CN1147481A - Prodn process of high-purity fine titanate powder - Google Patents
Prodn process of high-purity fine titanate powder Download PDFInfo
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- CN1147481A CN1147481A CN 95116070 CN95116070A CN1147481A CN 1147481 A CN1147481 A CN 1147481A CN 95116070 CN95116070 CN 95116070 CN 95116070 A CN95116070 A CN 95116070A CN 1147481 A CN1147481 A CN 1147481A
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Abstract
Primary titanium dioxide (or meta-titanic acid) and carbonate of alkali earth metals (such as Ba, Sr, Ca, etc.) as raw material are produced into titanate powder with purity not lower than 99.5% and average size smaller than 4.5 micron through purification, composition, fining and other processes. The said prodn process is simple, low in power consumption, easy to realize large-scale prodn of titanate powder. The product is mainly used in electronic industry.
Description
Production process of high-purity fine titanate powder belongs to fine chemistry industry (or hydrometallurgy) field.The titanate powder of producing in this way is mainly used in electronic industry, is a kind of electronic material.
Known is raw material with titanium dioxide and alkaline-earth metal (as barium, strontium, calcium etc.) carbonate, and the method for synthetic high-purity fine titanate powder has following several:
1, solid solid-phase synthesis.Titanium dioxide and alkaline-earth metal (as barium, strontium, calcium etc.) two kinds of solids of carbonate are put into the ball mill ball milling after 20 hours by ratio of components, agglomerating to the powder pressing mold, agglomerate is put into calcining kiln 1150～1350 ℃ of calcinings down, and the titanate agglomerate after the calcining gets titanate powder behind ultra-fine mill (or comminution by gas stream).This method is industrializing implementation.Its main drawback is that the purity and the composition uniformity coefficient of synthesizing titanate powder is not enough, if make raw material then cost improves greatly with high-purity titanium dioxide and carbonate.
2, patent JP81104770. powdered ceramic material contacts calcining with gas fuel combustion flame.For example, titanium dioxide and barium carbonate mix by mole ratio at 1: 1.Water and binding agent mix, make ball, drying again, contact with ethylene combustion flame calcine barium titanate.
3, patent JP6246904. makes ball (2～30 millimeters of long diameters) with two or more powder raw materials mixing with roll type briquetting machine, puts into a chest then equably and carries out sintering reaction, thereby obtain the synthesis oxide agglomerate.For example, barium carbonate powder (0.2 micron of diameter) and titanium dioxide powder (0.2 micron of diameter) are mixed by mole ratio at 1: 1, make the granule of 2～30 millimeters of diameters, put into the alchlor chest equably, form the barium titanate pellet at 1000 ℃ of following sintering, be ground into powder again.
4, patent JP63265820 titanate powder production process comprises: (1), fusion mixture, its component is according to AO-TiO
2-B
2O
3Ternary phase diagrams is chosen (A=Ba, Be, Mg, Ca, Sr or Ra); (2), rapid cooling mixture, generate noncrystal: (3), make noncrystal crystallization; (4), from separating titanium hydrochlorate through the object that Overheating Treatment and diluted acid were handled.For example, BaCO
3-TiO
2-H
3BO
2Mixture is 1300～1400 ℃ of fusings, by nozzle spray, and cools off rapidly by water cold drum, thereby obtain the amorphous thin plate, this thin plate is pulverized, 750-850 ℃ of following sintering 5 hours, pulverize, leaching can be isolated the barium titanate microparticles of 0.7 micron of mean particle size.5, patent R096820.Barium carbonate, titanium dioxide and alchlor wet method homogenizing are produced barium titanate.With mol mixtures such as barium carbonate and titanium dioxide, the aluminium oxide additive wet method homogenizing with 0.6～0.7%, after filtration, and drying, sintering, two sections fine grindings and dusting cover branch obtain barium carbonate powder.
The data that retrieves just sees, known is that the method for raw material production titanate powder has three shortcomings with titanium dioxide and carbonate:
(1), not removal of impurity ability in the existing technical process, impurity only can increase in the building-up process, can not reduce.Therefore, if the grade of raw material is low, production cost is low, and the grade of finished product titanate powder is also low; Obtain high-grade titanate powder, the grade of desired raw material requires very high, and cost improves greatly.Be difficult to realize scale operation;
(2), to carry out the mixing element of two kinds of solid phases by ball milling inhomogeneous, inefficiency, and two kinds of solid phase contact surfaces are little, synthetic calcining temperature is up to 1200 ℃;
(3), because the calcining temperature height, it is unfavorable that the product activity reduces back step operation, and the granularity of calcining back product titanate is bigger, ball milling just can reach granularity requirements once more.
Titanium dioxide of the present invention (or metatitanic acid) and alkaline-earth metal (as barium, strontium, calcium etc.) carbonate raw material is elementary Chemicals.Purify, operations such as synthetic, refinement, byproduct recovery finish in a flow process, quality product height, stable performance, but and at same flow process output multiple product.Therefore, the present invention be easy to realize low-cost, produce high grade fine titanate powder on a large scale, in high quality.
The objective of the invention is with first grade titanium dioxide (or metatitanic acid) and alkaline-earth metal (as barium, strontium, calcium etc.) carbonate is raw material, through technologies such as feedstock purification, synthetic, refinement, byproduct recovery, obtain grade greater than (or equaling) 99.5%, mean particle size is less than 4.5 microns titanate powder.
Process flow sheet of the present invention as shown in Figure 1.
Technical process of the present invention, processing condition and operation steps are as follows:
Titanium dioxide (or metatitanic acid) leaches with pure hydrochloric acid, obtains higher-grade titanium dioxide (or metatitanic acid) filter cake through purifying, filter, washing.Filtrate and washings send the carbonate purification process;
Carbonate is put into filtrate and the washings that above-mentioned operation sends here and is leached, and the pH value that liquid when finishing is leached in control is 5～6.Adding ammoniacal liquor adjusting slurry to pH value is stabilized in more than 11.Leave standstill, filter and obtain clear liquid, clear liquid is through evaporative crystallization, and xln is made into saturated salt ion seminal fluid and send synthetic parcel operation;
In synthetic parcel operation, titanium dioxide (or metatitanic acid) filter cake is pulled an oar with unsaturated carbonate hydrogen ammonium liquid (or salt ion seminal fluid), add the alkanolamine compounds simultaneously as additive, the inclusion that slowly adds unsaturated carbonate hydrogen ammonium liquid (or salt ion seminal fluid) carbonate synthesis salt pair titanium dioxide (or metatitanic acid) then, it is the solid phase inclusion, after filtration, the washing after send calcination process, the solid phase inclusion after 980～1200 ℃ of calcinings, cool off titanate powder.
The concrete operations step:
(1), the purification of titanium dioxide (or metatitanic acid)
1, the required titanium dioxide of synthesizing titanate (or metatitanic acid) (grade＞95%) excessive 0.5～2.0%, join in 25～35% the chemical pure hydrochloric acid solution, liquid-solid ratio is 2.0～4.0, and the agitation leach temperature is a room temperature, extraction time is 3～6 hours, and stirring intensity is greater than 180 rev/mins;
2, centrifuging slurries, filter cake returns steel basin, and washs with the deionized water making beating, liquid-solid ratio 4.0, recentrifuge filters, and repetitive scrubbing like this is filled into the washing lotion pH value and is about 3.5; Leach liquor and washing lotion are sent the carbonate purification process.The titanium dioxide of wash clean (or metatitanic acid) filter cake is stand-by.
(2), alkaline-earth metal (as barium, strontium, calcium etc.) carbonate is purified
1, carbonate (grade＞95%) is pressed expection synthesizing titanate aequum excessive 40%, put into the leach liquor and the washing lotion of titanium dioxide (or metatitanic acid) liquid, if the not enough restock part of hydrochloric acid hydrochloric acid, only surplus small amount of carbonate solid at the bottom of steel basin, the pH value of liquid is about 5～6, add ammoniacal liquor adjusting slurry pH value and be stabilized in more than 11, continue to stir 1 hour, leave standstill more than 2 hours again.Carefulness filters out clear liquid, abandons it behind the residue washing.
2, clear liquid carries out single vaporization and crystallizes to that the amount of main metal ion in the residual mother liquor is 15～25% of a main metal ion total amount, and mother liquor returns the single vaporization or the open circuit removal of impurity.Xln is made into and carries out double evaporation-cooling behind the saturated solution and crystallize to that the amount of main metal ion in the residual mother liquor is 10～15% of a main metal ion total amount, and mother liquor returns single vaporization, and xln is made into saturated salt ion seminal fluid.
(3), synthetic and calcining
1, titanium dioxide (or metatitanic acid) filter cake of wash clean and metering is pulled an oar with unsaturated carbonate hydrogen ammonium liquid, and the bicarbonate of ammonia amount generates 110～125% of carbonate aequum for the salt ion in the precipitation synthesizing titanate.The making beating intensity greater than 150 rev/mins, about 30 minutes of beating time.Add additive (alkanolamine compounds) in making beating liquid, then, slowly add the required salt ion seminal fluid of synthesizing titanate by products scheme, stirring velocity is greater than 200 rev/mins, and churning time was greater than 120 minutes.
2, also can be with titanium dioxide (or metatitanic acid) filter cake of wash clean with the making beating of salt ion seminal fluid, making beating intensity is greater than 200 rev/mins, about 60 minutes of beating time.Add additive (alkanolamine compounds) in making beating in the liquid, then, slowly add the required unsaturated carbonate hydrogen ammonium liquid of synthesizing titanate, bicarbonate of ammonia is excessive 10～20%, and stirring velocity is greater than 200 rev/mins, and churning time was greater than 120 minutes.
3, synthetic gained carbonate filters with whizzer the inclusion of titanium dioxide (or metatitanic acid), and filtrate is ammonium chloride, send evaporative crystallization to get ammonium chloride.Filter cake with deionized water repeatedly agitation and filtration wash that chlorine ion concentration is lower than 0.01 grams per liter to the wash water.
4, the carbonate of wash clean send the calcining furnace calcining to the inclusion of titanium dioxide (or metatitanic acid), and calcining temperature is 980～1200 ℃, and the time is 120 minutes.The calcination product titanate powder is cooled to 250 ℃ and comes out of the stove.Gained titanate powder grade is greater than (or equaling) 99.5%, and the powder mean particle size is 4.5～3.5 microns.
5, when requiring the titanate powder mean particle size, the calcination product titanate powder is carried out ultra-fine wet-milling get final product less than 3.5 microns.For example, will be with 3 hours barium carbonate powder mean particle sizes of zirconia ball (3 millimeters of diameters) wet-milling less than 1.0 microns.
Comparing the present invention with known technology has the following advantages:
(1), not high to ingredient requirement, purify, synthetic, refinement, recovery byproduct all finish in a stream becomes.An ancient unit of weight such as the composition proportion of titanate powder, grade, mean particle size can be adjusted.Flow process adaptability is strong, and production cost is low, the quality product height;
(2), under liquid-phase condition the inclusion of carbonate synthesis salt pair titanium dioxide (or metatitanic acid), the contact surface between two solid phases is big, calcining temperature is reduced in 980～1200 ℃, cuts down the consumption of energy;
(3), since calcining temperature low, the drawing together property of product titanate is big, mean particle size is thinner, except that particular requirement, needn't carry out fine grinding.
(4), be easy to realize low cost, produce the titanate powder of used in electronic industry on a large scale, in high quality.
Fig. 1 is a process flow sheet of the present invention.
Embodiment one: the production technique of barium carbonate powder and condition.
Elementary titanium dioxide powder grade 98%
First grade barium carbonate powder grade 95%
Additive is a thanomin
The technical qualification of selecting for use:
(1), the purification process of titanium dioxide
1, first grade titanium dioxide excessive 2.0%;
2, the chemical pure concentration of hydrochloric acid 25%, and liquid-solid ratio is 4.0;
3, extraction time is 6 hours, 190 rev/mins of stirring intensities;
4, centrifuging slurries, filter cake making beating washing liquid-solid ratio is 4.0, repetitive scrubbing is filled into the washing lotion pH value and is about 3.5.
(2), barium carbonate purification process
1, first grade barium carbonate excessive 40%;
2, the pH value that leaches into liquid is 5～6, adds ammoniacal liquor adjusting slurry pH value and is stabilized in 12, continues to stir 1 hour, leaves standstill 4 hours again;
3, single vaporization crystallizes to that the amount of barium ion in the residual mother liquor is 15% of a barium ion total amount.Double evaporation-cooling crystallizes to that the amount of barium ion in the residual mother liquor is 10% of a barium ion total amount.
(3), synthetic and calcination process
1, the titanium dioxide filter cake of wash clean and metering is pulled an oar with unsaturated carbonate hydrogen ammonium liquid, and the bicarbonate of ammonia amount is 120% of a theoretical aequum;
2, making beating intensity is 180 rev/mins.The thanomin that in making beating liquid, adds dried titanium dioxide amount 0.5%;
When 3, slowly adding barium ion liquid, 210 rev/mins of stirring velocitys, churning time 120 minutes.
4, synthetic gained barium carbonate filters with whizzer the inclusion of titanium dioxide.Filter cake with deionized water repeatedly agitation and filtration wash that chlorine ion concentration is lower than 0.01 grams per liter to the wash water.
5, calcining temperature is 1000 ℃, and the time is 120 minutes.The calcination product barium carbonate powder is cooled to 250 ℃ and comes out of the stove.
The product barium carbonate powder grade that obtains is 99.5%, 4.0 microns of mean particle sizes.
Embodiment two: the production technique of Sr titanate powder and condition
Elementary metatitanic acid powder grade 98%
Elementary strontium carbonate powder grade 95%
Additive is a thanomin
The technical qualification of selecting for use:
(1), the purification process of metatitanic acid
1, elementary metatitanic acid excessive 2.0%;
2, the chemical pure concentration of hydrochloric acid 30%, and liquid-solid ratio is 4.0;
3, extraction time is 3 hours, 190 rev/mins of stirring intensities;
4, centrifuging slurries, filter cake making beating washing liquid-solid ratio is 4.0, repetitive scrubbing is filled into the washing lotion pH value and is about 3.5.
(2), Strontium carbonate powder purification process
1, first grade strontium carbonate excessive 40%;
2, the pH value that leaches into liquid is 5～6, adds ammoniacal liquor adjusting slurry pH value and is stabilized in 14, continues to stir 1 hour, leaves standstill 4 hours again;
3, single vaporization crystallizes to that the amount of strontium ion in the residual mother liquor is 20% of a strontium ion total amount.Double evaporation-cooling crystallizes to that the amount of strontium ion in the residual mother liquor is 15% of a strontium ion total amount.
(3), synthetic and calcination process
1, the metatitanic acid filter cake of wash clean and metering is pulled an oar with saturated strontium ion liquid;
2, making beating intensity is 180 rev/mins.The thanomin that in making beating liquid, adds dried metatitanic acid amount 0.5%;
3, slowly adding unsaturated carbonate hydrogen ammonium liquid measure is 120% of theoretical aequum, 200 rev/mins of stirring velocitys, churning time 120 minutes;
4, synthetic gained Strontium carbonate powder filters with whizzer the inclusion of metatitanic acid.Filter cake with deionized water repeatedly agitation and filtration wash that chlorine ion concentration is lower than 0.01 grams per liter to the wash water:
5, calcining temperature is 1150 ℃, and the time is 120 minutes.The calcination product Sr titanate powder is cooled to 250 ℃ and comes out of the stove;
6, the calcination product Sr titanate powder carried out wet-milling three hours with zirconia ball (3 millimeters of diameters).
The product Sr titanate powder grade that obtains is 99.8%, 1.0 microns of mean particle sizes.
Claims (3)
1, a kind of production process of high-purity fine titanate powder, it is characterized in that, technical process is by the purification of first grade titanium dioxide (or metatitanic acid), the purification of elementary carbonate, synthetic inclusion is formed with the calcining three parts, that is: titanium dioxide (or metatitanic acid) leaches with pure hydrochloric acid, obtains higher-grade titanium dioxide (or metatitanic acid) filter cake through purifying, filter, washing, and filtrate and washings send the carbonate purification process; Carbonate is put into filtrate and the washings that above-mentioned operation sends here and is leached, the pH value that liquid when finishing is leached in control is 5～6, adding ammoniacal liquor adjusting slurry to pH value is stabilized in more than 11, leave standstill, filter and obtain clear liquid, clear liquid is through evaporative crystallization, and xln is made into saturated salt ion seminal fluid and send synthetic parcel operation; In synthetic parcel operation, titanium dioxide (or metatitanic acid) filter cake is pulled an oar with salt ion seminal fluid (or unsaturated carbonate hydrogen ammonium liquid), add the alkanolamine compounds simultaneously as additive, the inclusion that slowly adds unsaturated carbonate hydrogen ammonium liquid (or salt ion seminal fluid) carbonate synthesis salt pair titanium dioxide (or metatitanic acid) then, be the solid phase inclusion, after filtration, the washing after send calcination process; The solid phase inclusion after 980～1200 ℃ of calcinings, cool off titanate powder,
Concrete operations step and processing condition are:
(1), the purification of titanium dioxide (or metatitanic acid)
(1), the required titanium dioxide of synthesizing titanate (or metatitanic acid) (grade＞95%) excessive 0.5～2.0%, join in 25～35% the chemical pure hydrochloric acid solution, liquid-solid ratio is 2.0～4.0, and the agitation leach temperature is a room temperature, extraction time is 3～6 hours, and stirring intensity is greater than 180 rev/mins;
(2), the centrifuging slurries, filter cake returns steel basin, and with deionized water making beating washing, liquid-solid ratio 4.0, recentrifuge filters; Repetitive scrubbing like this is filled into the washing lotion pH value and is about 3.5; Leach liquor and washing lotion are sent the carbonate purification process, and the titanium dioxide of wash clean (or metatitanic acid) filter cake is stand-by,
(2), alkaline-earth metal (as barium, strontium, calcium etc.) carbonate is purified
(1), carbonate (grade＞95%) is pressed expection synthesizing titanate aequum excessive 40%, put into the leach liquor and the washing lotion of titanium dioxide (or metatitanic acid) liquid, if the not enough restock part of hydrochloric acid hydrochloric acid, only surplus small amount of carbonate solid at the bottom of steel basin, the pH value of liquid is about 5～6, adds ammoniacal liquor adjusting slurry pH value and is stabilized in more than 11, continue to stir 1 hour, leave standstill more than 2 hours, carefulness filters out clear liquid again, abandons it behind the residue washing;
(2), clear liquid carries out single vaporization and crystallizes to that the amount of main metal ion in the residual mother liquor is 15～25% of a main metal ion total amount, mother liquor returns the single vaporization or the open circuit removal of impurity, xln is made into and carries out double evaporation-cooling behind the saturated solution and crystallize to that the amount of main metal ion in the residual mother liquor is 10～15% of a main metal ion total amount, mother liquor returns single vaporization, xln is made into saturated salt ion seminal fluid
(3), synthetic and calcining
(1), titanium dioxide (or metatitanic acid) filter cake of wash clean and metering is with the making beating of unsaturated carbonate hydrogen ammonium liquid, the bicarbonate of ammonia amount generates 110～125% of carbonate aequum for the salt ion in the precipitation synthesizing titanate, making beating intensity is greater than 150 rev/mins.About 30 minutes of beating time adds additive (alkanolamine compounds) in making beating liquid, then, slowly add the required salt ion seminal fluid of synthesizing titanate by products scheme, and stirring velocity is greater than 200 rev/mins, and churning time was greater than 120 minutes;
(2), also titanium dioxide (or metatitanic acid) filter cake of wash clean can be pulled an oar with the salt ion seminal fluid, making beating intensity is greater than 200 rev/mins, about 60 minutes of beating time, in making beating liquid, add additive (alkanolamine compounds), then, slowly add the required unsaturated carbonate hydrogen ammonium liquid of synthesizing titanate, bicarbonate of ammonia excessive 10～20%, stirring velocity is greater than 200 rev/mins, and churning time was greater than 120 minutes;
(3), synthetic gained carbonate filters with whizzer the inclusion of titanium dioxide (or metatitanic acid), filtrate is ammonium chloride, send evaporative crystallization to get ammonium chloride, filter cake with deionized water repeatedly agitation and filtration wash that chlorine ion concentration is lower than 0.01 grams per liter to the wash water;
(4), the carbonate of wash clean send the calcining furnace calcining to the inclusion of titanium dioxide (or metatitanic acid), calcining temperature is 980～1200 ℃, time is 120 minutes, the calcination product titanate powder is cooled to 250 ℃ and comes out of the stove, gained titanate powder grade is greater than (or equaling) 99.5%, and the powder mean particle size is 4.5～3.5 microns;
(5), when requiring the titanate powder mean particle size less than 3.5 microns, the calcination product titanate powder is carried out ultra-fine wet-milling gets final product, for example, will be with zirconia ball (3 millimeters of diameters) wet-milling 3 hours barium carbonate powder mean particle sizes less than 1.0 microns.
2, production process of high-purity fine titanate powder according to claim 1 is characterized in that, the technology and the technical qualification of producing barium carbonate powder are as follows:
Elementary titanium dioxide powder grade 98%
First grade barium carbonate powder grade 95%
Additive is a thanomin
The technical qualification of selecting for use:
(1), the purification process of titanium dioxide
(1), first grade titanium dioxide excessive 2.0%;
(2), chemical pure concentration of hydrochloric acid 25%, liquid-solid ratio is 4.0;
(3), extraction time is 6 hours, 190 rev/mins of stirring intensities;
(4), centrifuging slurries.Filter cake making beating washing liquid-solid ratio is 4.0.Repetitive scrubbing is filled into the washing lotion pH value and is about 3.5,
(2), barium carbonate purification process
(1), first grade barium carbonate excessive 40%;
(2), the pH value that leaches into liquid is 5～6, adds ammoniacal liquor adjusting slurry pH value and is stabilized in 12, continues to stir 1 hour, left standstill again 4 hours;
(3), single vaporization crystallizes to that the amount of barium ion in the residual mother liquor is 15% of a barium ion total amount, double evaporation-cooling crystallizes to that the amount of barium ion in the residual mother liquor is 10% of a barium ion total amount,
(3), synthetic and calcination process
(1), the titanium dioxide filter cake of wash clean and metering is with the making beating of unsaturated carbonate hydrogen ammonium liquid, the bicarbonate of ammonia amount is 120% of a theoretical aequum;
(2), 180 rev/mins of intensity of making beating, in making beating liquid, add the thanomin of dried titanium dioxide amount 0.5%;
When (3), slowly adding the barium ion seminal fluid, 210 rev/mins of stirring velocitys, churning time 120 minutes;
(4), synthetic gained barium carbonate filters with whizzer the inclusion of titanium dioxide, filter cake with deionized water repeatedly agitation and filtration wash that chlorine ion concentration is lower than 0.01 grams per liter to the wash water;
(5), calcining temperature is 1000 ℃, the time is 120 minutes, the calcination product barium carbonate powder is cooled to 250 ℃ and comes out of the stove.
3, production process of high-purity fine titanate powder according to claim 1 is characterized in that, the technology and the technical qualification of producing Sr titanate powder are:
Elementary metatitanic acid powder grade 98%
Elementary strontium carbonate powder grade 95%
Additive is a thanomin
The technical qualification of selecting for use:
(1), the purification process of metatitanic acid
(1), elementary metatitanic acid excessive 2.0%;
(2), chemical pure concentration of hydrochloric acid 30%, liquid-solid ratio is 4.0;
(3), extraction time is 3 hours, 190 rev/mins of stirring intensities;
(4), the centrifuging slurries, filter cake making beating washing liquid-solid ratio is 4.0, repetitive scrubbing is filled into the washing lotion pH value and is about 3.5,
(2), Strontium carbonate powder purification process
(1), first grade strontium carbonate excessive 40%;
(2), the pH value that leaches into liquid is 5～6, adds ammoniacal liquor adjusting slurry pH value and is stabilized in 14, continues to stir 1 hour, left standstill again 4 hours;
(3), single vaporization crystallizes to that the amount of strontium ion in the residual mother liquor is 20% of a strontium ion total amount.Double evaporation-cooling crystallizes to that the amount of strontium ion in the residual mother liquor is 15% of a strontium ion total amount,
(3), synthetic and calcination process
(1), the metatitanic acid filter cake of wash clean and metering is pulled an oar with saturated strontium ion seminal fluid;
(2), 180 rev/mins of intensity of making beating, in making beating liquid, add the thanomin of dried metatitanic acid amount 0.5%;
(3), slowly adding unsaturated carbonate hydrogen ammonium liquid measure is 120% of theoretical aequum, 200 rev/mins of stirring velocitys, churning time 120 minutes;
(4), synthetic gained Strontium carbonate powder filters with whizzer the inclusion of metatitanic acid, filter cake with deionized water repeatedly agitation and filtration wash that chlorine ion concentration is lower than 0.01 grams per liter to the wash water;
(5), calcining temperature is 1150 ℃, the time is 120 minutes, the calcination product Sr titanate powder is cooled to 250 ℃ and comes out of the stove;
(6), the calcination product Sr titanate powder carried out wet-milling three hours with chromic oxide ball (3 millimeters of diameters).
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|---|---|---|---|
| CN95116070A CN1042724C (en) | 1995-10-11 | 1995-10-11 | Prodn process of high-purity fine titanate powder |
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| CN95116070A CN1042724C (en) | 1995-10-11 | 1995-10-11 | Prodn process of high-purity fine titanate powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993242A (en) * | 2009-08-19 | 2011-03-30 | 湖南人文科技学院 | Ultrafine lead titanate and lead barium titanate ceramic powder and preparation method thereof |
| CN107032393A (en) * | 2017-06-05 | 2017-08-11 | 山东东佳集团股份有限公司 | The method that slurries fixation prepares barium metatitanate |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5945928A (en) * | 1982-09-08 | 1984-03-15 | Sony Corp | Preparation of fine particle from strontium titanate |
| JPS6131345A (en) * | 1984-07-25 | 1986-02-13 | 堺化学工業株式会社 | Manufacture of composition |
| DE3739853A1 (en) * | 1987-11-25 | 1989-06-08 | Philips Patentverwaltung | METHOD FOR PRODUCING BARIUM TITANATE IN POWDER FORM |
-
1995
- 1995-10-11 CN CN95116070A patent/CN1042724C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993242A (en) * | 2009-08-19 | 2011-03-30 | 湖南人文科技学院 | Ultrafine lead titanate and lead barium titanate ceramic powder and preparation method thereof |
| CN107032393A (en) * | 2017-06-05 | 2017-08-11 | 山东东佳集团股份有限公司 | The method that slurries fixation prepares barium metatitanate |
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| CN1042724C (en) | 1999-03-31 |
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