 3%；Wherein silicic acid of the D50 less than 7 μm
Zirconium micro mist clout is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%, aluminium oxide powder clout of 17%, the D50 less than 7 μm is by partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm
Powder composition, mass percent is respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 2h in 3 D stereo batch mixer, is sufficiently mixed raw material uniformly.
(3) tide is mixed: mixing mixed in (2) being added to the deionized water of mass percent 7%, then in planetary wet stone roller
It is mixed that tide is carried out in machine.
(4) ageing mixture: the mixed raw material of tide in (3) is removed into planetary edge runner-wet mill, stands 48h.
(5) raw material being stranded in (4) encryption compacting: is pressed into strip and block, pressure 580MPa with press.
(6) it is crushed: the strip and block product in (5) is crushed with pulverizer, air-dry.
(7) it sieves: the material after air-drying in (6) is sieved, choose particle of the partial size no more than 75 μm and carry out (8)
Step, the particle greater than 75 μm return again to carry out (6) step.
(8) pelletizing: by the particle obtained in (7) no more than 75 μm as ball, D50 is less than 7 μm by mass percentage
The ratio of the aluminium oxide powder clout 25% of zirconium silicate micro mist clout 75%, D50 less than 7 μm uniformly mixed work is added
Industry micro mist clout, add the deionized water of mass percent 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90, double dynamical strong
Pelletizing in power pelletizer.
(9) it chooses shuttles: semi-finished product obtained in (8) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(10) it dries: semi-finished product obtained in (9) is dried into 1.2h at 118 DEG C.
(11) it is sintered: semi-finished product obtained in (10) being sintered in kiln, sintering curve are as follows: with 60 in kiln
DEG C/speed of h from room temperature rises to 300 DEG C, 0.5h is kept the temperature, then 1100 DEG C are warming up to the speed of 120 DEG C/h, then again with 90
DEG C/speed of h is warming up to 1490 DEG C of heat preservation 2h, it is cooled to room temperature, kiln discharge.
(12) selected, finished product obtained in (11) is carried out to selected, finished product of the selection sphericity greater than 95%.
(13) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (12), (partial size is not more than 20 to carbide fine powder
μm) be polished directly.
(14) it cleans, finished product obtained in (13) is cleaned with deionized water.
(15) it dries: finished product obtained in (14) is dried into 1.2h at 90 DEG C.
Comparative example 2
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate of the D50 less than 7 μm is micro- are carried out in proportion
Powder clout 75%, aluminium oxide powder clout 22% of the D50 less than 7 μm, lignin 3%；Wherein silicic acid of the D50 less than 7 μm
Zirconium micro mist clout is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%, aluminium oxide powder clout of 17%, the D50 less than 7 μm is by partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm
Powder composition, mass percent is respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 2.5h in 3 D stereo batch mixer, is sufficiently mixed raw material
It is even.
(3) pelletizing: will obtain mixing in (2), add the deionized water of mass percent 11%, 2% glycerol, 2%
30 POVIDONE K 30 BP/USP 90, the pelletizing in double dynamical strong granulating machine.
(4) moulding encrypts: by the sphere made in (3), moulding is encrypted in the formula sugar coating machine that topples, in moulding ciphering process
It is heated, is kept for 75 DEG C of temperature, time 2.3h, balling-up partial size is 63-600 μm.
(5) it chooses shuttles: semi-finished product obtained in (4) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(6) it dries: semi-finished product obtained in (5) is dried into 1.5h at 115 DEG C.
(7) it screens: semi-finished product obtained in (6) being sieved, the semi-finished product of required partial size are obtained.
(8) be sintered: semi-finished product obtained in (7) being sintered in kiln, sintering curve are as follows: kiln it is interior with 60 DEG C/
The speed of h rises to 300 DEG C from room temperature, keeps the temperature 0.5h, is then warming up to 1100 DEG C with the speed of 120 DEG C/h, then again with 90 DEG C/
The speed of h is warming up to 1490 DEG C of heat preservation 2h, is cooled to room temperature, kiln discharge.
(9) selected, finished product obtained in (8) is carried out to selected, finished product of the selection sphericity greater than 95%.
(10) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (9), (partial size is not more than 20 μ to carbide fine powder
M) it is polished directly.
(11) it cleans, finished product obtained in (10) is cleaned with deionized water.
(12) it dries: finished product obtained in (11) is dried into 1.2h at 90 DEG C.
Comparative example 3
(1) ingredient: the preparation of raw material, mass percent in formula are as follows: zirconium silicate of the D50 less than 7 μm is micro- are carried out in proportion
Powder clout 75%, aluminium oxide powder clout 22% of the D50 less than 7 μm, lignin 3%；Wherein silicic acid of the D50 less than 7 μm
Zirconium micro mist clout is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%, aluminium oxide powder clout of 17%, the D50 less than 7 μm is by partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm
Powder composition, mass percent is respectively 3%, 80%, 17%.
(2) dry-mixed: the raw material prepared in (1) being mixed into 2.6h in 3 D stereo batch mixer, is sufficiently mixed raw material
It is even.
(3) tide is mixed: mixing mixed in (2) being added to the deionized water of mass percent 7%, then in planetary wet stone roller
It is mixed that tide is carried out in machine.
(4) ageing mixture: the mixed raw material of tide in (3) is removed into planetary edge runner-wet mill, stands 48h.
(5) raw material being stranded in (4) encryption compacting: is pressed into strip and block, pressure 580MPa with press.
(6) it is crushed: the strip and block product in (5) is crushed with pulverizer, air-dry.
(7) it sieves: the material after air-drying in (6) is sieved, choose particle of the partial size no more than 75 μm and carry out (8)
Step, the particle greater than 75 μm return again to carry out (6) step.
(8) pelletizing: by the particle obtained in (7) no more than 75 μm as ball, D50 is less than 7 μm by mass percentage
The ratio of the aluminium oxide powder clout 25% of zirconium silicate micro mist clout 75%, D50 less than 7 μm uniformly mixed work is added
Industry micro mist clout, add the deionized water of mass percent 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90, double dynamical strong
Pelletizing in power pelletizer.
(9) moulding encrypts: by the sphere made in (8), moulding is encrypted in the formula sugar coating machine that topples, in moulding ciphering process
It is heated, is kept for 75 DEG C of temperature, time 2-3h, balling-up partial size is 63-600 μm.
(10) it chooses shuttles: semi-finished product obtained in (9) is chosen shuttles, choose the semi-finished product that sphericity is greater than 95%.
(11) it dries: semi-finished product obtained in (10) is dried into 1.5h at 115 DEG C.
(12) it screens: semi-finished product obtained in (11) being sieved, the semi-finished product of required partial size are obtained.
(13) it is sintered: semi-finished product obtained in (12) being sintered in kiln, sintering curve are as follows: with 120 in kiln
DEG C/speed of h is warming up to 1490 DEG C of heat preservation 2h, it is cooled to room temperature, kiln discharge.
(14) selected, finished product obtained in (13) is carried out to selected, finished product of the selection sphericity greater than 95%.
(15) it polishes: ammonium citrate dispersing agent is added in finished product obtained in (14), (partial size is not more than 20 to carbide fine powder
μm) be polished directly.
(16) it cleans, finished product obtained in (15) is cleaned with deionized water.
(17) it dries: finished product obtained in (16) is dried into 1.2h at 90 DEG C.
The performance of embodiment and comparative example is as shown in table 1.
Table 1
| Project | Partial size (μm) | Density (g/cm3) | Sphericity (%) | It wears away (g/kgh) |
| Embodiment 1 | 90-125 | 3.80 | 95 | 0.25 |
| Embodiment 2 | 150-180 | 3.85 | 95 | 0.28 |
| Embodiment 3 | 180-250 | 3.90 | 95 | 0.30 |
| Embodiment 4 | 250-300 | 3.94 | 96 | 0.26 |
| Embodiment 5 | 300-425 | 4.00 | 97 | 0.26 |
| Comparative example 1 | 300-425 | 3.66 | 95 | 0.49 |
| Comparative example 2 | 300-425 | 3.68 | 95 | 0.60 |
| Comparative example 3 | 300-425 | 3.88 | 96 | 0.55 |
When it can be seen from embodiment and comparative example without " moulding encryption " or without " tide is mixed ", " ageing mixture ", " encryption compacting system
When ball " or when " sintering curve is to directly heat final temperature ", the compounded microbeads partial size prepared is big, density is small, ball
Degree is poor, abrasion are larger.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.All
According to equivalent change or modification made by spirit of the invention, should be covered by the protection scope of the present invention.
Claims (8)
1. it is a kind of using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, which is characterized in that composition of raw materials
Mass percent are as follows: zirconium silicate micro mist clout 48%-88%, aluminium oxide powder clout 9%-49%, lignin 3%；Preparation step
Include: ingredient → dry-mixed → tide it is mixed → ageing mixture → encryption compacting → is chosen shuttles → is dried by broken → screening → pelletizing → moulding encrypts →
→ screening → sintering → selected → polishing → cleaning → drying.
2. it is according to claim 1 using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, it is special
Sign is that the zirconium silicate micro mist clout is during preparing zirconium silicate Polishing Powder, and the D50 abandoned as industrial clout is small
In 7 μm of micro mist, it is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent is respectively 3%,
80%,17%；The aluminium oxide powder clout is to lose during preparing aluminum oxide Polishing Powder as industrial clout
Micro mist of the D50 of abandoning less than 7 μm is made of partial size less than 2.0 μm, 2.0-5.0 μm, 5.0-7.0 μm of powder, mass percent
Respectively 3%, 80%, 17%.
3. it is according to claim 1 using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, it is special
Sign is that the mixed tide is that the deionized water that mass percent is 7% is added in mixed raw material, in planetary edge runner-wet mill
Middle progress tide is mixed.
4. it is according to claim 1 using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, it is special
Sign is that the ageing mixture is that the mixed raw material of tide is removed planetary edge runner-wet mill, stands 48h.
5. it is according to claim 1 using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, it is special
Sign is that the 1st screening is sieved to broken microparticle, chooses particle of the partial size no more than 75 μm and enters
The next step.
6. it is according to claim 1 using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, it is special
Sign is, the pelletizing is particle using partial size no more than 75 μm as ball, by mass percentage zirconium silicate micro mist clout
The industrial micro mist clout that the ratio addition of 50%-90%, aluminium oxide powder clout 10%-50% are uniformly mixed, adds quality
The deionized water of percentage 8%, 2% glycerol, 3% 30 POVIDONE K 30 BP/USP 90, the pelletizing in double dynamical strong granulating machine.
7. it is according to claim 1 using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, it is special
Sign is that the moulding encryption is that the sphere that will have been made carries out moulding encryption, moulding ciphering process in the formula sugar coating machine that topples
In heated, 70-85 DEG C of temperature, soaking time 2-3h.
8. it is according to claim 1 using clout prepare in density high-strength multipurpose zirconium silicate compounded microbeads method, it is special
Sign is, the sintering curve of the sintering are as follows: rises to 300 DEG C from room temperature with the speed of 60 DEG C/h in kiln, keeps the temperature 0.5h, so
1100 DEG C are warming up to the speed of 120 DEG C/h afterwards, 1400-1500 DEG C of heat preservation 2h is then warming up to the speed of 90 DEG C/h again, so
After be cooled to room temperature.
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