CN107855088A - A kind of efficient, intelligence reactive crystallization equipment - Google Patents
A kind of efficient, intelligence reactive crystallization equipment Download PDFInfo
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- CN107855088A CN107855088A CN201711387448.3A CN201711387448A CN107855088A CN 107855088 A CN107855088 A CN 107855088A CN 201711387448 A CN201711387448 A CN 201711387448A CN 107855088 A CN107855088 A CN 107855088A
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- reactive crystallization
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a kind of equipment that can efficiently, intelligently, accurately control reaction crystallization process, it includes：Agent set reactor, constant temperature water bath apparatus is provided with the outside of the agent set, feed arrangement is provided with the agent set top, agitating device, pH electrodes, conductance electrode are provided with the agent set top, the constant temperature water bath apparatus, feed arrangement, agitating device, pH electrodes and conductance electrode etc. are all connected with programmable logic controller (PLC) PLC automatic control system, automated intelligent control is realized, meanwhile, the granularity of product can be monitored in real time by online granulometry system.Overall structure of the present invention is simply clear, reaction crystallization process full-automatic measurement, feedback and control can be realized, artificial running cost and manual operation error are reduced, reaction crystallization process is carried out all the time under the reaction condition set, so as to ensure the quality of required product and stability.
Description
Technical field
The present invention relates to chemical reaction to crystallize automation control area, more particularly to a kind of reaction knot efficiently, intelligent
Crystalline substance equipment.Quality control available for reactive crystallization in chemical industry, advanced material and medical product.
Background technology
The core of lithium ion battery is positive electrode, however, positive electrode current material precursor is in prepare with scale mistake
The problems such as crystal tap density is small, size distribution is wide, pattern is defective, quality is unstable in journey be present, need to accurately monitor on-line,
The reaction conditions such as charging rate, temperature, pH, electrical conductivity, speed of agitator in auto-control reaction system, to reach accurate control
The reaction crystallization process of positive electrode material precursor.
It is entitled such as patent CN105183026B：A kind of automatic regulating system of crystallization reaction acid-base value, its feature
Including：The pH electrodes of crystallization reaction acid-base value in the retort are detected in real time；The acid-base value that the pH electrodes are detected is received,
And the ISM transmitters for presetting acid-base value threshold value are provided between the alkali lye secondary flow gauge and the retort, according to described
The magnetic valve of the instruction automatic shutter of ISM transmitters.
It is entitled such as patent CN103551100B：A kind of continuous fast reaction crystallization improves the dress of crystal stability
Put and method, its feature include：By two or more reaction solutions respectively from the different feeds tube pump of liquid jet impact feed arrangement
Enter, reaction solution is sprayed in a manner of the collision that liquidates from nozzle enters tank reactor, in tank reactor in a manner of complete mixing flow
Reaction nucleation is carried out, reaction solution flows into tubular reactor afterwards, and carry out crystal growth is flowed in a manner of laminar flow, then after
Handle the crystal product stablized.
And for example patent CN104881062B, it is entitled：It is a kind of quickly to be controlled without toning crystallisation by cooling temperature of reaction kettle
Method, its summary include：This method is added using refrigeration compressor, the electronics based on pulse width modulation power of variable ratio frequency changer regulation power
Heat pipe, programmable controller, monitoring computer construction temperature control system.It is anti-that crystallization can be quantitatively adjusted using the invention
Answer the rate of temperature fall of kettle solution, it is ensured that reach the cooling desired value specified without toning, so as to be carried for the cooling of crystallization processes regulation
For a kind of convenient and reliable automation control method.
Current reactive crystallization automaton be auto-control a certain item operating condition, such as pH, temperature, no
It can realize to all operationss condition on-line monitoring and automatically control.And realize the automatic control for so including all operationss condition
System, is not the simple superposition of these single condition controls, but the control of various conditions is organically combined, and avoids in different bars
Contradiction is produced in the control of part, and there is presently no the good control strategy of such a integrality.Importantly, in large arch dam
In rate, opaque reactive crystallization system can real-time monitored crystal morphology and measure Lens capsule equipment there is not yet
Arrive.
The content of the invention
For the existing reactive crystallization automaton a certain item operating condition that has been auto-control, and can not be in height
The deficiency of real-time monitored crystal morphology and granularity in solid holdup, opaque reactive crystallization system, the invention provides a kind of high
The reactive crystallization equipment of effect, intelligence, for monitoring and automatically controlling the charging rate of reaction crystallization process, temperature, pH, electricity on-line
The all operationss condition such as condensate flow inside and outside conductance, speed of agitator and kettle, and in high solid concentration, opaque hot-die system
The pattern and size distribution of middle on-line measurement crystal grain.
In order to solve the above problems, the invention provides following technical scheme：
A kind of efficient, intelligence reactive crystallization equipment, it is characterised in that including：
The reactor of reactive crystallization is carried out for saline solution, complex liquid, alkali lye and acid solution；
For keeping the constant temperature water bath apparatus of inside reactor constant temperature；
For the feed arrangement fed to reactor inside；
Agitating device for stirring inside reactor；
For detecting the pH measurement apparatus of reactive crystallization acid-base value in the reactor in real time；
For detecting the conductivity measuring apparatus of reactive crystallization electrical conductivity in the reactor in real time；
For automatically controlling the FPGA of the conditions such as the charging rate of reactive crystallization, temperature, pH, electrical conductivity, speed of agitator
Controller PLC automatic control system；
For monitoring the online granulometry system of reactive crystallization granularity and pattern on-line；
Saline solution needed for reactive crystallization, complex liquid, alkali lye and acid solution are sent into by tank reactor by feed arrangement, pass through constant temperature
Water bath device control temperature in the kettle keeps constant, reactant in kettle is sufficiently mixed uniformly by agitating device, is measured by pH
PH and electrical conductivity and PLC automatic control system is fed back in device and conductivity measuring apparatus measurement kettle, automatically controlled by PLC and be
The addition speed for auto-control saline solution, complex liquid, alkali lye and the acid solution of uniting, makes pH and electrical conductivity in kettle be maintained at suitable reactive crystallization
Condition, be sent into online grain after the pretreatment such as dilute, tile from the crystalline product of the overfall overflow of continuous production discharging
Measuring system is spent, to observe crystal size and pattern.
Further, the constant temperature water bath apparatus includes thermal resistance, water-bath chuck, circulating cooling water coil, circulating pump, kettle
Interior condenser tube.
Further, the peripherally disposed baffle plate of reactor inwall, baffle number are 2-8.
Further, the kettle interior condenser tube is combined into one with baffle plate.
Further, the feed arrangement includes material liquid tank and corresponding feed pump.
Further, the agitating device includes agitating paddle, belt, stirring motor and automatic speed measuring device.
Further, the pH measurement apparatus includes pH electrodes, electrode protection set and is connected with pH electrodes automatic aobvious
Show instrument etc., pH measurement ranges are 0-14.
Further, the conductivity measuring apparatus includes conductance electrode, electrode protection set and is connected with conductance electrode
Meter of Automatic Display.
Further, the automatic control control system and some feed pumps, pH electrodes, conductance electrode, thermal resistance, condenser pipe,
Stirring motor, online granulometry system etc. are connected.
Further, the online granulometry system includes high definition photographic system, measuring platform and supporting computer, and granularity is surveyed
It is 1-10000 μm to measure scope.
It is compared with the prior art, the present invention has advantages below：
It is provided by the invention it is a kind of efficiently, intelligence reactive crystallization equipment be a set of Automatic Control continuous production device, energy
Enough charging rates monitored on-line and regulate and control reactive crystallization, temperature, pH, electrical conductivity, speed of agitator, the operation such as condensed water inside and outside kettle
Condition, it is whole without manually operated.Meanwhile a kind of efficient, intelligence reactive crystallization equipment provided by the invention carries high-resolution
The photographic means of rate, can high solid concentration, it is nontransparent in the case of online observation product shape characteristic and size distribution
Situation, convenient adjustment operating parameter in time, to ensure crystal mass.So as to ensure reaction crystallization process all the time to the full extent
Carried out under stable reaction condition, generate good pattern, uniform particle sizes, the crystal of product stabilization.
Brief description of the drawings
Fig. 1 is the block schematic illustration of the present invention.
Fig. 2 is the structural representation of agent set of the present invention.
Wherein, 1 is salt flow container, and 2 be alkali liquid tank, and 3 be complexing flow container, and 4 be acid solution tank, and 5 be baffle plate, and 6 be agitating device, 7
It is pH electrodes for conductance electrode, 8,9 be constant temperature water bath apparatus, and 10 be reactor, and 11 be online granulometry system, and 12 be PLC
Automatic control system.
Embodiment
Embodiment one
Reaction bottom liquid is added in 10 L reactors, including 9.5 L pure water, by 6:2:The nickel sulfate of 2 molar ratio weighing,
Cobaltous sulfate and manganese sulfate solid totally 623 g, 0.3 L ammoniacal liquor and 192 g sodium hydrate solids etc..By 6:2:2 molar ratio
The mixing salt solution of nickel sulfate, cobaltous sulfate and manganese sulfate that concentration is 0.8 mol/L adds the mol/L of salt flow container 1,1.4 hydrogen-oxygen
Change the ammonia spirit addition complexing flow container 3 that sodium solution adds the mol/L of alkali liquid tank 2,1, compound concentration is that 1 mol/L sulfuric acid is molten
Liquid adds acid solution tank 4.The inwall of reactor 10 sets baffle plate 5, peripherally disposed 4, reduces the directed flow of liquid, strengthens
Turbulence.PLC automatic control system 12 is the Automatic Centering Control of whole device, and various operating parameters are received by front-end probe
Signal simultaneously provides respective feedback and is adjusted.Revolution speed is fed by controlling, to adjust charging rate.Can by conductance electrode 7
Realize that the charging rate of saline solution and complex liquid controls the electrical conductivity in kettle in automated intelligent control reactor 10, makes solution in kettle
It is maintained at the degree of supersaturation for being adapted to crystallization.Similarly, the charging rate of acid solution and alkali lye is automatically controlled by pH electrodes 8 to control
It is 10.5 that pH is constant in reactor 10, and control accuracy is ± 0.02.The kettle interior condenser tube being arranged on inside baffle plate 5 can be to reactor
Material temperature controlling in 10, the temperature runaway of liquid is prevented, using also including thermal resistance, water-bath chuck, circulating cooling water coil and circulating pump
Constant temperature water bath apparatus 9 accurately control reactor temperature be 50oC, temperature-controlled precision are ± 0.1oC.Agitating device 6 is set
Speed of agitator is 700 r/min, and the actual speed of agitating paddle is measured with hall principle.It can be read in real time by Meter of Automatic Display
Take rotating speed, temperature, electrical conductivity, pH numerical value.From the product of the overfall outflow of continuous production discharging, through over sampling, dilution, put down
Online granulometry system 11 is put into after the pretreatment such as paving to be taken pictures, analyzed, so as to realize the online survey of Lens capsule
Amount, then feeds back to PLC automatic control system 12, according to the intelligent control for establishing control strategy and carrying out in real time operating parameter, makes
Particle size range is at 10-100 μm.
Embodiment two
In 2 m3Reaction bottom liquid is added in reactor, including 1940 L pure water, by 8:1:The sulfuric acid of 1 molar ratio weighing
Nickel, cobaltous sulfate and manganese sulfate solid totally 124.6 kg, 60 L ammoniacal liquor and 38.4 kg sodium hydrate solids etc..By 8:1:1 mole
Mixing salt solution than nickel sulfate, cobaltous sulfate and manganese sulfate that compound concentration is 0.8 mol/L adds the mol/L of salt flow container 1,1.4
Sodium hydroxide solution add alkali liquid tank 2,1 mol/L ammonia spirit and add complexing flow container 3, compound concentration is 1 mol/L's
Sulfuric acid solution adds acid solution tank 4.The inwall of reactor 10 sets baffle plate 5, peripherally disposed 8, reduces the oriented flow of liquid
It is dynamic, strengthen turbulence.PLC automatic control system 12 is the Automatic Centering Control of whole device, and various behaviour are received by front-end probe
Make the signal of parameter and provide respective feedback to be adjusted.Revolution speed is fed by controlling, to adjust charging rate.Pass through conductance
Electrode 7, which can be realized, automatically controls in reactor 10 charging rate of saline solution and complex liquid to control the electrical conductivity in kettle, makes in kettle
Solution is maintained at the degree of supersaturation for being adapted to crystallization.Similarly, automatically controlled by pH electrodes 8 charging rate of acid solution and alkali lye come
It is 11.5 that pH is constant in control reactor 10, and control accuracy is ± 0.02.The kettle interior condenser tube being arranged on inside baffle plate 5 can be to anti-
Material temperature controlling in kettle 10 is answered, prevents the temperature runaway of liquid, using also including thermal resistance, water-bath chuck, circulating cooling water coil and follow
It is 75 that the constant temperature water bath apparatus 9 of ring pump, which accurately controls reactor temperature,oC, temperature-controlled precision are ± 0.1oC.Agitating device is set
6 speed of agitator is 900 r/min, and the actual speed of agitating paddle is measured with hall principle.Can be real by Meter of Automatic Display
When read rotating speed, temperature, electrical conductivity, pH numerical value.From the product of the overfall outflow of continuous production discharging, through over sampling, dilute
Release, tile etc. and being put into online granulometry system 11 after pretreatment and taken pictures, analyzed, so as to realize Lens capsule
Line measure, then feed back to PLC automatic control system 12, according to establish control strategy carry out in real time operating parameter intelligence control
System, makes particle size range at 10-100 μm.
Overall structure of the present invention is simply clear, can realize the full-automatic intelligent control of reaction crystallization process, reduces people
Work running cost and manual operation error, reaction crystallization process is set to be carried out all the time under the reaction condition set, so as to ensure
The quality and stability and continuity of product.
A kind of efficient, intelligence reactive crystallization equipment provided by the present invention is described in detail above.Herein
Apply specific case to be set forth embodiments of the present invention, the explanation of above example is only intended to help and understands this
The core concept of invention.It should be pointed out that for those skilled in the art, the principle of the invention is not being departed from
Under the premise of, some improvements and modifications can also be made, these improvements and modifications also should be regarded as protection scope of the present invention, this implementation
The available prior art of each part being not known in example is realized.
Claims (10)
- A kind of 1. efficient, intelligence reactive crystallization equipment, it is characterised in that including：The reactor of reactive crystallization is carried out for saline solution, complex liquid, alkali lye and acid solution；For keeping the constant temperature water bath apparatus of constant temperature inside reactor；For the feed arrangement fed to reactor inside；Agitating device for stirring inside reactor；For detecting the pH measurement apparatus of reactive crystallization acid-base value in the reactor in real time；For detecting the conductivity measuring apparatus of reactive crystallization electrical conductivity in the reactor in real time；For automatically controlling the FPGA of the conditions such as the charging rate of reactive crystallization, temperature, pH, electrical conductivity, speed of agitator Controller PLC automatic control system；For monitoring the online granulometry system of reactive crystallization granularity and pattern on-line；Saline solution needed for reactive crystallization, complex liquid, alkali lye and acid solution are sent into by tank reactor by feed arrangement, pass through constant temperature Water bath device control temperature in the kettle keeps constant, reactant in kettle is sufficiently mixed uniformly by agitating device, is measured by pH PH and electrical conductivity and PLC automatic control system is fed back in device and conductivity measuring apparatus measurement kettle, automatically controlled by PLC and be The addition speed for auto-control saline solution, complex liquid, alkali lye and the acid solution of uniting, makes pH and electrical conductivity in kettle be maintained at suitable reactive crystallization Condition, from continuous production discharging overfall overflow crystalline product through over sampling, dilution, tiling etc. pre-process after be fed in Line granulometry system, to observe crystal size and pattern.
- 2. efficient, intelligence reactive crystallization equipment according to claim 1, it is characterised in that the constant temperature water bath apparatus Including thermal resistance, water-bath chuck, circulating cooling water coil, circulating pump, kettle interior condenser tube.
- 3. efficient, intelligence reactive crystallization equipment according to claim 1, it is characterised in that the reactor inwall edge Circumferencial direction sets baffle plate, and baffle number is 2-8.
- 4. efficient, the intelligent reactive crystallization equipment according to Claims 2 or 3, it is characterised in that the kettle interior condenser tube It is combined into one with baffle plate.
- 5. efficient, intelligence reactive crystallization equipment according to claim 1, it is characterised in that the feed arrangement includes Material liquid tank and corresponding feed pump.
- 6. efficient, intelligence reactive crystallization equipment according to claim 1, it is characterised in that the agitating device includes Agitating paddle, belt, stirring motor and automatic speed measuring device.
- 7. efficient, intelligence reactive crystallization equipment according to claim 1, it is characterised in that the pH measurement apparatus bag PH electrodes, electrode protection set and Meter of Automatic Display for being connected with pH electrodes etc. are included, pH measurement ranges are 0-14.
- 8. efficient, intelligence reactive crystallization equipment according to claim 1, it is characterised in that the conductivity measurement dress Put including conductance electrode, electrode protection set and the Meter of Automatic Display being connected with conductance electrode.
- 9. efficient, intelligence reactive crystallization equipment according to claim 1, it is characterised in that the automatic control control system It is connected with some feed pumps, pH electrodes, conductance electrode, thermal resistance, condenser pipe, stirring motor, online granulometry system etc..
- 10. efficient, intelligence reactive crystallization equipment according to claim 1, it is characterised in that the online granulometry System includes high definition photographic system, measuring platform and supporting computer, and granulometry scope is 1-10000 μm.
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| CN201711387448.3A CN107855088A (en) | 2017-12-20 | 2017-12-20 | A kind of efficient, intelligence reactive crystallization equipment |
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| CN201711387448.3A CN107855088A (en) | 2017-12-20 | 2017-12-20 | A kind of efficient, intelligence reactive crystallization equipment |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203114A (en) * | 2018-04-11 | 2018-06-26 | 宜春市鼎鑫高能科技有限公司 | A kind of system of brine crystallization lithium carbonate suitable for industrial automation production |
| CN108745252A (en) * | 2018-07-09 | 2018-11-06 | 北京市计量检测科学研究院 | A kind of micro Nano material preparation facilities |
| CN108905262A (en) * | 2018-06-12 | 2018-11-30 | 崇义章源钨业股份有限公司 | The system and method for ammonium para-tungstate crystal automation control |
| CN109116893A (en) * | 2018-09-30 | 2019-01-01 | 镇江华智睿安物联科技有限公司 | A kind of width Cheng Wendu is adjusted and the device of pH measurement |
| CN109187854A (en) * | 2018-08-10 | 2019-01-11 | 中国原子能科学研究院 | The measuring method of reaction solution extension rate when studying ionic crystal reaction nucleation rate |
| CN109182742A (en) * | 2018-09-28 | 2019-01-11 | 中国恩菲工程技术有限公司 | Rare-earth precipitation device |
| CN109187641A (en) * | 2018-08-10 | 2019-01-11 | 中国原子能科学研究院 | A kind of device of research ionic crystal reaction nucleation kinetics |
| CN109942655A (en) * | 2019-04-29 | 2019-06-28 | 宜昌东阳光药业股份有限公司 | A kind of continuous crystallisation process of erythromycin thiocyanate crude product |
| CN110160919A (en) * | 2019-07-04 | 2019-08-23 | 中国科学院青岛生物能源与过程研究所 | A kind of on-line measurement device of grain graininess and pattern |
| CN111154827A (en) * | 2020-01-22 | 2020-05-15 | 金河生物科技股份有限公司 | Method for producing oxytetracycline |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203114A (en) * | 2018-04-11 | 2018-06-26 | 宜春市鼎鑫高能科技有限公司 | A kind of system of brine crystallization lithium carbonate suitable for industrial automation production |
| CN108905262A (en) * | 2018-06-12 | 2018-11-30 | 崇义章源钨业股份有限公司 | The system and method for ammonium para-tungstate crystal automation control |
| CN108745252A (en) * | 2018-07-09 | 2018-11-06 | 北京市计量检测科学研究院 | A kind of micro Nano material preparation facilities |
| CN109187854A (en) * | 2018-08-10 | 2019-01-11 | 中国原子能科学研究院 | The measuring method of reaction solution extension rate when studying ionic crystal reaction nucleation rate |
| CN109187641A (en) * | 2018-08-10 | 2019-01-11 | 中国原子能科学研究院 | A kind of device of research ionic crystal reaction nucleation kinetics |
| CN109182742A (en) * | 2018-09-28 | 2019-01-11 | 中国恩菲工程技术有限公司 | Rare-earth precipitation device |
| CN109116893A (en) * | 2018-09-30 | 2019-01-01 | 镇江华智睿安物联科技有限公司 | A kind of width Cheng Wendu is adjusted and the device of pH measurement |
| CN109942655A (en) * | 2019-04-29 | 2019-06-28 | 宜昌东阳光药业股份有限公司 | A kind of continuous crystallisation process of erythromycin thiocyanate crude product |
| CN109942655B (en) * | 2019-04-29 | 2020-05-12 | 宜昌东阳光药业股份有限公司 | Continuous crystallization method of erythromycin thiocyanate crude product |
| CN110160919A (en) * | 2019-07-04 | 2019-08-23 | 中国科学院青岛生物能源与过程研究所 | A kind of on-line measurement device of grain graininess and pattern |
| CN111154827A (en) * | 2020-01-22 | 2020-05-15 | 金河生物科技股份有限公司 | Method for producing oxytetracycline |
| CN111154827B (en) * | 2020-01-22 | 2021-11-05 | 金河生物科技股份有限公司 | Method for producing oxytetracycline |
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Effective date of registration: 20180809 Address after: 266101 Songling Road, Laoshan District, Qingdao, Shandong Province, No. 189 Applicant after: QINGDAO INSTITUTE OF BIOENERGY AND BIOPROCESS TECHNOLOGY, CHINESE ACADEMY OF SCIENCES Applicant after: Institute of Process Engineering, Chinese Academy of Sciences Address before: 266101 Songling Road, Laoshan District, Qingdao, Shandong Province, No. 189 Applicant before: Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences |
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