CN107501230A - Crystallization couples the device and method for preparing electron level ethylene carbonate with rectifying - Google Patents
Crystallization couples the device and method for preparing electron level ethylene carbonate with rectifying Download PDFInfo
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- CN107501230A CN107501230A CN201710907828.9A CN201710907828A CN107501230A CN 107501230 A CN107501230 A CN 107501230A CN 201710907828 A CN201710907828 A CN 201710907828A CN 107501230 A CN107501230 A CN 107501230A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/36—Alkylene carbonates; Substituted alkylene carbonates
- C07D317/38—Ethylene carbonate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention belongs to the preparing technical field of electronic grade reagents, is related to crystallization and the device and method for preparing electron level ethylene carbonate is coupled with rectifying.Crystallization provided by the invention couples the device for preparing electron level ethylene carbonate, including raw material storage tank, falling-film crystallizer, rectifying column, the first products pot, transition tank and the second products pot with rectifying；Raw material storage tank is connected with the charging aperture of falling-film crystallizer, and being provided with discharging in the discharge outlet of falling-film crystallizer is responsible for, and the charging aperture with falling-film crystallizer, the first products pot and transition tank are connected discharging supervisor respectively；Transition tank is connected with rectifying column, and the tower top outlet of rectifying column is connected with the second products pot, and the bottom of towe outlet of rectifying column is connected with raw material storage tank.Two kinds of technologies of film-falling crystallization and rectifying are coupled by the present invention, learn from other's strong points to offset one's weaknesses, realize more preferable lock out operation, obtained ethylene carbonate can reach the electronics rank of super-clean high-purity；Meanwhile it is simple in construction, easy to operate, energy consumption is low, and cost is low.
Description
Technical field
The invention belongs to the preparing technical field of electronic grade reagents, is related to the preparation of electron level ethylene carbonate, it is specific and
Speech, it is related to crystallization and the device and method for preparing electron level ethylene carbonate is coupled with rectifying.
Background technology
Ethylene carbonate（EC）It is the organic solvent and organic synthesis intermediate of a kind of function admirable, has boiling point high, malicious
The advantages that property and corrosivity are small, water-soluble, acetone, ethanol equal solvent can dissolve polyvinyl chloride, polyacrylonitrile etc., can be used as
The liquid that reels off raw silk from cocoons in weaving；Also can be directly as the solvent of removing sour gas and the additive of concrete.It can be used as in medicine
The component and raw material of medicine；Also act as the stabilizer of plastics blowing agent and synthetic lubricant fluid.It is especially prominent, ethylene carbonate
It is widely used in lithium ion battery industry, can be as the fine solvent of lithium battery electrolytes；It is quick with lithium battery industry
Development, the demand of ethylene carbonate are also gradually increasing.
At present, oxirane and the carbon dioxide direct carbonate synthesis second under high temperature, catalyst action mainly industrially are used
Alkene ester.However, while esterification generation ethylene carbonate occurs for oxirane and carbon dioxide, it is also possible to epoxy be present
Ethane hydration generation ethylene glycol, oxirane and the hydrolysis of ethylene glycol generation diethylene glycol (DEG) and ethylene carbonate.The life of alcohols
Into and ethylene carbonate ester hydrolysis bad influence can be all brought to lithium ion battery.Further, since the moisture absorption of ethylene carbonate
Property, while containing above-mentioned impurity, also containing micro moisture content, this configuration to lithium-ion battery electrolytes be it is unfavorable,
Therefore ethylene carbonate must be processed and purified, to reach electron level, meet the requirement of high-quality lithium battery.
The mode purified at present to ethylene carbonate is more by the way of rectifying, but existing operating procedure has energy consumption
Greatly, the problems such as operation cycle is long, yield is low, loss of material is big in purge process.Simple prepares electronics by way of rectifying
The ethylene carbonate of level, the purity and yield of product are difficult to take into account, and production cost is high.In addition, also have by adding iron chloride, chlorine
Change the mode that aluminium, molecular sieve etc. remove alcohol cleaner, carry out the purifying of ethylene carbonate, and there is also operating condition for this mode
It is required that high, the operation cycle is grown, complex operation, the shortcomings such as yield is low.
In consideration of it, special propose the present invention.
The content of the invention
The first object of the present invention is that providing a kind of crystallization couples the device for preparing electron level ethylene carbonate with rectifying,
With simple in construction, manipulation convenience, it is possible to achieve the advantages of material liquid recycles, and cost is low, and the comprehensive benefit of device is high.
The second object of the present invention is that providing a kind of crystallization couples the method for preparing electron level ethylene carbonate with rectifying,
Ethylene carbonate is prepared by using said apparatus, has product purity high, high income, energy consumption is low, and material liquid can circulate profit
With saving cost, it is easy to accomplish the advantages of industrial-scale production.
To achieve the above object, the technical solution adopted by the present invention is：
According to an aspect of the present invention, the present invention provides a kind of dress for crystallizing and being coupled with rectifying and preparing electron level ethylene carbonate
Put, including raw material storage tank, falling-film crystallizer, rectifying column, the first products pot, transition tank and the second products pot；
The raw material storage tank is connected by feeding line with the charging aperture of falling-film crystallizer, is set in the discharge outlet of falling-film crystallizer
It is equipped with discharging supervisor, end connection pipeloop, the first product pipeline and the transition pipeline of the discharging supervisor, the circulation pipe
Line is connected with the charging aperture of falling-film crystallizer, and first product pipeline is connected with the first products pot, the transition pipeline and mistake
Tank is crossed to be connected；
The transition tank is connected by the first connecting pipeline with the liquor inlet of rectifying column, and the tower top outlet of the rectifying column passes through
Second product pipeline is connected with the second products pot, and the bottom of towe outlet of the rectifying column passes through the second connecting pipeline and raw material storage tank phase
Even.
In view of the purifier of ethylene carbonate of the prior art has high energy consumption, operation cycle length, yield is low,
The shortcomings of loss of material is big, the invention provides a kind of crystallize to couple the device for preparing electron level ethylene carbonate with rectifying.By
It is faster than fusion-crystallization process mass transfer in distillation process, it is adapted to the big system of separation relative volatility difference；And crystallize and boiled in separation
With very big advantage during point material that is close and needing high-purity.The present invention is by film-falling crystallization and rectifying both separation methods
Combine, learn from other's strong points to offset one's weaknesses, realize more preferable lock out operation, obtained ethylene carbonate can reach ultra-clean height
Pure electronics rank.
The inventive system comprises raw material storage tank, falling-film crystallizer, rectifying column, the first products pot, transition tank and the second production
Product tank；Wherein raw material storage tank is connected with the charging aperture of falling-film crystallizer, and the discharging of falling-film crystallizer is divided into three tunnels, the first via and the
One products pot is connected, and for collecting the material purified through falling-film crystallizer, finished product is produced；Second tunnel and falling-film crystallizer enter
Material mouth is connected, and feed liquid is circulated, and to realize that secondary crystallization purifies, further improves the purity of product；3rd tunnel and transition tank phase
Even, for collecting sweating raffinate, sweating raffinate is kept in；And transition tank is connected with rectifying column, using sweating raffinate as rectifying column
Material liquid, carry out rectification and purification；Rectifying column tower top is connected with the second products pot, light to collect the tower top that rectifying separates
Component, rectifying tower bottom are connected with raw material storage tank, and the tower bottom of rectifying tower product for reaching crystallizer feed needs returns to raw material storage
Tank, realize recycled.The present invention can realize feed liquid recycled, almost not lose, and energy consumption is low, cost-effective；Product
Quality is easily controlled, and purity is high；Meanwhile it is simple in construction, it is easy to operate, it is reasonable in design, greatly improve the comprehensive benefit of device
And the economic benefit of enterprise.
As further preferred technical scheme, feedstock transportation pump and regulating valve are provided with the feeding line；
Discharging main valve is provided with the discharging supervisor, is set respectively on the pipeloop, the first product pipeline and transition pipeline
The first valve, the second valve and the 3rd valve are equipped with, circulation feed liquid delivery pump, the circulation are additionally provided with the pipeloop
Pipeline is connected with the feeding line；
Outlet valve and feed pump, the tower of the rectifying column are provided with the first connecting pipeline that the transition tank is connected with rectifying column
Ejection mouth divides two-way after running through condenser by pipeline, is connected all the way with the liquid-phase reflux mouth of rectifying column, another way and the second production
QC line is connected, and tower top cooler is provided with second product pipeline；The rectifying column be connected with raw material storage tank second
Bottom of towe cooler, regulating valve and kettle liquid delivery pump are disposed with connecting pipeline.
By the setting of valve and pump on above-mentioned each pipeline in the present invention, in order to the conveying of material, and device is steady
Fixed operation, while it is easy to the regulation and control of flow.
Rectifying column in the present invention is material filling type rectifying column, and heat-insulation layer is provided with outside rectifying column.
Rectifying column tower top is provided with condenser, and bottom of towe sets reboiler, and condenser and reboiler therein can use existing
The condenser and reboiler commonly used in technology.
As further preferred technical scheme, the falling-film crystallizer sets overfall, and the overfall is arranged on falling liquid film
The top of crystallizer, and be connected by the 3rd connecting pipeline with the raw material storage tank.
The falling-film crystallizer of the present invention is provided with cooling medium inlet, cooling medium outlet, charging aperture, discharging opening, also sets
Overfall is equipped with, overfall therein can be such that unnecessary material is flowed out from overfall, avoid causing equipment to block, influence normally to transport
OK, to improve operating efficiency.
As further preferred technical scheme, spilling pipeline is provided with the transition tank, is set on the spilling pipeline
There is overflow valve.
As further preferred technical scheme, the raw material storage tank, the first products pot and transition tank are provided with thermal insulation clamp
Layer.
By the setting of heat preservation sandwich layer, it can prevent pot liquid from crystallizing, to ensure the production run efficiency of equipment, Jin Erjie
Save time, improve operating efficiency.
The first product pot bottom in the present invention is provided with finished product discharging pipeline, and being provided with finished product on finished product discharging pipeline goes out
Expect valve.
As further preferred technical scheme, the falling-film crystallizer is internally provided with cooling medium distribution tray and falling liquid film
Crystallizer, the cooling medium distribution tray and film-falling crystallization pipe right angle setting, the film-falling crystallization pipe is by upper perforated plate with
Tube sheet is fixed, and the top of the upper perforated plate is provided with top plate, and the lower section of the lower perforated plate is provided with low head.
As further preferred technical scheme, the film-falling crystallization pipe is more, and the every film-falling crystallization pipe upper end
Exhaust hole is provided with inserted with mozzle, the mozzle；
Arrangement position in the cooling medium distribution tray corresponding to film-falling crystallization pipe is provided with cooling medium pod apertures, downflow weir
And downspout, and the film-falling crystallization pipe passes through the pod apertures.
Preferably, the diameter ratio of the mozzle and film-falling crystallization pipe is 0.1~0.95.
Preferably, the diameter ratio of the cooling medium pod apertures and film-falling crystallization pipe is 0.1~0.95.
Falling-film crystallizer provided by the invention is simple in construction, and maintenance easy to maintain, cost is low, and can strengthen cooling and be situated between
Heat transfer between matter and crystal, it is more beneficial for obtaining high purity product.
According to another aspect of the present invention, a kind of crystallization of present invention offer couples with rectifying prepares electron level ethylene carbonate
The method of ester, including crystallization process and distillation process, the crystallization process comprise the following steps：
Crystallization：Ethylene carbonate material to be purified is delivered in falling-film crystallizer from raw material storage tank, material enters falling liquid film knot
Brilliant device inside and the film evaporation device in crystallizer, adjust the temperature of cooling medium so that material crystallizes in crystallizer, works as crystal layer
Stop charging when reaching certain thickness；
Sweating：Then being stepped up coolant temperature makes crystal layer sweating, and sweating raffinate is discharged into transition tank；
Crystals melt：After sweating terminates, further raise coolant temperature, crystal layer be all molten into liquid, and be discharged into
In first products pot；Ethylene carbonate liquid in first products pot produces directly as finished product, or by pipeloop again
It is secondary to be back to progress secondary crystallization purifying in falling-film crystallizer；
The distillation process is：Sweating raffinate in transition tank is delivered in rectifying column, by higher boiling and lower boiling composition point
From overhead collection low boiling product is simultaneously discharged into the second products pot, and it is molten that bottom of towe collects the ethylene carbonate through being further purified
Liquid, and return in raw material storage tank.
Refer to it should be noted that crystal layer of the present invention reaches certain thickness and consider crystallization temperature and knot
Brilliant time, resulting crystal layer thickness, the thickness value can be depending on actual conditions；Can be according to the purity of raw material in actual production
To determine crystallization time, both ensure certain product purity, ensure certain percent crystallization in massecuite again.
As further preferred technical scheme, the operating condition of the crystallization process is：
The feed flow rate of ethylene carbonate is 100L/h~500L/h, and feeding temperature is 39~45 DEG C;
Cooling step-length during film-falling crystallization is 1~2.5 DEG C/h, and crystallization time is 2~13h, and decrease temperature crystalline outlet temperature is
32~34 DEG C, constant temperature is then carried out, constant temperature time is 1~3h；
Heating step-length in sweating effort is 2~4 DEG C/h, and sweating sessions are 2~8h, and sweating outlet temperature is 36~38 DEG C；
Temperature during crystals melt is 40~60 DEG C.
As further preferred technical scheme, the operating condition of the distillation process is：
Operated using rectification under vacuum, tower pressure interior force is 1.33~2.67kPa, and column bottom temperature is 100~130 DEG C, return time 3
~6h.
Compared with prior art, the beneficial effects of the present invention are：
1st, crystallization provided by the invention couples the device for preparing electron level ethylene carbonate, including raw material storage tank, falling liquid film with rectifying
Crystallizer, rectifying column, the first products pot, transition tank and the second products pot, two kinds of technologies of film-falling crystallization and rectifying are coupling in one
Rise, learn from other's strong points to offset one's weaknesses, realize more preferable lock out operation, obtained ethylene carbonate can reach the electronics rank of super-clean high-purity；
Meanwhile it is simple in construction, reasonable in design, easy to operate, material does not almost lose, and energy consumption is low, and cost is low.
2nd, crystallization provided by the invention couples the method for preparing electron level ethylene carbonate with rectifying, by using above-mentioned dress
Put and prepare ethylene carbonate, rational technology, product purity is high, can obtain the ethylene carbonate of content more than 99.99%；Yield
Height, energy consumption is low, and material liquid can recycle, and saves cost, it is easy to accomplish industrial-scale production.
3rd, present invention process is simple, easy to operate, and equipment investment is few, and operating cost is low, and stable, reliable, energy consumption is low, operation
Cycle is short, and production cost is low, and loss of material is few, can obtain the electron level ethylene carbonate of super-clean high-purity, greatly improve enterprise
The economic benefit of industry, effectively alleviates the operation cycle length in the presence of prior art, complex operation, the problems such as yield is low.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The required accompanying drawing used is briefly described in embodiment or description of the prior art, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is that crystallization provided in an embodiment of the present invention couples with rectifying and prepares the apparatus structure of electron level ethylene carbonate and show
It is intended to；
Fig. 2 falling-film crystallizer structural representations provided in an embodiment of the present invention.
Icon：1- raw material storage tanks；2- falling-film crystallizers；3- rectifying columns；The products pots of 4- first；5- transition tanks；The products pots of 6- second；
201- charging apertures；202- discharging openings；203- cooling medium inlets；204- cooling mediums export；205- overfalls；206- coolings are situated between
Matter distribution tray；207- film-falling crystallization pipes；208- upper perforated plates；209- lower perforated plates；210- top plates；211- low heads；212- water conservancy diversion
Pipe；213- exhaust holes；214- downflow weirs；215- downspouts；301- liquor inlet；302- tower top outlets；303- bottom of towe exports；
304- liquid-phase reflux mouths；305- heat-insulation layers；306- condensers；307- reboilers；308- tower top coolers；309- bottom of towe cools down
Device；11- feeding lines；12- feedstock transportation pumps；13- regulating valves；21- discharging supervisors；22- discharging main valves；31- pipeloops；
The valves of 32- first；33- circulates feed liquid delivery pump；The product pipelines of 41- first；The valves of 42- second；43- finished products discharging pipeline；44-
Finished product outlet valve；51- transition pipelines；The valves of 52- the 3rd；61- overflows pipeline；62- overflow valves；71- outlet valves；72- feed pumps；
The product pipelines of 81- second；91- regulating valves；92- kettle liquid delivery pumps.
Embodiment
Technical scheme is clearly and completely described below in conjunction with accompanying drawing, it is clear that described implementation
Example is part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
In the description of the invention, it is necessary to explanation, term " " center ", " on ", " under ", "left", "right", " vertical ",
The orientation or position relationship of the instruction such as " level ", " interior ", " outer " be based on orientation shown in the drawings or position relationship, merely to
Be easy to the description present invention and simplify description, rather than instruction or imply signified device or element must have specific orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.In addition, term " first ", " second ",
" the 3rd " is only used for describing purpose, and it is not intended that instruction or hint relative importance.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected, or be integrally connected；Can
To be mechanical connection or electrical connection；Can be joined directly together, can also be indirectly connected by intermediary, Ke Yishi
The connection of two element internals.For the ordinary skill in the art, with concrete condition above-mentioned term can be understood at this
Concrete meaning in invention.
Below in conjunction with embodiment and accompanying drawing, the present invention will be further described in detail.
Embodiment 1
As shown in figure 1, the present embodiment provides a kind of device for crystallizing and being coupled with rectifying and preparing electron level ethylene carbonate, including original
Expect storage tank 1, falling-film crystallizer 2, rectifying column 3, the first products pot 4, the products pot 6 of transition tank 5 and second.
The annexation of each device is：
Raw material storage tank 1 is connected by feeding line 11 with the charging aperture 201 of falling-film crystallizer 2, in the discharging opening of falling-film crystallizer 2
Discharging supervisor 21, end connection pipeloop 31, the first product pipeline 41 and the transition pipeline of discharging supervisor 21 are provided with 202
51, pipeloop 31 is connected with the charging aperture 201 of falling-film crystallizer 2, and the first product pipeline 41 is connected with the first products pot 4, mistake
Pipeline 51 is crossed with transition tank 5 to be connected；
Transition tank 5 is connected by the first connecting pipeline A with the liquor inlet 301 of rectifying column 3, and the tower top outlet 302 of rectifying column 3 is logical
Cross pipeline and divide two-way after condenser 306, be connected all the way with the liquid-phase reflux mouth 304 of rectifying column 3, another way passes through the second production
QC line 81 is connected with the second products pot 6, and the bottom of towe outlet 303 of rectifying column 3 passes through the second connecting pipeline B and the phase of raw material storage tank 1
Even；
The overfall 205 of falling-film crystallizer 2 is arranged on the top of falling-film crystallizer 2, and is stored up by the 3rd connecting pipeline C and raw material
Tank 1 is connected.
Valve and pump in each connecting pipeline are arranged to：
Feedstock transportation pump 12 and regulating valve 13 are provided with feeding line 11；
Discharging main valve 22 is provided with discharging supervisor 21, is distinguished on pipeloop 31, the first product pipeline 41 and transition pipeline 51
The first valve 32, the second valve 42 and the 3rd valve 52 are provided with, circulation feed liquid delivery pump 33 is additionally provided with pipeloop 31,
Pipeloop 31 is connected with feeding line 11；
The bottom of first products pot 4 is provided with finished product discharging pipeline 43, and finished product outlet valve 44 is provided with finished product discharging pipeline 43；
Outlet valve 71 and feed pump 72 are provided with the first connecting pipeline that transition tank 5 is connected with rectifying column 3, is set on transition tank 5
It is equipped with and overflows pipeline 61, overflows and be provided with overflow valve 62 on pipeline 61；
Tower top cooler 308, the second connecting pipeline that rectifying column 3 is connected with raw material storage tank 1 are provided with second product pipeline 81
On be disposed with bottom of towe cooler 309, regulating valve 91 and kettle liquid delivery pump 92.
As shown in Fig. 2 the falling-film crystallizer 2 that the present embodiment provides is provided with cooling medium inlet 203, cooling medium outlet
204th, charging aperture 201, discharging opening 202 and overfall 205.Falling-film crystallizer 2 is internally provided with the He of cooling medium distribution tray 206
Film-falling crystallization pipe 207, cooling medium distribution tray 206 and the right angle setting of film-falling crystallization pipe 207, film-falling crystallization pipe 207 is by upper
Tube sheet 208 and lower perforated plate 209 are fixed, and the top of upper perforated plate 208 is provided with top plate 210, and the lower section of lower perforated plate 209 is provided with low head
211。
Wherein, film-falling crystallization pipe 207 is more, and the every upper end of film-falling crystallization pipe 207 is led inserted with mozzle 212
Flow tube 212 is provided with exhaust hole 213；Arrangement position in cooling medium distribution tray 206 corresponding to film-falling crystallization pipe 207 is set
There are cooling medium pod apertures, downflow weir 214 and downspout 215, and film-falling crystallization pipe 207 passes through pod apertures.
It is being independent disconnected for conveying the cooling medium in falling-film crystallizer 2 and film-falling crystallization pipe 207.
The diameter ratio of mozzle 212 and film-falling crystallization pipe 207 is 0.1~0.95.Cooling medium pod apertures and film-falling crystallization
The diameter ratio of pipe 207 is 0.1~0.95.
In the present embodiment, rectifying column 3 is material filling type rectifying column, and heat-insulation layer 305 is provided with outside rectifying column 3.The tower of rectifying column 3
Top is provided with condenser 306, and bottom of towe sets reboiler 307, and condenser 306 and reboiler 307 therein can use prior art
In commonly use condenser and reboiler.
In the present embodiment, raw material storage tank 1, the first products pot 4 and transition tank 5 are provided with heat preservation sandwich layer.
The crystallization that the present embodiment provides couples the operation principle of the device for preparing electron level ethylene carbonate with rectifying：
The regulating valve 13 on feeding line 11 is opened, by feedstock transportation pump 12 by ethylene carbonate material to be purified from raw material
Storage tank 1 is delivered in falling-film crystallizer 2, and material is at the top of falling-film crystallizer 2 by mozzle 212 in film-falling crystallization pipe 207
Film evaporation device, adjust the temperature of cooling medium so that material crystallizes in film-falling crystallization pipe 207, when crystal layer reaches certain thickness
When stop charging.Then being stepped up coolant temperature makes crystal layer sweating, opens the discharging valve 52 of main valve 22 and the 3rd, will send out
Sweat raffinate is discharged into transition tank 5.
After sweating terminates, the 3rd valve 52 is closed, opens the second valve 42, and further raises coolant temperature, is made
Crystal layer is all molten into liquid, is discharged into the first products pot 4, closes discharging main valve 22.
If ethylene carbonate content fails to reach requirement in the first products pot 4, the first valve 32 is opened, by circulating feed liquid
Liquid in first products pot 4 is re-circulated to falling-film crystallizer 2 by delivery pump 33, carries out secondary crystallization, is gone out conversely, opening finished product
Expect valve 44, ethylene carbonate uses directly as product.Outlet valve 71 is opened, by feed pump 72 by the sweating in transition tank 5
Raffinate is delivered in rectifying column 3, is cooled down as the material liquid of rectifying column 3, the overhead collection low boiling product of rectifying column 3 and by tower top
Device 308 is discharged into the second products pot 6 after cooling down, and the tower reactor product for reaching the feed needs of falling-film crystallizer 2 cools down by bottom of towe
Device 309 is returned in raw material storage tank 1 after cooling down with kettle liquid delivery pump 92.
Embodiment 2
The present embodiment provides a kind of method for crystallizing and being coupled with rectifying and preparing electron level ethylene carbonate, including crystallization process and essence
Process is evaporated, crystallization process comprises the following steps：
Crystallization：Ethylene carbonate material to be purified is delivered in falling-film crystallizer 2 from raw material storage tank 1, material enters falling liquid film
The inside of crystallizer 2 and the film evaporation device in crystallizer, adjusting the temperature of cooling medium so that material crystallizes in crystallizer, when
Crystal layer stops charging when reaching certain thickness；
Sweating：Then being stepped up coolant temperature makes crystal layer sweating, and sweating raffinate is discharged into transition tank 5；
Crystals melt：After sweating terminates, further raise coolant temperature, crystal layer be all molten into liquid, and be discharged into
In first products pot 4；Ethylene carbonate liquid in first products pot 4 produces directly as finished product, or passes through pipeloop
31 return again to progress secondary crystallization purifying in falling-film crystallizer 2.The present embodiment is by the way of secondary crystallization purifying.
Wherein, the operating condition of crystallization process is：
The feed flow rate of ethylene carbonate is 100L/h, and feeding temperature is 39 DEG C;
Cooling step-length during film-falling crystallization is 1 DEG C/h, and crystallization time 7h, decrease temperature crystalline outlet temperature is 32 DEG C, then
Carry out constant temperature, constant temperature time 17h；
Heating step-length in sweating effort is 2 DEG C/h, and sweating sessions 2h, sweating outlet temperature is 36 DEG C；
Temperature during crystals melt is 40 DEG C.
Distillation process is：Sweating raffinate in transition tank 5 is delivered in rectifying column 3, by higher boiling and lower boiling composition
Separation, overhead collection low boiling product are simultaneously discharged into the second products pot 6, and bottom of towe collects the ethylene carbonate through being further purified
Solution, and return in raw material storage tank 1.
Wherein, the operating condition of distillation process is：
Operated using rectification under vacuum, tower pressure interior force 1.33kPa, column bottom temperature is 100 DEG C, return time 3h.
Final electronic grade product is obtained by the above method, finally obtains the purity of ethylene carbonate in product（Quality point
Number）For 99.9921%, yield 98.8%.
Embodiment 3
The operating condition of crystallization process and the operating condition of distillation process as different from Example 2, remaining with the phase of embodiment 2
Together.
In the present embodiment, the operating condition of crystallization process is：
The feed flow rate of ethylene carbonate is 200L/h, and feeding temperature is 42 DEG C;
Cooling step-length during film-falling crystallization is 1.5 DEG C/h, and crystallization time 6h, decrease temperature crystalline outlet temperature is 33 DEG C, with
After carry out constant temperature, constant temperature time 2h；
Heating step-length in sweating effort is 3 DEG C/h, and sweating sessions 3h, sweating outlet temperature is 37 DEG C；
Temperature during crystals melt is 45 DEG C.
The operating condition of distillation process is：
Operated using rectification under vacuum, tower pressure interior force 2.0kPa, column bottom temperature is 110 DEG C, return time 4h.
Final electronic grade product is obtained by the above method, finally obtains the purity of ethylene carbonate in product（Quality point
Number）For 99.9991%, yield 97.5%.
Embodiment 4
The operating condition of crystallization process and the operating condition of distillation process as different from Example 2, remaining with the phase of embodiment 2
Together.
In the present embodiment, the operating condition of crystallization process is：
The feed flow rate of ethylene carbonate is 500L/h, and feeding temperature is 45 DEG C;
Cooling step-length during film-falling crystallization is 2.5 DEG C/h, and crystallization time 4h, decrease temperature crystalline outlet temperature is 34 DEG C, with
After carry out constant temperature, constant temperature time 3h；
Heating step-length in sweating effort is 4 DEG C/h, and sweating sessions 2h, sweating outlet temperature is 38 DEG C；
Temperature during crystals melt is 50 DEG C.
The operating condition of distillation process is：
Operated using rectification under vacuum, tower pressure interior force 2.67kPa, column bottom temperature is 130 DEG C, return time 6h.
Final electronic grade product is obtained by the above method, finally obtains the purity of ethylene carbonate in product（Quality point
Number）For 99.9911%, yield 99.2%.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. a kind of crystallize the device for being coupled with rectifying and preparing electron level ethylene carbonate, it is characterised in that including raw material storage tank, drop
Membrane crystallizer, rectifying column, the first products pot, transition tank and the second products pot；
The raw material storage tank is connected by feeding line with the charging aperture of falling-film crystallizer, is set in the discharge outlet of falling-film crystallizer
It is equipped with discharging supervisor, end connection pipeloop, the first product pipeline and the transition pipeline of the discharging supervisor, the circulation pipe
Line is connected with the charging aperture of falling-film crystallizer, and first product pipeline is connected with the first products pot, the transition pipeline and mistake
Tank is crossed to be connected；
The transition tank is connected by the first connecting pipeline with the liquor inlet of rectifying column, and the tower top outlet of the rectifying column passes through
Second product pipeline is connected with the second products pot, and the bottom of towe outlet of the rectifying column passes through the second connecting pipeline and raw material storage tank phase
Even.
2. crystallization according to claim 1 couples the device for preparing electron level ethylene carbonate with rectifying, it is characterised in that
Feedstock transportation pump and regulating valve are provided with the feeding line；
Discharging main valve is provided with the discharging supervisor, is set respectively on the pipeloop, the first product pipeline and transition pipeline
The first valve, the second valve and the 3rd valve are equipped with, circulation feed liquid delivery pump, the circulation are additionally provided with the pipeloop
Pipeline is connected with the feeding line；
Outlet valve and feed pump, the tower of the rectifying column are provided with the first connecting pipeline that the transition tank is connected with rectifying column
Ejection mouth divides two-way after running through condenser by pipeline, is connected all the way with the liquid-phase reflux mouth of rectifying column, another way and the second production
QC line is connected, and tower top cooler is provided with second product pipeline；The rectifying column be connected with raw material storage tank second
Bottom of towe cooler, regulating valve and kettle liquid delivery pump are disposed with connecting pipeline.
3. crystallization according to claim 1 couples the device for preparing electron level ethylene carbonate with rectifying, it is characterised in that
The falling-film crystallizer sets overfall, and the overfall is arranged on the top of falling-film crystallizer, and passes through the 3rd connecting pipeline
It is connected with the raw material storage tank.
4. crystallization according to claim 1 couples the device for preparing electron level ethylene carbonate with rectifying, it is characterised in that
Spilling pipeline is provided with the transition tank, overflow valve is provided with the spilling pipeline.
5. crystallization according to claim 1 couples the device for preparing electron level ethylene carbonate with rectifying, it is characterised in that
The raw material storage tank, the first products pot and transition tank are provided with heat preservation sandwich layer.
6. the crystallization according to claim any one of 1-5 couples the device for preparing electron level ethylene carbonate with rectifying, its
It is characterised by, the falling-film crystallizer is internally provided with cooling medium distribution tray and film-falling crystallization pipe, the cooling medium point
With tower tray and film-falling crystallization pipe right angle setting, the film-falling crystallization pipe is fixed by upper perforated plate and lower perforated plate, the upper perforated plate
Top is provided with top plate, and the lower section of the lower perforated plate is provided with low head.
7. crystallization according to claim 6 couples the device for preparing electron level ethylene carbonate with rectifying, it is characterised in that
The film-falling crystallization pipe is more, and the every film-falling crystallization pipe upper end is provided with inserted with mozzle, the mozzle
Exhaust hole；
Arrangement position in the cooling medium distribution tray corresponding to film-falling crystallization pipe is provided with cooling medium pod apertures, downflow weir
And downspout, and the film-falling crystallization pipe passes through the pod apertures.
8. a kind of equipment crystallization of usage right requirement 1 couples the method for preparing electron level ethylene carbonate with rectifying, it is special
Sign is, including crystallization process and distillation process, and the crystallization process comprises the following steps：
Crystallization：Ethylene carbonate material to be purified is delivered in falling-film crystallizer from raw material storage tank, material enters falling liquid film knot
Brilliant device inside and the film evaporation device in crystallizer, adjust the temperature of cooling medium so that material crystallizes in crystallizer, works as crystal layer
Stop charging when reaching certain thickness；
Sweating：Then being stepped up coolant temperature makes crystal layer sweating, and sweating raffinate is discharged into transition tank；
Crystals melt：After sweating terminates, further raise coolant temperature, crystal layer be all molten into liquid, and be discharged into
In first products pot；Ethylene carbonate liquid in first products pot produces directly as finished product, or by pipeloop again
It is secondary to be back to progress secondary crystallization purifying in falling-film crystallizer；
The distillation process is：Sweating raffinate in transition tank is delivered in rectifying column, by higher boiling and lower boiling composition point
From overhead collection low boiling product is simultaneously discharged into the second products pot, and it is molten that bottom of towe collects the ethylene carbonate through being further purified
Liquid, and return in raw material storage tank.
9. crystallization according to claim 8 couples the method for preparing electron level ethylene carbonate with rectifying, it is characterised in that
The operating condition of the crystallization process is：
The feed flow rate of ethylene carbonate is 100L/h~500L/h, and feeding temperature is 39~45 DEG C;
Cooling step-length during film-falling crystallization is 1~2.5 DEG C/h, and crystallization time is 2~13h, and decrease temperature crystalline outlet temperature is
32~34 DEG C, constant temperature is then carried out, constant temperature time is 1~3h；
Heating step-length in sweating effort is 2~4 DEG C/h, and sweating sessions are 2~8h, and sweating outlet temperature is 36~38 DEG C；
Temperature during crystals melt is 40~60 DEG C.
10. crystallization according to claim 8 couples the method for preparing electron level ethylene carbonate with rectifying, its feature exists
In the operating condition of the distillation process is：
Operated using rectification under vacuum, tower pressure interior force is 1.33~2.67kPa, and column bottom temperature is 100~130 DEG C, return time 3
~6h.
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