CN105664521A - Dynamic crystallization equipment and dynamic crystallization method - Google Patents

Dynamic crystallization equipment and dynamic crystallization method Download PDF

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Publication number
CN105664521A
CN105664521A CN201610107401.6A CN201610107401A CN105664521A CN 105664521 A CN105664521 A CN 105664521A CN 201610107401 A CN201610107401 A CN 201610107401A CN 105664521 A CN105664521 A CN 105664521A
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Prior art keywords
crystallization
liquid
kettle
crystallization kettle
dynamic
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CN201610107401.6A
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CN105664521B (en
Inventor
侯红军
杨华春
李云峰
薛旭金
闫春生
张永明
晁金伟
贾棉
贾蕾蕾
王艳君
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Duofudo New Material Co.,Ltd.
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Duo Fluoride Chemicals Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • B01D9/0009Crystallisation cooling by heat exchange by direct heat exchange with added cooling fluid

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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses dynamic crystallization equipment and a dynamic crystallization method. The dynamic crystallization equipment comprises a crystallization kettle, wherein a kettle outside circulation channel is arranged outside the crystallization kettle and is used for realizing circulation flow of to-be-crystallized liquid inside and outside the kettle; the kettle outside circulation channel is provided with two liquid absorbing inlets or more, and the liquid absorbing inlets are connected to parts, with different heights, of the crystallization kettle, and are used for realizing the circulation flow of the to-be-crystallized liquid at the parts with different heights. According to the dynamic crystallization equipment, by arranging liquid sucking points with different heights, good circulation flow and mixing of the to-be-crystallized liquid in the crystallization kettle can be realized in the initial stage of crystallization, and crystal nucleuses uniform in size can be formed favorably; in the later stage of crystallization, crystal particles gather at the middle-lower part of the crystallization kettle, and closing lower circulation can be selected, so that the liquid circulates at the middle-upper part of the crystallization kettle, thus the fine crystal particles can continuously grow, and finally crystal particles uniform in particle size and complete in crystal form are obtained.

Description

A kind of dynamic crystallization equipment and dynamic crystallization method
Technical field
The invention belongs to technical field of chemical, be specifically related to a kind of dynamic crystallization equipment and dynamic crystallization method.
Background technology
For the crystallization process of solvent method, traditional stationary crystallization, owing to process is wayward, the crystal grain formed is bigger, solvent and solute form complex and can be covered by the crystal of product, be difficult to eliminate, reduce product purity in follow-up heat drying process; Crystallization for lithium hexafluoro phosphate, the industrialized preparing process of current lithium hexafluoro phosphate mostly is Fluohydric acid. solvent method, obtains with lithium hexafluoro phosphate for solute, and Fluohydric acid. is the lithium hexafluorophosphate solution of solvent, the crystallization process of lithium hexafluorophosphate solution, has material impact to the quality of final products. Traditional stationary crystallization method, the product after crystallize easily forms bulk entirety, peels off and follow-up broken difficulty, be not only difficult to obtain even-grained product, and be readily incorporated impurity from partial crystallization groove. Stirring and crystallizing relatively stationary crystallization has better effect, and stirring can improve crystal nucleation and growth rate; But the crystal obtained by the mode of stirring and crystallizing is relatively big, and crystal growth granule is uneven, and can not stop crystallization wall built-up, meanwhile, mixing speed controls improper meeting and causes the shearing-crushing of crystal, affects the product quality of crystallization.
CN201930572U discloses a kind of continuous vacuum cooling crystallizing device, including wrapping the crystallizer being provided with cooling jacket, be connected with crystallizer by overlapping the pumped vacuum systems that steam jet ejector and condenser are constituted more, and one end is connected with the bottom of crystallizer, the circulating line that the other end is connected with the middle part of crystallizer. This device, by the low temperature in maintenance crystallizer and low pressure, enables solvent to be prone to remove under the cryogenic conditions of applicable solution crystallization, improves precipitation and the speed of growth of crystal. Utilizing the crystallization process that this device carries out, temperature-fall period evaporates with solvent, and crystallization solution is in thermodynamic instability state all the time, is unfavorable for nucleation and the uniform growth of crystal; Meanwhile, for the crystalloid solution of nonaqueous solvent, the solvent of this device contains large quantity of moisture after steam jet ejector reclaims, it is impossible to directly using as nonaqueous solvent, follow-up removal process adds production cost; Liquid to be crystallized is when bottom and middle part are circulated flowing, and Efficient Cycle amount is little, and mobility and Combination that liquid to be crystallized is overall are affected by restriction, it is difficult to obtain even-grained crystal.
Summary of the invention
It is an object of the invention to provide a kind of dynamic crystallization equipment, thus solving in prior art, the crystallization process of solvent method, mobility and the Combination of liquid to be crystallized are limited, it is difficult to the problem obtaining epigranular crystal.
Second purpose of the present invention is to provide a kind of dynamic crystallization method.
In order to realize object above, the technical solution adopted in the present invention is:
A kind of dynamic crystallization equipment, including crystallization kettle, crystallization kettle is externally provided with still outer circulation passage and flows at still inner-outer circulation for realizing liquid to be crystallized; Described still outer circulation passage is provided with two or more liquid sucting port, and liquid sucting port is connected on the differing heights of crystallization kettle, for realizing circulating of differing heights place liquid to be crystallized.
Dynamic crystallization equipment provided by the present invention, the system internal circulation flow that liquid to be crystallized forms with still outer circulation passage in crystallization kettle, setting by differing heights entry point, liquid to be crystallized in crystallization kettle can be made to realize good circulating and mix at the crystallization initial stage, advantageously form nucleus of uniform size; Along with the carrying out of crystallization, the rate of circulating flow of liquid to be crystallized can be slowed down, the basis of the good mixed performance of system makes crystal homoepitaxial; Phase after crystallisation, crystal grain is enriched with in crystallization kettle middle and lower part, optional closes bottom circulation, makes liquid circulate in middle and upper part, such that it is able to make fine crystals granule continued growth, finally gives epigranular, crystal grain that crystal formation is complete.
Further, at least it is connected to described liquid sucting port in the upper, middle and lower of crystallization kettle. The setting of high, medium and low three grades of entry points, it is possible to form upper, middle and lower-ranking circulating line, the mobility of material and Combination better, create good external environment condition for obtaining even-grained crystal grain. Adopt the dynamic crystallization equipment of three layers circulating line, phase after crystallisation, lower floor's circulating line can be closed, control upper strata and intercycle pipe flow speed slows down, crystalline particle is enriched with in crystallization kettle middle and lower part, tiny crystalline particle continues cycling through flowing crystallization, and good mixed performance can make strength of fluid to be crystallized homogeneous, steady change, promote crystal homoepitaxial, the crystal grain size formed is uniform, and substantially reduces crystallization time, it also avoid crystallographic wall built-up or the situation of the blocking mouth of pipe.
Still outer circulation passage has leakage fluid dram, and each liquid sucting port shares leakage fluid dram. Each liquid sucting port place can arrange valve and draws the switch of liquid to be crystallized to regulate each At The Height and draw the flow of liquid to be crystallized. The setting sharing leakage fluid dram also makes the design of whole equipment compacter, decreases the quantity of circulating pump, adds the operable degree that circular flow is controlled.
The link position of leakage fluid dram can be selected according to physical condition. Preferably, leakage fluid dram is connected to the top of crystallization kettle.
Still outer circulation passage is additionally provided with chiller. Described chiller is pipe bundle condenser. The quantity of pipe bundle condenser can be more than one; Preferably, plural pipe bundle condenser is arranged in still outer circulation passage with parallel way, such that it is able to more effective, crystallized liquid is realized gradient cooling.
Crystallization kettle is further opened with inert gas import, is used for passing into noble gas, maintain positive pressure environment in crystallization kettle.
The chiller of crystallization kettle can be the cooling jacket being sheathed on outside still.
Described crystallization kettle is preferably leptosomic type crystallization kettle.
The mixture that liquid to be crystallized obtains through above-mentioned dynamic crystallization process, through solid-liquid separation, mother liquid obtained can return is continuing with, and gained crystal gets product after drying. Preferably, above-mentioned dynamic crystallization equipment, also include the Filter dryer being connected with crystallization kettle, for being filtered drying to the mixture obtained after dynamic crystallization in crystallization kettle.
Mixture directly can be entered Filter dryer by the leakage fluid dram of crystallization kettle bottom. Preferably, Filter dryer being connected to the pumping device for being evacuated in Filter dryer by mixture in crystallization kettle, described pumping device includes the liquid suction pipe stretched within crystallization kettle and the drawing liquid pump being connected with liquid suction pipe. By the setting of above-mentioned pumping device, the crystal accumulation blocking mouth of pipe can be prevented further.
The upper end of described Filter dryer is pyramidal structure, and lower end is inverted cone-shaped structure. Described Filter dryer is provided externally with heater, and inside is provided with screen plate; Described heater includes being sheathed on the heating agent chuck that Filter dryer is peripheral, is used for controlling the dry heating rate of crystal. The aperture of screen plate is 200 orders; Filter dryer is connected with mother liquor outlet.
In above-mentioned dynamic crystallization equipment, crystallization kettle and Filter dryer are both preferably 316L stainless steel, and inner lining material is politef. Condenser tubulation, crystallization kettle chuck and exsiccator chuck are both preferably SUS314 material.
In above-mentioned chiller, coolant used is chosen as one or both mixture in ether, ethylene glycol, ethyl chloride, bromoethane, chloromethanes, carbon tetrachloride etc., it is preferred to ethyl chloride or chloromethanes or the two mixture. In heater, heating agent used is chosen as one or both organic mixtures in ether, ethylene glycol, ethyl chloride, bromoethane, chloromethanes, carbon tetrachloride, water, it is preferred to water.
Crystallization kettle and Filter dryer with the use of, crystallization kettle ensures that the crystal particle diameter obtained after dynamic crystallization is uniform, Filter dryer then realizes the filtration drying function of product simultaneously, mother solution is continuing with by directly leaching return bottom bipyramid, crystal drying is expelled directly out, simple to operation, work efficiency improves. Simultaneously in whole process, it is not added with agitating device, produces gas and can pass through relief valve discharge collection, in commercial Application more safe and reliable, the production process being particularly suitable in mother solution containing severe corrosive and poisonous gas, such as the dynamic crystallization process of lithium hexafluoro phosphate, is suitable for promoting the use of.
A kind of dynamic crystallization method, it is draw and send back to crystallization kettle from the differing heights of crystallization kettle by liquid to be crystallized to be circulated, in cyclic process, according to crystal formation size, regulate each At The Height and draw the switch of liquid to be crystallized and draw the flow of liquid to be crystallized.
At the crystallization initial stage, regulate each At The Height and draw the flow velocity quickening of liquid to be crystallized, make the overall quickly mixing of liquid to be crystallized, form nucleus of uniform size; Along with the carrying out of crystallization, the rate of circulating flow of liquid to be crystallized can be slowed down, the basis of the good mixed performance of system makes crystal homoepitaxial; Phase after crystallisation, crystal grain is enriched with in crystallization kettle middle and lower part, optional closes bottom circulation, makes crystallized liquid circulate in middle and upper part, such that it is able to make fine crystals granule continued growth, finally gives epigranular, crystal grain that crystal formation is complete.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the embodiment of the present invention 1 dynamic crystallization equipment;
Fig. 2 is the schematic diagram of the embodiment of the present invention 2 dynamic crystallization equipment;
Fig. 3 is the schematic diagram of the embodiment of the present invention 3 dynamic crystallization equipment.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
The dynamic crystallization equipment of the present embodiment, as it is shown in figure 1, include the crystallization kettle 1 being arranged with cooling jacket 3, crystallization kettle offers material inlet 5, and this material inlet can be used for passing into noble gas, makes to keep in still malleation, or is used for passing into liquid to be crystallized; Discharge gate 16 it is provided with bottom crystallization kettle; Crystallization kettle is externally provided with still outer circulation passage, still outer circulation passage has two liquid sucting ports, respectively the first liquid sucting port 13 and the second liquid sucting port 15, also there is shared leakage fluid dram 17, first liquid sucting port is connected with the discharge gate bottom crystallization kettle, second liquid sucting port 15 is connected with the middle part of crystallization kettle, shares leakage fluid dram and is connected with the top of crystallization kettle; Still outer circulation passage is additionally provided with circulating pump 2. Cooling jacket is provided with coolant import 31 and refrigerant exit 32. Discharge gate bottom crystallization kettle is also associated with residual liquid row's mouth 12, is used for discharging material in still. First liquid sucting port and the second liquid sucting port place are provided with valve for controlling the flow velocity of liquid to be crystallized.
The dynamic crystallization method of the present embodiment, liquid to be crystallized enters in crystallization kettle from material inlet, may select and continues to pass into nitrogen so that being full of nitrogen in crystallization kettle, it is to avoid crystallization process and air contact; ON cycle pump, liquid to be crystallized enters still outer circulation passage, and at the crystallization initial stage, the valve at the first liquid sucting port and the second liquid sucting port place is in open mode, liquid fast cycles to be crystallized mixing in still, gradually forms nucleus of uniform size; Along with growing up of crystal, control rate of circulating flow and slow down, make crystal homoepitaxial; In the crystallization later stage, the crystalline particle grown is enriched with in crystallization kettle middle and lower part, optional closedown the first liquid sucting port, the continued growth in still outer circulation passage of tiny crystalline particle, and crystallization obtains crystalline particle of uniform size after completing; Crystal suspensions after dynamic crystallization can be arranged mouth by residual liquid and discharge, and operates through solid-liquid separation, respectively obtains crystal and mother solution.
Embodiment 2
The dynamic crystallization equipment of the present embodiment, as in figure 2 it is shown, include the crystallization kettle 1 being arranged with cooling jacket 3, crystallization kettle offers material inlet 5, and this material inlet can be used for passing into noble gas, makes to keep in still malleation, or is used for passing into liquid to be crystallized; Discharge gate 16 it is provided with bottom crystallization kettle; Crystallization kettle is externally provided with still outer circulation passage, still outer circulation passage has three liquid sucting ports, it is connected to the bottom of crystallization kettle, middle part and top, respectively the first liquid sucting port the 13, second liquid sucting port 14 and the 3rd liquid sucting port 15, also having shared leakage fluid dram 17, shared leakage fluid dram is connected to the top of crystallization kettle; Being additionally provided with chiller and circulating pump 2 on still outer circulation passage, chiller is two pipe bundle condensers being set up in parallel 4. Cooling jacket and pipe bundle condenser are equipped with coolant import 31 and refrigerant exit 32. Discharge gate bottom crystallization kettle is also associated with residual liquid row's mouth 12, is used for discharging material in still. Still outer circulation passage Shang Ge import department is equipped with valve for controlling the flow velocity of liquid to be crystallized.
The dynamic crystallization method of the present embodiment, still outer circulation passage separately constitutes upper, middle and lower-ranking circulation canal, crystallization initial stage, opens the valve of upper, middle and lower-ranking circulating line simultaneously, liquid to be crystallized is in and good circulates state, is beneficial to and is formed uniformly nucleus; Along with the prolongation of crystallization time, valve can be controlled and slow down the flow velocity of three layers circulating line; In the crystallization later stage, crystal grain is enriched with in crystallization kettle middle and lower part, and the concentration of crystallization kettle middle and upper part crystalloid solution is little, lower floor's circulation canal can be closed, slow down the flow velocity of upper strata and intercycle pipeline, regulates condenser simultaneously and controls gradient cooling, so that crystal grain is uniformly grown up; Mixture after dynamic crystallization can be arranged mouth by residual liquid and discharge, and operates through solid-liquid separation, respectively obtains crystal and mother solution.
Embodiment 3
The dynamic crystallization equipment of the present embodiment, as it is shown on figure 3, include crystallization kettle and the Filter dryer 7 being connected with crystallization kettle, the structure of crystallization kettle is identical with embodiment 2, and the mixture in crystallization kettle is evacuated to inside Filter dryer by pumping device by Filter dryer 7; Pumping device includes the liquid suction pipe stretched within crystallization kettle and the drawing liquid pump 6 being connected with liquid suction pipe, and drawing liquid delivery side of pump is connected with the material import and export 11 of Filter dryer; Being provided with filter plate 10 in described Filter dryer, bottom is provided with mother liquor outlet 8. Being arranged with heating agent chuck 9 outside Filter dryer, heating agent chuck is provided with Heating medium 91 and heating agent outlet 92, and Heating medium is positioned at the lower section of heating agent outlet.
This equipment is operationally, by pumping device, the mixture obtained after dynamic crystallization is squeezed in Filter dryer, a small amount of residual liquid is arranged mouth by residual liquid and is discharged, enter the mixture in Filter dryer after filter plate, filtrate is returned mother solution synthesis groove by mother liquor outlet 8 and is continuing with, by heating agent chuck, gained crystal being carried out intensification to dry, the crystal after drying can be discharged by material import and export, carries out finished product packing.
In other embodiments of the invention, the character according to liquid to be crystallized, there is the situation of two liquid sucting ports, liquid sucting port also can lay respectively at bottom/top or the middle part/top of crystallization kettle; Each liquid sucting port can be connected to independent leakage fluid dram, circulating pump and chiller, and leakage fluid dram may connect to the top of crystallization kettle, middle part or bottom. Also dependent on the shape of equipment, arranging the liquid sucting port of more than 4 exemplary distribution, so that the mixed performance of liquid to be crystallized is better, in dynamic crystallization process, circulate performance good, the concentration of liquid to be crystallized is homogeneous, steady change, crystallize even particle size.

Claims (10)

1. a dynamic crystallization equipment, including crystallization kettle, it is characterised in that crystallization kettle is externally provided with still outer circulation passage and flows at still inner-outer circulation for realizing liquid to be crystallized; Described still outer circulation passage is provided with two or more liquid sucting port, and liquid sucting port is connected on the differing heights of crystallization kettle, for realizing circulating of differing heights place liquid to be crystallized.
2. dynamic crystallization equipment as claimed in claim 1, it is characterised in that be at least connected to described liquid sucting port in the upper, middle and lower of crystallization kettle.
3. dynamic crystallization equipment as claimed in claim 1 or 2, it is characterised in that still outer circulation passage has leakage fluid dram, and each liquid sucting port shares leakage fluid dram.
4. dynamic crystallization equipment as claimed in claim 3, it is characterised in that leakage fluid dram is connected to the top of crystallization kettle.
5. dynamic crystallization equipment as claimed in claim 1 or 2, it is characterised in that be additionally provided with chiller on still outer circulation passage.
6. dynamic crystallization equipment as claimed in claim 1 or 2, it is characterised in that be further opened with inert gas import on crystallization kettle, be used for passing into noble gas, maintain positive pressure environment in crystallization kettle.
7. dynamic crystallization equipment as claimed in claim 1 or 2, it is characterised in that described crystallization kettle is leptosomic type vertical response still.
8. dynamic crystallization equipment as claimed in claim 1 or 2, it is characterised in that also include the Filter dryer being connected with crystallization kettle, for being filtered drying to the mixture obtained after dynamic crystallization in crystallization kettle.
9. dynamic crystallization equipment as claimed in claim 8, it is characterised in that be connected to the pumping device for being evacuated in Filter dryer by mixture in crystallization kettle on Filter dryer.
10. a dynamic crystallization method, it is characterized in that, from the differing heights of crystallization kettle, crystallization kettle is drawn and sent back to liquid to be crystallized and be circulated, in cyclic process, according to crystal formation size, regulate each At The Height and draw the switch of liquid to be crystallized and draw the flow of liquid to be crystallized.
CN201610107401.6A 2016-02-25 2016-02-25 A kind of dynamic crystallization equipment and dynamic crystallization method Active CN105664521B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107233745A (en) * 2017-07-18 2017-10-10 四川思特瑞科技有限公司 Circulating crystallizer and circulating crystal system
CN107244681A (en) * 2017-03-29 2017-10-13 东营石大胜华新能源有限公司 A kind of continuous method and apparatus for preparing lithium hexafluoro phosphate
CN110201415A (en) * 2019-06-19 2019-09-06 中国人民解放军陆军特色医学中心 A kind of drug purification processing unit
CN113845506A (en) * 2021-10-18 2021-12-28 惠州市宙邦化工有限公司 Dynamic crystallization purification method of ethylene carbonate
CN113856235A (en) * 2021-09-29 2021-12-31 浙江大华技术股份有限公司 Cooling crystallization control method, device, electronic equipment and system
WO2023098189A1 (en) * 2021-11-30 2023-06-08 苏州华一新能源科技股份有限公司 Preparation process for fluoroethylene carbonate and lithium battery applying fluoroethylene carbonate

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63209702A (en) * 1987-02-25 1988-08-31 Ishikawajima Harima Heavy Ind Co Ltd Method for operating crystallizer
CN2609628Y (en) * 2003-04-01 2004-04-07 化工部长沙设计研究院 Stage inorganic salt multi-decomposition reaction crystallizer
CN102371080A (en) * 2010-08-23 2012-03-14 中国石油化工股份有限公司 Crystallizing method utilizing external circulation of crystal slurry
CN102371081A (en) * 2010-08-23 2012-03-14 中国石油化工股份有限公司 Crystallization method with a fine crystal elimination
CN202983275U (en) * 2012-11-22 2013-06-12 中节能六合天融环保科技有限公司 Vacuum crystallizer with DTB (Drabt Tube Babbled) characteristic
CN104692575A (en) * 2014-12-22 2015-06-10 内蒙古久科康瑞环保科技有限公司 Crystallization treatment method and device of high salt wastewater
CN105289037A (en) * 2015-11-11 2016-02-03 广东鑫国泰科技有限公司 Sodium chlorate crystallizer

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63209702A (en) * 1987-02-25 1988-08-31 Ishikawajima Harima Heavy Ind Co Ltd Method for operating crystallizer
CN2609628Y (en) * 2003-04-01 2004-04-07 化工部长沙设计研究院 Stage inorganic salt multi-decomposition reaction crystallizer
CN102371080A (en) * 2010-08-23 2012-03-14 中国石油化工股份有限公司 Crystallizing method utilizing external circulation of crystal slurry
CN102371081A (en) * 2010-08-23 2012-03-14 中国石油化工股份有限公司 Crystallization method with a fine crystal elimination
CN202983275U (en) * 2012-11-22 2013-06-12 中节能六合天融环保科技有限公司 Vacuum crystallizer with DTB (Drabt Tube Babbled) characteristic
CN104692575A (en) * 2014-12-22 2015-06-10 内蒙古久科康瑞环保科技有限公司 Crystallization treatment method and device of high salt wastewater
CN105289037A (en) * 2015-11-11 2016-02-03 广东鑫国泰科技有限公司 Sodium chlorate crystallizer

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107244681A (en) * 2017-03-29 2017-10-13 东营石大胜华新能源有限公司 A kind of continuous method and apparatus for preparing lithium hexafluoro phosphate
CN107233745A (en) * 2017-07-18 2017-10-10 四川思特瑞科技有限公司 Circulating crystallizer and circulating crystal system
CN110201415A (en) * 2019-06-19 2019-09-06 中国人民解放军陆军特色医学中心 A kind of drug purification processing unit
CN110201415B (en) * 2019-06-19 2021-04-13 中国人民解放军陆军特色医学中心 Medicine purification processing apparatus
CN113856235A (en) * 2021-09-29 2021-12-31 浙江大华技术股份有限公司 Cooling crystallization control method, device, electronic equipment and system
CN113845506A (en) * 2021-10-18 2021-12-28 惠州市宙邦化工有限公司 Dynamic crystallization purification method of ethylene carbonate
US11958820B2 (en) 2021-10-18 2024-04-16 Shenzhen Capchem Technology Co., Ltd. Method for purifying ethylene carbonate through dynamic crystallization
WO2023098189A1 (en) * 2021-11-30 2023-06-08 苏州华一新能源科技股份有限公司 Preparation process for fluoroethylene carbonate and lithium battery applying fluoroethylene carbonate

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