CN101434407A - Process for continuously preparing barium titanate powder - Google Patents
Process for continuously preparing barium titanate powder Download PDFInfo
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- CN101434407A CN101434407A CNA2008101393623A CN200810139362A CN101434407A CN 101434407 A CN101434407 A CN 101434407A CN A2008101393623 A CNA2008101393623 A CN A2008101393623A CN 200810139362 A CN200810139362 A CN 200810139362A CN 101434407 A CN101434407 A CN 101434407A
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Abstract
The invention provides a production process for continually producing barium titanate, which comprises the steps of preparing pure water, confecting a titanium oxychloride solution, confecting and washing a precursor, and starting a tubular continuous synthesis reactor to continuously produce, wash and dry the barium titanate, and the like. Being continuously carried out, the production process has the advantages of doubling the output within unit time, improving energy utilization, saving energy, reducing thermal energy consumption by 30-40, and lowering cost. The barium titanate products with different specifications can be obtained from the synthesized product after being calcined at 900-1050 DEG C, thus completely reaching the quality level of the batch-type products.
Description
Technical field:
The present invention relates to a kind of production work of producing the chemical barium titanate, especially a kind of production technique of tubular type continuous production barium titanate.
Background technology:
Liquid phase method synthesis of barium titanate technology has possessed the production technique of comparative maturity, carries out intermittent production in the synthesis reactor but present production technique is based on.Intermittent production advantage is: the equipment structure is independent simple, easy control easy and simple to handle, and operating skill requires low, industrialization easily.Shortcoming is that labour intensity is big, and energy consumption height, energy utilization rate are low, yields poorly, and processing parameter fluctuation religion affected by environment is big, and product performance fluctuate thereupon.Along with the increase of social production to the demand of barium titanate, take measures to improve output, reduce energy consumption, stability, has important economic implications, along with the growing tension save energy of the energy also has important economic and social benefit, reducing labour intensity in addition and improve work situation, is human a kind of pursuit in productive labor.Successive reaction can satisfy this requirement on certain degree, we have made for this reason, continuously synthesis reactor.The advantage of building-up reactions is that production is continuous, energy utilization rate is high, energy consumption is low continuously, the output height, and labour intensity is low.It is high that its shortcoming is that operating skill requires, in case the break down product rejection or the defective material that cause are many, and equipment structure more complicated.Along with social production to the increase of the demand of barium titanate and production technology constantly improve and progressive, continous way produces that to replace batch production be a kind of inevitable trend.
Summary of the invention:
The object of the present invention is to provide a kind of production technique of continuous production barium titanate.
The object of the present invention is achieved like this:
(1) preparation pure water: utilize the prior art for preparing pure water, water conductivity≤0.5 μ s/cm;
(2) preparation dichloro oxygen titanium solution: pure water is added to enamel still, with the water cycle cooling, adds titanium tetrachloride while stirring, and solution temperature is less than 55 ℃, and compound concentration per-cent is 23---32% dichloro oxygen titanium solution;
(3) presoma preparation: pure water is added to enamel still, and not stirring down adding concentration is 10
-20% ammonia soln stirs the dichloro oxygen titanium solution that adds step (2) gained down, and the control feed rate is 10-20 minute/liter; Add pure water, stirred 10 minutes.
(4) washing of presoma: the presoma of step (2) gained is by volume diluted a times, be transported in the band filter and filter, all filter to slurry;
(5) add pure water in the dosing enamel still, washed presoma is gone on the limit while stirring, adds barium hydroxide, adds titanium mole number 0.3
-0.5% auxiliary agent polyoxyethylene glycol adds pure water, stirs, and is delivered to the buffer storage jar, prepares synthetic;
(6) start the continuous synthesis reactor of tubular type, hot spots is a double-pipe exchanger, set 180-250 ℃ of heat conductive oil inlet temperature, 160-200 ℃ of thermal oil temperature out, the temperature out of slurry is 130-160 ℃, insulating sections is the tubular type warmer, and holding temperature 130-160 ℃, the cooling part is a double-pipe exchanger, 60-110 ℃ of heat conductive oil inlet temperature, 100-130 ℃ of thermal oil temperature out
(7) the material-handling pump opening for feed is transformed into the buffer storage jar, and first blended slurry enters into the continuous synthesis reactor of tubular type; The flow of setting material-handling pump makes material stop 150-300 minute at insulating sections; Product is collected in the still that connects material;
(8) washing: venting mother liquor after about for some time of sedimentation in the still that connects material pumps into the washing of washing still; Add an amount of pure water, stir and stopped stirring sedimentation in 10 minutes, after sedimentation for some time, venting upper strata waste liquid; Like this repetitive scrubbing is 1.000 ± 0.003 qualified until material washing barium titanium mol ratio;
(9) drying: with drying machine material is carried out drying, control input concentration 20-30%, temperature out 120-150 ℃.
Synthesis reactor mainly contains five parts composition continuously: the one, and material-handling pump; The 2nd, hot spots---double-pipe exchanger and auxiliary equipment thereof, the 3rd, insulating sections---tubular type insulating sections and magnetic stirring apparatus and their auxiliary equipment; The 4th, cooling part double-pipe exchanger and auxiliary equipment thereof; The 5th, still connects material.
Being characterized as of products obtained therefrom:
(1) particle diameter 0.05-0.150um, the narrow particle size distribution globulate;
(2) crystallinity is good, has a cube phase perovskite structure;
(3)Ba/Ti＝1.000±0.003；
(4)SSA＝6-18m2/g；
(5) has good sintering activity.
Advantage compared with prior art of the present invention has: production process is carried out continuously, has improved the output in the unit time, can improve more than 1 times; Improve energy utilization rate, save energy, can reduce 30-40 heat energy consumption, reduce cost.The 900-1050 ℃ of calcining of product process that synthesizes can obtain the barium titanate product of different size, can reach the intermittent type product quality level fully.
Description of drawings:
Fig. 1 is embodiment 1 a gained barium titanate stereoscan photograph;
Fig. 2 is embodiment 1 a gained barium titanate XRD diffractogram;
Fig. 3 is embodiment 2 gained barium titanate stereoscan photographs;
Fig. 4 is embodiment 2 gained barium titanate XRD diffractograms;
Fig. 5 is the double-pipe exchanger structural representation.
Embodiment:
(1) preparation pure water: utilize the prior art for preparing pure water, water conductivity≤0.5 μ s/cm;
(2) preparation dichloro oxygen titanium solution: pure water is added to enamel still, with the water cycle cooling, adds titanium tetrachloride while stirring, and solution temperature is less than 55 ℃, and compound concentration per-cent is 23---32% dichloro oxygen titanium solution;
(3) presoma preparation: pure water is added to enamel still, and not stirring down adding concentration is 10
-20% ammonia soln stirs the dichloro oxygen titanium solution that adds step (2) gained down, and the control feed rate is 10-20 minute/liter; Add pure water, stirred 10 minutes.
(4) washing of presoma: the presoma of step (2) gained is by volume diluted a times, be transported in the band filter and filter, all filter to slurry;
(5) add pure water in the dosing enamel still, washed presoma is gone on the limit while stirring, adds barium hydroxide, adds titanium mole number 0.3
-0.5% auxiliary agent polyoxyethylene glycol adds pure water, stirs, and is delivered to the buffer storage jar, prepares synthetic;
(6) start the continuous synthesis reactor of tubular type, hot spots is a double-pipe exchanger, set 180-250 ℃ of heat conductive oil inlet temperature, 160-200 ℃ of thermal oil temperature out, the temperature out of slurry is 130-160 ℃, insulating sections is the tubular type warmer, and holding temperature 130-160 ℃, the cooling part is a double-pipe exchanger, 60-110 ℃ of heat conductive oil inlet temperature, 100-130 ℃ of thermal oil temperature out
(7) the material-handling pump opening for feed is transformed into the buffer storage jar, and first blended slurry enters into the continuous synthesis reactor of tubular type; The flow of setting material-handling pump makes material stop 150-300 minute at insulating sections; Product is collected in the still that connects material;
(8) washing: venting mother liquor after about for some time of sedimentation in the still that connects material pumps into the washing of washing still; Add an amount of pure water, stir and stopped stirring sedimentation in 10 minutes, after sedimentation for some time, venting upper strata waste liquid; Like this repetitive scrubbing is 1.000 ± 0.003 qualified until material washing barium titanium mol ratio;
(9) drying: with drying machine material is carried out drying, control input concentration 20-30%, temperature out 120-150 ℃.
Produce the technical parameter of 1 ton of continuous tubular type synthesis reactor of barium titanate daily.
1) add the 400kg pure water in the enamel still, not stirring down the concentration that adds 550Kg is 10% ammonia soln, stirs down 25.72% the dichloro oxygen titanium solution 424.8Kg that requires weight with the accurate metering process of electronic scales, controls feed rate 10-20 minute.1600 liters of moisturizings were stirred 10 minutes.
2) the presoma dilution is one times above, is transported in the band filter and filters, and all filters until slurry to finish.
3) pure water of adding 200Kg in the liquid enamel still under agitation, adds washed presoma, and the barium hydroxide of accurate weighing 230kg, adding 6.9Kg concentration is 10% polyoxyethylene glycol, all the other replenish 800 liters with pure water, stir, be delivered to the buffer storage jar, prepare synthetic;
4) go up process and carry out continuously, and will guarantee that the buffer storage jar can not be sky, uninterruptedly carry out to guarantee continuous synthetic.
5) moving continuous synthesis reactor: 245 liters/hour of the flows of the first blended material-handling pump of setting; Set 130 ℃ of tubular type tubular heat exchanger slurry outlet temperature, set 180 ℃ of thermal oil temperature inlet temperatures, 165 ℃ of thermal oil temperature temperature outs, 130 ℃ of holding temperatures; With pure water (replacing mixture just) trial run, that following parameter regulation is stable;
6) the transferpump opening for feed is transformed into the buffer storage jar, and first blended slurry enters into the continuous synthesis reactor of tubular type; Adjust the setup parameter above meeting according to flow, temperature variation;
7) stablize and deposited separately with interior product in back 4 hours, later product was collected among connect material still 1# and the 2# in 4 hours;
8) performance index: the one section quality of getting the material testing product in every interval at discharge port, detecting index has slurry concentration, pH value, Ba/Ti, SSA;
9) the about venting mother liquor after for some time of sedimentation in the still that connects material pumps into the washing of washing still; Add an amount of pure water, stir and stopped stirring sedimentation in 10 minutes, after sedimentation for some time, venting upper strata waste liquid; Like this repetitive scrubbing is 1.000 ± 0.003 qualified until material washing barium titanium mol ratio;
10) with drying machine material is carried out drying: control input concentration 20-30%, temperature out 120-150 ℃;
11) packing of sieving;
12) product detects
| Ba/Ti | Chlorion | SSA | Granule-morphology | XRD detects |
| 0.9998 | 260 | 20.58 | As Fig. 1 | As Fig. 2 |
Embodiment 2
1) add the 400kg pure water in enamel still, not stirring down the concentration that adds 370.5Kg is 20% ammonia soln, stirs down 31.97% the dichloro oxygen titanium solution 242.8Kg that requires weight with the accurate metering process of electronic scales, controls feed rate 10-20 minute.1600 liters of moisturizings were stirred 10 minutes;
2) with one times of top presoma dilution, be transported in the band filter and filter, finish until whole filtration of slurry;
3) pure water of adding 200Kg in the dosing enamel still under agitation, adds washed presoma, and the barium hydroxide of accurate weighing 235.5kg, adding 7.7Kg concentration is 15% polyoxyethylene glycol, all the other replenish 800 liters with pure water, stir, be delivered to the buffer storage jar, prepare synthetic;
4) above process is carried out continuously, and will guarantee that the buffer storage jar can not be sky, uninterruptedly carries out to guarantee continuous synthetic;
5) start continuous synthesis reactor: 327 liters/hour of the flows of the first blended material-handling pump of setting; Set 150 ℃ of tubular type tubular heat exchanger slurry outlet temperature, set 215 ℃ of thermal oil temperature inlet temperatures, 185 ℃ of thermal oil temperature temperature outs, 150 ℃ of holding temperatures; With pure water (replacing mixture just) trial run, above-mentioned parameter is regulated stable:
6) the material-handling pump opening for feed is transformed into the buffer storage jar, and first blended slurry enters into the continuous synthesis reactor of tubular type; Adjust the setup parameter above meeting according to flow, temperature variation;
7) deposited separately with interior product in 3 hours behind the parameter stability, later product was collected among connect material still 1# and the 2# in 3 hours;
8) detect performance index: the one section quality of getting the material testing product in every interval at discharge port, detecting index has slurry concentration, pH value, Ba/Ti, SSA;
9) washing: venting mother liquor after about for some time of sedimentation in the still that connects material pumps into the washing of washing still; Add an amount of pure water, stir and stopped stirring sedimentation in 10 minutes, after sedimentation for some time, venting upper strata waste liquid; Like this repetitive scrubbing is 1.000 ± 0.003 qualified until material washing barium titanium mol ratio;
10) drying: material is carried out drying: control input concentration 20-30%, temperature out 120-150 ℃ with drying machine;
11) packing of sieving;
12) product detects
| Ba/Ti | Chlorion | SSA | Granule-morphology | XRD detects |
| 1.0005 | 280 | 18.34 | As Fig. 3 | As Fig. 4 |
Claims (3)
1, a kind of technology of continuous preparation barium carbonate powder comprises: the preparation pure water, and obtain solution, continuous resulting solution, divides grade packagedly at washing, it is characterized in that:
(1) preparation pure water: utilize the prior art for preparing pure water, water conductivity≤0.5 μ s/cm;
(2) preparation dichloro oxygen titanium solution: pure water is added to enamel still, with the water cycle cooling, adds titanium tetrachloride while stirring, and solution temperature is less than 55 ℃, and compound concentration per-cent is 23---32% dichloro oxygen titanium solution;
(3) presoma preparation: pure water is added to enamel still, and not stirring down adding concentration is 10-20% ammonia soln, stirs the dichloro oxygen titanium solution that adds step (2) gained down, and the control feed rate is 10-20 minute/liter; Add pure water, stirred 10 minutes;
(4) washing of presoma: the presoma of step (2) gained is by volume diluted a times, be transported in the band filter and filter, all filter to slurry;
(5) add pure water in the dosing enamel still, washed presoma is gone on the limit while stirring, adds barium hydroxide, adds titanium mole number 0.3-0.5% auxiliary agent polyoxyethylene glycol, adds pure water, stirs, and is delivered to the buffer storage jar, prepares synthetic;
(6) start the continuous synthesis reactor of tubular type, hot spots is a double-pipe exchanger, set 180-250 ℃ of heat conductive oil inlet temperature, 160-200 ℃ of thermal oil temperature out, the temperature out of slurry is 130-160 ℃, insulating sections is the tubular type warmer, holding temperature 130-160 ℃, the cooling part is a double-pipe exchanger, 60-110 ℃ of heat conductive oil inlet temperature, 100-130 ℃ of thermal oil temperature out;
(7) the material-handling pump opening for feed is transformed into the buffer storage jar, and first blended slurry enters into the continuous synthesis reactor of tubular type; The flow of setting material-handling pump makes material stop 150-300 minute at insulating sections; Product is collected in the still that connects material;
(8) washing: venting mother liquor after about for some time of sedimentation in the still that connects material pumps into the washing of washing still; Add an amount of pure water, stir and stopped stirring sedimentation in 10 minutes, after sedimentation for some time, venting upper strata waste liquid; Like this repetitive scrubbing is 1.000 ± 0.003 qualified until material washing barium titanium mol ratio;
(9) drying: with drying machine material is carried out drying, control input concentration 20-30%, temperature out 120-150 ℃.
2, the technology of a kind of continuous preparation barium carbonate powder according to claim 1 is characterized in that: above process is carried out continuously, and will guarantee that the buffer storage jar can not be sky, uninterruptedly carries out to guarantee continuous synthetic.
3, the technology of a kind of continuous preparation barium carbonate powder according to claim 1 is characterized in that: synthesis reactor mainly contains five parts composition continuously: the one, and material-handling pump; The 2nd, hot spots---double-pipe exchanger and auxiliary equipment thereof, the 3rd, insulating sections---tubular type insulating sections and magnetic stirring apparatus and their auxiliary equipment; The 4th, cooling part double-pipe exchanger and auxiliary equipment thereof; The 5th, still connects material.
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| CN2008101393623A CN101434407B (en) | 2008-09-01 | 2008-09-01 | Process for continuously preparing barium titanate powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746814A (en) * | 2009-12-21 | 2010-06-23 | 山东国瓷功能材料有限公司 | Production technology for preparing tetragonal phase barium titanate powder |
| CN103058271A (en) * | 2012-12-20 | 2013-04-24 | 济南裕兴化工有限责任公司 | Connection device of film-coating process and washing process in titanium dioxide production |
| CN105836794A (en) * | 2016-04-22 | 2016-08-10 | 广东风华高新科技股份有限公司 | Preparation method of barium titanate powder |
| CN110040770A (en) * | 2019-06-10 | 2019-07-23 | 北京石油化工学院 | A kind of method that microchannel continuity method prepares nano-level sphere barium titanate |
| CN110040771A (en) * | 2019-06-10 | 2019-07-23 | 北京石油化工学院 | A kind of preparation method of submicron order spherical shape barium titanate particles |
-
2008
- 2008-09-01 CN CN2008101393623A patent/CN101434407B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746814A (en) * | 2009-12-21 | 2010-06-23 | 山东国瓷功能材料有限公司 | Production technology for preparing tetragonal phase barium titanate powder |
| CN103058271A (en) * | 2012-12-20 | 2013-04-24 | 济南裕兴化工有限责任公司 | Connection device of film-coating process and washing process in titanium dioxide production |
| CN105836794A (en) * | 2016-04-22 | 2016-08-10 | 广东风华高新科技股份有限公司 | Preparation method of barium titanate powder |
| CN110040770A (en) * | 2019-06-10 | 2019-07-23 | 北京石油化工学院 | A kind of method that microchannel continuity method prepares nano-level sphere barium titanate |
| CN110040771A (en) * | 2019-06-10 | 2019-07-23 | 北京石油化工学院 | A kind of preparation method of submicron order spherical shape barium titanate particles |
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| CN101434407B (en) | 2011-04-13 |
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Inventor after: Song Xibin Inventor after: Zhang Bing Inventor after: Zhang Xi Inventor before: Zhang Bing Inventor before: Chen Shichun Inventor before: Zhang Peng Inventor before: Ying Hong Inventor before: Wu Suwen |
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Free format text: CORRECT: INVENTOR; FROM: ZHANG BING CHEN SHICHUN ZHANG PENG YING HONG WU SUWEN TO: SONG XIBIN ZHANGBING ZHANG XI |
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