CN1712356A - Reactor, reacting method and product for preparing barium titanate powder - Google Patents
Reactor, reacting method and product for preparing barium titanate powder Download PDFInfo
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- CN1712356A CN1712356A CN 200410027720 CN200410027720A CN1712356A CN 1712356 A CN1712356 A CN 1712356A CN 200410027720 CN200410027720 CN 200410027720 CN 200410027720 A CN200410027720 A CN 200410027720A CN 1712356 A CN1712356 A CN 1712356A
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Abstract
A reactor of barium titanate powder, its production and product are disclosed. The reactor consists of first reactor (1), second reactor (2) and ageing device (3). Sandwich (71) and (72) are arranged in reactor (1) and reactor (2) for full reaction. The production is carried out by first reaction, second reaction, ageing, thermolysis, break and calcinations. It has higher efficiency and is simple, grain size achieves 0.03-1.00mum.
Description
Technical field
The present invention relates to a kind of reaction unit, method therefor and products obtained therefrom for preparing barium titanate powder, more particularly, the present invention relates to a kind of fractional order reaction device of barium titanate powder, the preparation method of fractional order reaction and barium titanate powder of gained of preparing.
Background technology
The preparation method of barium titanate powder has a variety of, for example hydrolysis method, sol-gel processing, hydrothermal method and oxalate precipitation method or the like.The industrial the most frequently used method for preparing barium titanate powder is the oxalate precipitation method of Clabaugh invention at present.This invention is pressed about 1: 1 mixed with barium chloride solution and titanium tetrachloride aqueous solution, the barium titanium solution that mixes slowly joins in the oxalic acid solution of certain temperature, reaction precipitation goes out barium titanium oxalate, clean up foreign ions such as oxalate denominationby, chlorion, calcining synthesis of barium titanate powder.Because throw out titanium oxyoxalate titanate particle is the reunion attitude, at high temperature calcines the synthetic barium titanate powder and can produce serious hard aggregation, loose density is big, has hindered application.
In order to reduce the hard aggregation of barium titanate powder, the method that a kind of oxalate method prepares barium titanate powder is disclosed among the Chinese patent application CN 01118560.0, this method principal feature is to pulverize the barium titanate throw out with the mode of wet-milling before calcining, so that make its average particulate size less than 5 μ m, the barium titanium oxalate slurries that form adopt spray-dryer to carry out drying, calcine then, can obtain the barium titanate powder of median size less than 0.9 μ m through pulverizing.But, owing to need carry out spraying drying, cause particle to form secondary agglomeration, still can produce hard aggregation to a certain degree after the calcining.
The method that a kind of hydrolysis method prepares barium titanate powder is disclosed among the Chinese patent application CN 98121320.0, this method is with IPA solution (also can the add La) hybrid reaction of baryta water and pure titanium, through overaging, centrifuge dehydration, stirring and washing, centrifuge dehydration again in hot water, in ethanol, mix and steps such as centrifuge dehydration, drying, crushing, obtaining particle size is the barium titanate powder of 0.05 μ m, cube crystal phase structure.Though this method can obtain more tiny even barium titanate powder,, the technical process complexity of this method, the cost height is unfavorable for carrying out scale operation.
Therefore, be necessary to work out a kind of anti-reaction unit and preparation method that can solve the hard aggregation problem of barium titanate powder up hill and dale, and make preparation process be convenient to operation as much as possible, to adapt to the needs of industrialized production.
Summary of the invention
One of purpose of the present invention provides a kind of fractional order reaction device for preparing barium titanate powder, when utilizing this fractional order reaction device to prepare barium titanate powder, reaction is carried out continuously, the reaction soln thorough mixing is even, reaction density is dynamic equalization all the time, sufficient reacting is thorough, and the barium titanium oxalate of generation is evenly tiny.
Fractional order reaction device of the present invention comprises A reactor, second reactor and digestion tank; Be respectively equipped with interlayer in A reactor and the second reactor; Interlayer is divided into sandwich portion and inner chamber part respectively with the inside of A reactor and second reactor; Bottom at inner chamber is respectively equipped with slit, and inner chamber communicates with interlayer by slit; In addition, also be provided with feeding unit on the A reactor, this feeding unit passes through the sandwich portion of A reactor and directly links to each other with the inner cavity branch of A reactor; The interlayer of A reactor is provided with discharge port, and this discharge port passes through the sandwich portion of second reactor by pipeline and directly links to each other with the inner cavity branch of second reactor; Also be provided with discharge port on the interlayer of second reactor, this discharge port then links to each other with digestion tank by pipeline.
In the above-mentioned fractional order reaction device, the thickness of the interlayer of two reactors preferably is respectively 1-10cm; And the height of the slit of two reactors can several millimeters to tens centimetres, are preferably 1-5cm.The size of the thickness of interlayer and the height of slit and each stage reactor, feeding rate, discharging speed etc. are relevant, and the volume of each stage reactor can be adjusted according to industrial scale, and its size is also relevant with feeding rate, discharging speed etc.Generally speaking, the volume of each stage reactor of the present invention can be basic identical or close, and size can be controlled between the 100-1000L, preferably between 100-300L.
The position of the discharge port of each stage reactor of the present invention is also very important, and generally speaking, they are separately positioned on apart from the position more than 1/2 height of respective reaction device bottom, preferably are arranged on apart from the position of reactor bottom 1/2～2/3.
Can be provided with two or more feed pipe on the feeding unit of the present invention, perhaps be provided with a T-valve feed pipe.
In addition, between the second reactor of described fractional order reaction device and digestion tank, the one or more reactor that has interlayer be can also be connected with, three reactor, fourth-order reaction device and even staged reactor for example are connected with.But can make reaction solution react relatively fully owing to only have the fractional order reaction device of A reactor and second reactor, reach industrial requirement.
The working process of fractional order reaction device of the present invention is roughly as follows: material solution adds in the A reactor along different feed pipes, under constantly stirring, material solution is mixed fully, and reaction constantly, generate small precipitate particles, form mixed solution, and in the mixed solution of reactor bottom, the content of precipitate particles is high more.Along with the material solution of adding constantly in A reactor, the mixed solution of A reactor bottom will pass through slit lentamente, overflows discharge port along interlayer, flow in the second reactor along pipeline then.Like this, just the mixed solution that precipitate particles content is high in the A reactor is transferred in the second reactor continuously and lentamente.In second reactor, this mixed solution continues reaction, thereby generates more particles.Similarly, the mixed solution of second reactor bottom also can pass through slit lentamente, overflows discharge port along interlayer, flow in the digestion tank along pipeline, finally forms the titanium oxyoxalate precipitated barium.
Another object of the present invention provides a kind of fractional order reaction method hard aggregation problem, the preparation barium titanate powder that can solve barium titanate powder, and this preparation method may further comprise the steps:
(1) aqueous solution with oxalic acid, titanium tetrachloride and bariumchloride adds in the A reactor, and makes its thorough mixing;
(2) mixed solution in the A reactor is transferred in the second reactor, and abundant mixing;
(3) mixed solution in the second reactor is transferred in the digestion tank, under 20～90 ℃ temperature, carried out ageing, obtain the barium titanium oxalate throw out;
(4) the above-mentioned barium titanium oxalate throw out that obtains of washing, centrifuge dehydration then;
(5) the barium titanium oxalate throw out after the above-mentioned centrifuge dehydration is carried out thermolysis under 400～1100 ℃ temperature, and the powder that obtains after the thermolysis is pulverized;
(6) powder that obtains after the above-mentioned pulverizing is calcined under 900～1300 ℃ temperature;
(7) powder that obtains after the above-mentioned calcining is carried out gradation sizing or pulverizing, obtain final barium titanate powder.
In the aforesaid method, the mixed solution in step (2) and the step (3) shifts, and is that the bottom of mixed solution by the respective reaction device moved to earlier more than the mid-way of this reactor, and the position as 1/2 to 2/3 is transferred in the next stage reaction unit then.
In above-mentioned step (1), the mol ratio of titanium tetrachloride and bariumchloride is preferably 1: 1～and 1.2: 1.The hybrid mode of oxalic acid, titanium tetrachloride and bariumchloride can be earlier titanium tetrachloride and bariumchloride to be made mixing solutions, adds to this mixing solutions and oxalic acid solution in the A reactor respectively again; Also can be earlier oxalic acid and titanium tetrachloride to be made mixing solutions, add to this mixing solutions and barium chloride solution in the A reactor respectively again; Or be that oxalic acid solution, titanium tetrachloride solution and barium chloride solution are added in the A reactor separately respectively.Preferred one of the preceding two kinds of hybrid modes that adopt.Specifically, step (1) is preferably by following dual mode operation:
Purified titanium tetrachloride is slowly joined temperature be lower than in 30 ℃ the pure water, obtaining concentration is the titanium tetrachloride aqueous solution of 3～6mol/L.Then a certain amount of solid oxalic acid or oxalic acid solution are joined in the titanium tetrachloride aqueous solution, mix, add ammoniacal liquor or liquefied ammonia, be mixed with mixing solutions while stir, the pH value of solution value is about 2.5～3.5, and the concentration of calculating with titanium tetrachloride is about 0.5～1.0mol/L.Dissolve BaCl with pure water
22H
2O, and remove impurity in the barium chloride solution, obtaining concentration is the barium chloride solution of 0.5～1.5mol/L.At last, the mixed solution with oxalic acid and titanium tetrachloride mixes with barium chloride solution.Perhaps
Mode 2
Dissolve BaCl with pure water
22H
2O, and remove impurity in the barium chloride solution, obtaining concentration is the barium chloride solution of 0.5～1.5mol/L.Purified titanium tetrachloride is slowly joined temperature be lower than in 30 ℃ the pure water, obtaining concentration is the titanium tetrachloride aqueous solution of 3～6mol/L.Then, barium chloride solution and titanium tetrachloride aqueous solution are become uniform mixed solution by 1: 1～1.2: 1 mixed in molar ratio, the concentration of calculating with titanium tetrachloride is 0.5～1.0mol/L.Dissolve H with pure water
2C
2O
42H
2O, and remove impurity in the oxalic acid solution, obtaining concentration is the oxalic acid aqueous solution of 1～1.5mol/L.And to make its temperature be 20～90 ℃.At last, the mixed solution with titanium tetrachloride and bariumchloride mixes with oxalic acid solution.
(see figure 3) is preferably finished in above-mentioned step (1)～(3) in fractional order reaction device of the present invention.
The step of aforesaid method (3), ageing is preferably carried out under 20～90 ℃ condition.By ageing, particle is constantly sunk and grow, form precipitation.
The step of aforesaid method (4) by washing, can be removed Cl
-, C
2O
4 2-, NH
4 2+Deng foreign ion; Preferably, after washing precipitation, with the centrifugal precipitation surface moisture of removing of whizzer.
The step of aforesaid method (5) by thermolysis, obtains the primary barium titanate powder, and this powder comprises BaO, BaCO
3With in other barium titanyl compositions one or more, wherein the content of free barium is expressed as 2～80% with BaO%.Thermolysis is preferably under 400～1100 ℃ the temperature to be carried out 1～6 hour.The method of pulverizing is preferably dry type and pulverizes, and can adopt pulverizer pulverizing or other Dry Crushing to pulverize.
The step of aforesaid method (6), calcining is 1～6 hour under 900～1300 ℃ temperature preferably.
Aforesaid method can further include homodisperse step: the barium titanate powder that step (6) is obtained carries out homodisperse, makes its loose density≤1.8g/ml.Homodisperse method can be the screening or other can make barium titanate powder dispersive method.By disperseing, the barium titanate powder loose density that obtains in addition can≤1.0g/ml.Preferably, adopt the barium titanate powder of dispersion back loose density≤1.0g/ml to make piezoelectric ceramics, posistor (PTC), multilayer chip capacitor (MLCC), cold light technology electronic components such as (EL).
A further object of the present invention provide in above-mentioned fractional order reaction device, prepare or by the preparation of above-mentioned fractional order reaction method barium titanate powder, the crystalline phase of this barium titanate powder is cube phase and/or cubic phase, the mol ratio of barium and titanium is 0.990～1.008, median size is 0.03～1.00 μ m, loose density≤1.8g/ml.
Because reaction sorting equipment of the present invention can make reaction and ageing continuously carry out, and reaction solution is reacted fully, produces more titanium oxyoxalate precipitated barium as much as possible, the deposit seeds of generation is evenly tiny.And method of the present invention is easy and simple to handle, can avoid the barium titanium oxalate particle in the process of preparation hard aggregation to take place up hill and dale.
Description of drawings
Fig. 1 is a kind of process flow sheet of the present invention.
Fig. 2 is an another kind of process flow sheet of the present invention.
Fig. 3 is a fractional order reaction schematic representation of apparatus of the present invention.
Fig. 4 is the stereoscan photograph of the barium titanate powder for preparing of the present invention.
Among the figure, each Reference numeral implication is:
1------A reactor 2-------second reactor
3--------digestion tank 5--------feeding unit
10-------feed pipe 10-------feed pipe
41-------drainage line 42-------drainage line
61-------discharge port 62-------discharge port
71-------interlayer 72-------interlayer
81-------slit 82-------slit
91-------inner chamber 92-------inner chamber
Embodiment
Press the technical process of Fig. 1, it is that 2.0mol/L, volume are in the titanium tetrachloride aqueous solution of 480L that about 266 kilograms solid oxalic acid (or oxalic acid solution) is joined weaker concn, mixing, add ammoniacal liquor (or liquefied ammonia) while stirring, be mixed with mixing solutions, the pH value of solution value is 3.05, and the concentration of calculating with titanium tetrachloride is 0.5mol/L.Dominant discharge is 2500L/Hr, is concentration 0.525mol/L, the barium chloride solution of 1920L and above-mentioned mixing solutions join in the A reactor (1) of Fig. 3 device, about the volume 200L of this reactor, reaction soln is fully mixed in this reactor, when the reaction soln in this reactor constantly increases, the reaction soln that contains the barium titanium oxalate particle is by slit (81), overflow the discharge port (61) of distance reactor (1) bottom about 2/3 along interlayer (71), flow into (volume of its volume and A reactor (1) is basic identical) in the second reactor (2) by drainage line (41), further mix herein, then, the reaction soln that contains barium titanate particles in the second reactor (2) flow in the digestion tank (3) by drainage line (42) again by slit (82).At last, in digestion tank (3),, obtain the tiny barium titanium oxalate throw out of uniform particles in 50 ℃ of ageings 2 hours.In the titanium oxyoxalate precipitated barium, add pure water and carry out agitator treating, remove Cl
-, C
2O
4 2-, NH
4 2+Deng foreign ion, use the whizzer centrifuge dehydration.The barium titanium oxalate that has dewatered is carried out thermolysis, and the pyrolysated condition is to be heated to 500 ℃ and be incubated 2.5 hours in continuous tunnel furnace, obtains original barium titanate powder, and the free barium of this powder is expressed as 40.84% with BaO%.Pulverize above-mentioned barium titanate powder with pulverizer, obtaining mean particle size is the powder of 0.35 μ m (recording by particle-size analyzer).This powder is calcined under 950 ℃ condition and was obtained to have a cube phase structure (recording by x-ray diffractometer) in 2.5 hours, the barium titanium than be 0.998, median size is that 0.43 μ m, particle morphology are the barium titanate powder of sphere or almost spherical.Fig. 4 is the stereoscan photograph of the prepared the finished product barium titanate powder of present embodiment.As can see from Figure 4, the prepared barium titanate powder particle of the present invention has the pattern of subglobular, and has good dispersion state, and this illustrates that method of the present invention has solved the hard aggregation problem in the barium titanate powder preparation process.With screen(ing) machine screening be mixed into dispersive, loose density is the barium titanate powder of 0.617g/ml.In this powder, add Sr, Ca, Pb, Zr, La, Y, Nb, Ta; and mix with the tackiness agent of vinyl-acetic ester and so on; through granulation, to be pressed into diameter be that 8mm and thickness are the round billet sheet of 1mm; under protection of inert gas in 1300 ℃ of sintering 120 minutes; obtain semiconductor ceramic chip; recording room temperature resistivity is 30 Ω .cm, and withstand voltage is 1055V/mm, and residual current is 2.6mA.
In following embodiment, the size of barium titanate powder all records by particle-size analyzer, the crystalline phase of barium titanate powder all records by x-ray diffractometer, and the particle morphology of barium titanate powder is observed with scanning electron microscope, explains no longer in addition later on.
Embodiment 2
Press the technical process of Fig. 2, the titanium tetrachloride aqueous solution of 240 liters of 4.0mol/L and the barium chloride solution of 800 liters of 1.2mol/L are mixed into uniform clarifying mixing solutions, 1600 liters of 1.5mol/L oxalic acid aqueous solutions are heated to 50 ℃ in advance, and dominant discharge is 2500L/Hr.Above-mentioned solution adds in the A reactor (1) (the about 200L of volume) of device shown in Figure 3, the abundant stirring and evenly mixing of reaction soln quilt in reactor (1), when wherein reaction soln constantly increases, bottom contains the reaction soln of barium titanium oxalate particle by slit (81), overflow the discharge port (61) of distance reactor (1) bottom about 2/3 along interlayer (71), flow in the second reactor (2) (the about 200L of volume) by drainage line (41), further mix herein, then, reactor (2) bottom contains the reaction soln of barium titanium oxalate particle again by slit (82), flow in the digestion tank (3) by drainage line (42).50 ℃ of ageings 2 hours in digestion tank (3) at last obtain the tiny barium titanium oxalate throw out of uniform particles.Add pure water in this throw out and carry out agitator treating, remove Cl
-, C
2O
4 2-Deng foreign ion, use the whizzer centrifuge dehydration.The titanium oxyoxalate precipitated barium that has dewatered is carried out thermolysis, and the pyrolysated condition is to be heated to 900 ℃ and be incubated 2.5 hours in continuous tunnel furnace, obtains original barium titanate powder, and the free barium of this powder is expressed as 5.51% with BaO%.With pulverizer above-mentioned powder being pulverized is that mean particle size is the powder of 0.53 μ m.The powder of calcining under the condition of 1150 ℃ and 2.5 hours through pulverizing, obtain to have tetragonal phase structure, the barium titanium than be 1.004, median size is that 0.81 μ m, particle morphology are the barium titanate powder of sphere or almost spherical.Screen(ing) machine is mixed into dispersive, loose density is the barium titanate powder of 0.991g/ml.In this powder, add some useful things (as elements such as Cu, Mn, Ni, Ti) that mix, make the X7R multilayer chip capacitor.Physical properties is with to record electrical property as shown in table 1.
The physical properties of table 1 embodiment 2 gained barium titanate powders and the comparison of MLCC performance and prior art
| Project | Physical properties | Electrical property | ||||||
| Median size (μ m) | Loose density (g/ml) | ??Ba/Ti | Crystalline phase | ??C(nF) | Loss (%) | ??IR ??(10 11??Ω) | ??TCC(％) | |
| Embodiment 2 | ??0.81 | ??0.991 | ??1.004 | 40,000 | ??15.4 | ??1.5 | ??0.7 | ??-2.5/-7.7 |
| The prior art sample | ??0.85 | ??0.956 | ??0.999 | 40,000 | ??12.9 | ??1.5 | ??0.7 | ??-2.8/-8.4 |
Embodiment 3
Press the technical process of Fig. 1, about 89 kilograms solid oxalic acid (or oxalic acid solution) joined to be diluted to concentration be that 2.0mol/L, volume are in the titanium tetrachloride aqueous solution of 160L, mix, add ammoniacal liquor (or liquefied ammonia) while stirring, be mixed with mixing solutions, the pH value of solution value is 3.01, and the concentration of calculating with titanium tetrachloride is 0.5mol/L.Dominant discharge is 1000L/Hr, with concentration is 0.525mol/L, the barium chloride solution of 640L and above-mentioned mixing solutions add in the A reactor (1) (the about 160L of volume) of device shown in Figure 3, reaction soln is fully mixed in reactor (1), when wherein reaction soln constantly increases, the reaction soln that contains the barium titanium oxalate particle is by slit (81), overflow the discharge port (61) of distance reactor (1) bottom about 2/3 along interlayer (71), flow in the second reactor (2) (the about 160L of volume) by drainage line (41), further mix herein, then, the reaction soln that contains the barium titanium oxalate particle in the second reactor (2) flow in the digestion tank (3) by drainage line (42) again by slit (82).20～90 ℃ of ageings 2 hours in digestion tank (3) at last obtain the tiny barium titanium oxalate throw out of uniform particles.Add pure water in this throw out and carry out agitator treating, remove Cl
-, C
2O
4 2-, NH
4 2+Deng foreign ion, use the whizzer centrifuge dehydration.The barium titanium oxalate that has dewatered is carried out thermolysis, and the pyrolysated condition is to be heated to 600 ℃ and be incubated 2.5 hours in continuous tunnel furnace, obtains original barium titanate powder, and the free barium of this powder is expressed as 18.11% with BaO%.Pulverize above-mentioned barium titanate powder with pulverizer, obtaining mean particle size is the powder of 0.45 μ m.This powder was calcined 2.5 hours under 1150 ℃ condition, obtain to have tetragonal phase structure, the barium titanium than be 1.005, median size is that 0.98 μ m, particle morphology are the barium titanate powder of sphere or almost spherical.Through sieving machine be mixed into dispersive, loose density is the barium titanate powder of 0.999g/ml.This powder can be used for piezoelectric ceramics, posistor (PTC), multilayer chip capacitor (MLCC), cold light technology (EL) etc. and does the medium layer material.
Claims (10)
1, a kind of fractional order reaction device is characterized in that, described fractional order reaction device comprises A reactor (1), second reactor (2) and digestion tank (3); Be respectively equipped with interlayer (71) and interlayer (72) in A reactor (1) and the second reactor (2); Interlayer (71) is divided into interlayer (71) part and inner chamber (91) part with the inside of A reactor (1), and interlayer (72) is divided into interlayer (72) part and inner chamber (92) part with the inside of second reactor (2); Be respectively equipped with slit (81), (82) in the bottom of inner chamber (91), (92), inner chamber (91), (92) communicate with interlayer (71), (72) respectively by slit (81), (82); A reactor (1) is provided with feeding unit (5), and this feeding unit (5) passes through the interlayer (71) of A reactor (1) and directly links to each other with the inner chamber (91) of A reactor (1); The interlayer (71) of A reactor (1) is provided with discharge port (61), and discharge port (61) passes through the interlayer (72) of second reactor (2) by pipeline (41) and directly links to each other with the inner chamber (92) of second reactor (2); The interlayer (72) of second reactor (2) is provided with discharge port (62), and discharge port (62) links to each other with digestion tank (3) by pipeline (42).
2, fractional order reaction device as claimed in claim 1 is characterized in that, the thickness of described reactor interlayer (71), (72) is respectively 1-10cm; The height of described slit (81), (82) is respectively 1-5cm.
3, fractional order reaction device as claimed in claim 1 is characterized in that, described discharge port (61), (62) are separately positioned on apart from the position more than 1/2 height of respective reaction device bottom.
4, fractional order reaction device as claimed in claim 1 is characterized in that, described feeding unit (5) is provided with two or more feed pipe (10).
5, fractional order reaction device as claimed in claim 1 is characterized in that, is connected with the one or more reactor that has interlayer between the second reactor (2) of described fractional order reaction device and digestion tank (3).
6, a kind of method that adopts fractional order reaction to prepare barium titanate powder, this method may further comprise the steps:
(1) aqueous solution with oxalic acid, titanium tetrachloride and bariumchloride adds in the A reactor, and makes its thorough mixing;
(2) mixed solution in the A reactor is transferred in the second reactor, and abundant mixing;
(3) mixed solution in the second reactor is transferred in the digestion tank, under 20～90 ℃ temperature, carried out ageing, obtain the barium titanium oxalate throw out;
(4) the above-mentioned barium titanium oxalate throw out that obtains of washing, centrifuge dehydration then;
(5) the barium titanium oxalate throw out after the above-mentioned centrifuge dehydration is carried out thermolysis under 400～1100 ℃ temperature, and the powder that obtains after the thermolysis is pulverized;
(6) powder that obtains after the above-mentioned pulverizing is calcined under 900～1300 ℃ temperature;
(7) powder that obtains after the above-mentioned calcining is sieved or pulverizes, obtain final barium titanate powder.
7, method as claimed in claim 6, it is characterized in that, mixed solution described in step (2) and the step (3) shifts, and is that the bottom of described mixed solution by the respective reaction device moved to earlier more than the mid-way of this reactor, transfers to then in the next stage reaction unit.
8, method as claimed in claim 6 is characterized in that, in the step (1), earlier titanium tetrachloride and bariumchloride is made mixing solutions, this mixing solutions and oxalic acid solution is added to respectively in the described A reactor again; Perhaps earlier oxalic acid and titanium tetrachloride are made mixing solutions, again this mixing solutions and barium chloride solution are added to respectively in the described A reactor; Perhaps oxalic acid solution, titanium tetrachloride solution and barium chloride solution are added to respectively in the described A reactor.
9, method as claimed in claim 6 is characterized in that, the mixed solution in the step (3) in the second reactor was transferred to earlier in the reactor more than three grades or three grades before transferring to digestion tank.
10, a kind of barium titanate powder that requires the described method of one of 6-9 to prepare according to aforesaid right, the crystalline phase of this barium titanate powder is cube phase and/or cubic phase, and the mol ratio of barium and titanium is 0.990～1.008, and median size is 0.03～1.00 μ m.
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| CN102432454A (en) * | 2010-09-07 | 2012-05-02 | 日本化学工业株式会社 | Barium titanyl oxalate particle, method for preparing the same and method for preparing barium titanate |
| CN103796956A (en) * | 2011-09-15 | 2014-05-14 | 日本化学工业株式会社 | Method for producing barium titanyl oxalate and method for producing barium titanate |
| CN106380194A (en) * | 2016-08-31 | 2017-02-08 | 仙桃市中星电子材料有限公司 | Production technology of nanometer tetragonal barium titanate |
| CN110526286A (en) * | 2019-10-10 | 2019-12-03 | 重庆中坛洋铭化工科技有限公司 | A kind of environment-friendly and energy-efficient barium titanate production system and technique |
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| CN110526286B (en) * | 2019-10-10 | 2024-04-26 | 重庆中坛洋铭化工科技有限公司 | Environment-friendly energy-saving barium titanate production system and process |
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2004
- 2004-06-21 CN CN 200410027720 patent/CN1712356A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102432454A (en) * | 2010-09-07 | 2012-05-02 | 日本化学工业株式会社 | Barium titanyl oxalate particle, method for preparing the same and method for preparing barium titanate |
| CN103796956A (en) * | 2011-09-15 | 2014-05-14 | 日本化学工业株式会社 | Method for producing barium titanyl oxalate and method for producing barium titanate |
| CN103796956B (en) * | 2011-09-15 | 2016-01-20 | 日本化学工业株式会社 | The manufacture method of barium titanium oxalate and the manufacture method of barium titanate |
| CN106380194A (en) * | 2016-08-31 | 2017-02-08 | 仙桃市中星电子材料有限公司 | Production technology of nanometer tetragonal barium titanate |
| CN113784927A (en) * | 2019-10-02 | 2021-12-10 | 株式会社Lg化学 | Method for preparing precursor of positive electrode active material for lithium secondary battery |
| US11855287B2 (en) | 2019-10-02 | 2023-12-26 | Lg Chem, Ltd. | Method of preparing positive electrode active material precursor for lithium secondary battery |
| CN110526286A (en) * | 2019-10-10 | 2019-12-03 | 重庆中坛洋铭化工科技有限公司 | A kind of environment-friendly and energy-efficient barium titanate production system and technique |
| CN110526286B (en) * | 2019-10-10 | 2024-04-26 | 重庆中坛洋铭化工科技有限公司 | Environment-friendly energy-saving barium titanate production system and process |
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