CN107362567A - A kind of distillation system and solvent purification system - Google Patents
A kind of distillation system and solvent purification system Download PDFInfo
- Publication number
- CN107362567A CN107362567A CN201710755870.3A CN201710755870A CN107362567A CN 107362567 A CN107362567 A CN 107362567A CN 201710755870 A CN201710755870 A CN 201710755870A CN 107362567 A CN107362567 A CN 107362567A
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- Prior art keywords
- distillation system
- rectifying
- temperature
- return tank
- temperature sensor
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4205—Reflux ratio control splitter
Abstract
A kind of distillation system and solvent purification system, it is related to chemical products technical field of purification, the distillation system includes rectifying still, rectifying column, condenser and the return tank being sequentially connected, and is provided with the first temperature sensor at the top of rectifying column, the bottom of return tank is provided with second temperature sensor.The temperature of return tank inner condensat liquid can be accurately determined by second temperature sensor, temperature at the top of rectifying column can accurately be determined by the first temperature sensor, the temperature conditions of integrated condensation liquid and the temperature conditions of rectifying column tower top, to determine to be back to the amount of the condensate liquid of tower top, so that in the range of the temperature of tower top maintains a relative constancy, ensure the effect of rectifying.The equipment of the distillation system is simple and convenient to operate, and accurately reflux ratio is controlled using temperature as Con trolling index, meets the rectifying requirement of fine chemistry industry.The solvent purification system includes above-mentioned distillation system.Its equipment is simple and convenient to operate, and can accurately control reflux ratio, reaches preferable purification effect.
Description
Technical field
The present invention relates to chemical products technical field of purification, in particular to a kind of distillation system and solvent purification
System.
Background technology
Rectifying be it is a kind of liquid mixture is obtained the distillating method of high-purity separation using backflow, be industrial application most
Wide liquid mixture lock out operation, is widely used in the departments such as oil, chemical industry, light industry, food, metallurgy.In distillation operation, by
Rectifying column tower top returns to the ratio of the phegma flow L and overhead product flow D in tower, as reflux ratio.The size of reflux ratio,
Separating effect and economy to distillation process have important influence.Therefore, in distillation design, reflux ratio is that a need are recognized
Very selected parameter.
But in the prior art, want there is one more to accurately control to reflux ratio, then need the control for being related to complexity
System processed, cause the higher of production cost.Cost Problems are limited to, reflux ratio can only control general at one in many cases
In the range of, this is not by far up to the mark for fine chemistry industry.Therefore, a kind of equipment is developed to be simple and convenient to operate and energy
The distillation system of accurate control reflux ratio is very necessary.
The content of the invention
It is an object of the invention to provide a kind of distillation system, its equipment is simple and convenient to operate, it is not necessary to complicated control
System, you can meet accurate reflux ratio control, meet the rectifying requirement of fine chemistry industry.
Another object of the present invention is to provide a kind of solvent purification system, it includes above-mentioned distillation system, the letter of its equipment
It is single, easy to operate, purification effect is good, available for large-scale industrial production.
What embodiments of the invention were realized in：
A kind of distillation system, including rectifying still, rectifying column, condenser and return tank, rectifying still, rectifying column, condenser and
Return tank is sequentially connected, and return tank is communicated to the tower top of rectifying column by reflux line, is provided with the top of rectifying column for surveying
Determine the first temperature sensor of temperature in rectifying column, the bottom of return tank is provided with for determining return tank inner condensat liquid temperature
Second temperature sensor.
Further, in the other preferred embodiments of the present invention, distance of first temperature sensor apart from rectifying column top
For the 5~10% of rectifying tower height degree.
Further, in the other preferred embodiments of the present invention, the first temperature sensor is included along rectifying column length direction
The distance between spaced two sensitive measurement plates, two sensitive measurement plates are the 0.5~3% of rectifying tower height degree.
Further, in the other preferred embodiments of the present invention, the bottom of return tank is provided with phegma outlet and finished product
Outlet, phegma outlet connect with reflux line, and product outlet connects with finished pot, and phegma outlet is higher than product outlet, returns
Flow liquid outlet is provided with extraction valve.
Further, in the other preferred embodiments of the present invention, reflux line includes one section of U-shaped liquid sealing pipe.
Further, in the other preferred embodiments of the present invention, distillation system is also included to control extraction valve opening and closing
First controller, the first controller electrically connect with the first temperature sensor.
Further, in the other preferred embodiments of the present invention, exhaust outlet is provided with the top of return tank, exhaust outlet is with dividing
The input connection of son sieve adsorption column, the output end of molecular sieve adsorption post are provided with motor-driven valve.
Further, in the other preferred embodiments of the present invention, it is provided with and is used between exhaust outlet and molecular sieve adsorption post
Hold discoloration silica gel regards cup.
Further, in the other preferred embodiments of the present invention, distillation system also includes providing refrigerant for condenser
Cold medium feedway and second controller for controlling refrigerant flow, second controller and second temperature sensor
Electrical connection.
A kind of solvent purification system, it includes above-mentioned distillation system.
The beneficial effect of the embodiment of the present invention is：
The invention provides a kind of distillation system, including rectifying still, rectifying column, condenser and return tank, rectifying still, rectifying
Tower, condenser and return tank are sequentially connected, and the first temperature sensor is provided with the top of rectifying column, and the bottom of return tank is provided with
Second temperature sensor.The temperature of return tank inner condensat liquid can be accurately determined by second temperature sensor, passes through the first temperature
Degree sensor can accurately determine the temperature at the top of rectifying column, the temperature conditions of integrated condensation liquid and the temperature feelings of rectifying column tower top
Condition, to determine to be back to the amount of the condensate liquid of tower top, so that in the range of the temperature of tower top maintains a relative constancy, from
And ensure the effect of rectifying.The equipment of the distillation system is simple and convenient to operate, and is accurately controlled back using temperature as Con trolling index
Ratio is flowed, meets the rectifying requirement of fine chemistry industry.
The embodiment of the present invention additionally provides a kind of solvent purification system, and it includes above-mentioned distillation system.Its equipment is simple, behaviour
Facilitate, reflux ratio is accurately controlled by straightforward procedure, preferable purification effect can be reached, it is raw available for large-scale industry
Production.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below by embodiment it is required use it is attached
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, therefore be not construed as pair
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
A kind of connection diagram for distillation system that Fig. 1 is provided by the embodiment of the present invention；
A kind of schematic diagram of the condenser for distillation system that Fig. 2 is provided by the embodiment of the present invention；
A kind of schematic diagram of the gas-liquid separator for distillation system that Fig. 3 is provided by the embodiment of the present invention；
A kind of workflow diagram for distillation system that Fig. 4 is provided by the embodiment of the present invention.
Icon：10- distillation systems；100- rectifying stills；200- rectifying columns；The temperature sensors of 210- first；The sensitive surveys of 211-
Template；300- condensers；310- hot side entrances；320- hot side outlets；330- cold side input ports；340- cold side outlet ports；400- flows back
Tank；410- reflux lines；411-U type liquid sealing pipes；420- phegmas export；430- product outlets；440- second temperature sensors；
450- produces valve；460- exhaust outlets；470- molecular sieve adsorption posts；480- motor-driven valves；490- regards cup；500- finished pots.
Embodiment
To make the purpose, technical scheme and advantage of embodiment of the present invention clearer, implement below in conjunction with the present invention
Accompanying drawing in mode, the technical scheme in embodiment of the present invention is clearly and completely described, it is clear that described reality
The mode of applying is a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained under the premise of creative work is not made, belongs to the present invention
The scope of protection.Therefore, below the detailed description of the embodiments of the present invention to providing in the accompanying drawings be not intended to limit will
The scope of the present invention of protection is sought, but is merely representative of the selected embodiment of the present invention.Based on the embodiment in the present invention,
The every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, belong to this
Invent the scope of protection.
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", " on ", " under ", "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outer ", " up time
The orientation or position relationship of the instruction such as pin ", " counterclockwise " are based on orientation shown in the drawings or position relationship, are for only for ease of
Description is of the invention to be described with simplified, rather than the equipment or element of instruction or hint meaning must be with specific orientation, Yi Te
Fixed azimuth configuration and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are only used for describing purpose, and it is not intended that instruction or hint relative importance
Or the implicit quantity for indicating indicated technical characteristic.Thus, define " first ", the feature of " second " can be expressed or
Implicitly include one or more this feature.In the description of the invention, " multiple " are meant that two or more,
Unless otherwise specifically defined.
In the present invention, unless otherwise clearly defined and limited, term " installation ", " connected ", " connection ", " fixation " etc.
Term should be interpreted broadly, for example, it may be fixedly connected or be detachably connected, or integrally；Can be that machinery connects
Connect or electrically connect；Can be joined directly together, can also be indirectly connected by intermediary, can be in two elements
The connection in portion or the interaction relationship of two elements.For the ordinary skill in the art, can be according to specific feelings
Condition understands the concrete meaning of above-mentioned term in the present invention.
In the present invention, unless otherwise clearly defined and limited, fisrt feature second feature it " on " or it " under "
Can directly it be contacted including the first and second features, it is not directly to contact but pass through it that can also include the first and second features
Between other characterisation contact.Moreover, fisrt feature second feature " on ", " top " and " above " to include first special
Sign is directly over second feature and oblique upper, or is merely representative of fisrt feature level height and is higher than second feature.Fisrt feature exists
Second feature " under ", " lower section " and " following " fisrt feature that includes are immediately below second feature and obliquely downward, or be merely representative of
Fisrt feature level height is less than second feature.
Embodiment
The present embodiment provides a kind of distillation system 10, and shown in reference picture 1, it includes rectifying still 100, rectifying column 200, condensation
Device 300 and return tank 400.Wherein, rectifying still 100, rectifying column 200, condenser 300 and return tank 400 are sequentially connected, return tank
400 are communicated to the tower top of rectifying column 200 by reflux line 410.
As shown in figure 1, rectifying still 100 is used to hold the mixed solution for treating rectifying and mixed solution heated to be formed
Mixed gas.The gaseous phase outlet at the top of rectifying still 100 connects with the gas phase entrance of the bottom of rectifying column 200, is produced in rectifying still 100
Mixed gas can be entered by the gas phase entrance of the bottom of rectifying column 200 rectifying is carried out in rectifying column 200.Wherein, rectifying still 100
Preferably use enamel glass chuck rectifying still, in chuck can admittance deep fat rectifying still 100 is heated.Rectifying still 100 is set
Paddle agitator (not shown) is equipped with, its rotating speed reaches more than 300rpm, and the mixed solution that it can be made internal obtains sufficiently
Stirring, allows even heat to be distributed in mixed solution, increases the efficiency of rectifying.
The internal diameter of rectifying column 200 is 4~220cm, is highly 2~30m, filling glass spring filler, stainless steel west in tower
At least one of tower ring, stainless steel Pall ring, stainless steel structured packing and ceramic packing.The bottom of rectifying column 200 is filled with
The Anhydrous potassium carbonate filler that one section of height is 0.5~2m, to remove a small amount of steam in mixed gas.The top of rectifying column 200
Portion is provided with the first temperature sensor 210 for determining temperature in rectifying column 200, and the first temperature sensor 210 is apart from rectifying
The distance on the top of tower 200 is the 5~10% of the height of rectifying column 200.First temperature sensor 210 is used for the top of rectifying column 200
Temperature measure, allow user to adjust the amount for the condensate liquid for being back to tower top according to temperature change.
Further, the first temperature sensor 210 is included along the spaced two sensitive surveys of the length direction of rectifying column 200
Template 211, by the temperature measuring of two different zones, can prevent amount of localized heat from accumulating, caused by measurement error.Two spirits
The distance between quick measurement plate 211 is the 0.5~3% of the height of rectifying column 200.Found by inventor's creative work, at this
Under spacing, degree of disturbance is smaller between two sensitive measurement plates 211, and the data measured are more accurate.
As depicted in figs. 1 and 2, the gaseous phase outlet at the top of rectifying column 200 is communicated to the hot side entrance 310 of condenser 300, cold
The hot side outlet 320 of condenser 300 is communicated to the input of return tank 400.The cold side input port 330 of condenser 300 is communicated to cold Jie
Matter feedway (not shown), the cold side outlet port 340 of condenser 300 are communicated to cold medium retracting device (not shown).By rectifying
The gaseous component self-heating side entrance 310 of the gaseous phase outlet output at the top of tower 200 enters in condenser 300, is situated between with the refrigeration of cold side
Heat exchange occurs for matter, is condensed into condensate liquid, and be delivered to return tank 400 by hot side outlet 320.Wherein, refrigerant can be
Chilled water, anti-icing fluid, cold air etc..It is worth noting that, in the other preferred embodiments of the present invention, cold medium feedway and
Cold medium retracting device can be integrated into the circulating pump with refrigerating plant, so as to realize recycling for refrigerant.
As shown in figure 3, the bottom of return tank 400 is provided with phegma outlet 420 and product outlet 430, phegma outlet
420 connect with reflux line 410, and product outlet 430 connects with finished pot 500.By conveyed in condenser 300 Lai condensate liquid one
Part is delivered to the top of rectifying column 200 by reflux line 410, and another part is then exported to finished pot 500 by product outlet 430
Store stand-by.The bottom of return tank 400 is provided with the second temperature sensor for determining the inner condensat liquid temperature of return tank 400
440, user can be according to the temperature of condensate liquid, to determine to be back to the amount of the condensate liquid of tower top, so as to ensure the temperature of tower top
It is stable.
Further, phegma outlet 420 is higher than product outlet 430, and phegma outlet 420 is provided with extraction valve 450.Adopt
Go out valve 450 may be controlled to product outlet 430 condensation flow quantity, when produce valve 450 be opened into maximum when, condensate liquid all via
Product outlet 430 is delivered to finished pot 500, and hydrops will not be formed in return tank 400, and liquid level can not reach phegma outlet 420
Height, now no condensate liquid be back to the top of rectifying column 200.And by controlling extraction valve 450 to reduce product outlet 430
Condensation flow quantity, then can make slowly to form hydrops in return tank 400, when the height of hydrops cover phegma outlet 420 when,
Then condensate liquid can be back to the top of rectifying column 200 via reflux line 410.Therefore, by adjusting the cold of product outlet 430
Condensate flow, the amount that control simultaneously is back to the condensate liquid at the top of rectifying column 200 can be used for, and be delivered to the condensation of production tube
The amount of liquid.
Further, as shown in figures 1 and 3, the top of return tank 400 is provided with exhaust outlet 460, and exhaust outlet 460 is with dividing
The input connection of son sieve adsorption column 470, preferably 4A molecular sieve adsorptions post 470, the output end of molecular sieve adsorption post 470 are set
There are motor-driven valve 480, preferably electrical ball valve.Motor-driven valve 480 is opened when rectifying starts, to avoid the internal pressure of distillation system 10
It is too high.Meanwhile it is closed at the end of rectifying, the inside of distillation system 10 and atmosphere, the vapor completely cut off in air are avoided.
Molecular sieve adsorption post 470 can then play good water sorption, even if there is part water vapour to pass through motor-driven valve 480, also can
Adsorbed by the molecular sieve in molecular sieve adsorption post 470, so as to avoid to being polluted inside distillation system 10.Preferably, arrange
It is provided between gas port 460 and molecular sieve adsorption post 470 and regards cup 490 for holding discoloration silica gel, passes through the change for the silica gel that changes colour
Pornographic condition, it can preferably monitor whether that vapor enters and whether molecular sieve column fails, if the discoloration silicon in cup 490
When glue changes colour, then discoloration silica gel and molecular sieve adsorption post 470 should be changed in time.
Further, reflux line 410 includes one section of U-shaped liquid sealing pipe 411, and the U-shaped liquid sealing pipe 411 returns in no condensate liquid
One section of fluid column can be remained during stream, in it, this section of fluid column can play a part of fluid-tight, it is ensured that the gaseous component in rectifying column 200
It will not be entered by reflux line 410 in return tank 400.
Preferably, in embodiment, distillation system 10 is also included to control the first controller that extraction valve 450 is opened and closed
(not shown), the first controller electrically connect with the first temperature sensor 210.Further, distillation system 10 also includes being used to control
The second controller (not shown) of refrigerant flow processed, second controller electrically connect with second temperature sensor 440.
As shown in figure 4, in working condition, second temperature sensor 440 gathers the temperature of condensate liquid in return tank 400,
When the condensate temperature that second temperature sensor 440 is monitored in return tank 400 is too high, then the second control is delivered a signal to
Device, the flow of second controller control increase refrigerant, to increase the condensation effect of condenser 300, to reduce condensate liquid
Temperature, so as to which the condensate liquid in return tank 400 is maintained in a metastable temperature range, advantageously in backflow
Amount to the condensate liquid at the top of rectifying column 200 is judged, is more accurately controlled with reaching the temperature pushed up to rectifying column 200.
Meanwhile first temperature sensor 210 temperature at the top of rectifying column 200 is detected, when the first temperature sensor 210 monitors
When temperature is relatively low, then the first controller is delivered a signal to, the first controller control extraction valve 450 is opened greatly, and essence is back to reduce
The amount of the condensate liquid at the top of tower 200 is evaporated, temperature is gone up.Conversely, when the first temperature sensor 210 monitors temperature drift
When, then the first controller is delivered a signal to, the first controller control extraction valve 450 turns down, and being back to rectifying column 200 with increase pushes up
The amount of the condensate liquid in portion, is minimized temperature.Pass through the cooperation of the first temperature sensor 210 and second temperature sensor 440
Effect, you can keep the stabilization of the head temperature of rectifying column 200, reach preferable purification effect.
The embodiment of the present invention additionally provides a kind of solvent purification system, and it includes above-mentioned distillation system 10.Pass through rectifying system
The accurate control for 10 pairs of reflux ratios of uniting, the solvent purification system can reach preferable purification effect, available for large-scale industry
Production.
In summary, the invention provides a kind of distillation system, including rectifying still, rectifying column, condenser and return tank, essence
Evaporate kettle, rectifying column, condenser and return tank to be sequentially connected, the first temperature sensor is provided with the top of rectifying column, return tank
Bottom is provided with second temperature sensor.The temperature of return tank inner condensat liquid can be accurately determined by second temperature sensor,
Temperature at the top of rectifying column, the temperature conditions and rectifying tower of integrated condensation liquid can accurately be determined by the first temperature sensor
The temperature conditions on top, to determine to be back to the amount of the condensate liquid of tower top, so that the temperature of tower top maintains a relative constancy
In the range of, so as to ensure the effect of rectifying.The equipment of the distillation system is simple and convenient to operate, and Con trolling index is used as using temperature
Reflux ratio accurately is controlled, meets the rectifying requirement of fine chemistry industry.
The embodiment of the present invention additionally provides a kind of solvent purification system, and it includes above-mentioned distillation system.Its equipment is simple, behaviour
Facilitate, reflux ratio is accurately controlled by straightforward procedure, preferable purification effect can be reached, it is raw available for large-scale industry
Production.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. a kind of distillation system, including rectifying still, rectifying column, condenser and return tank, the rectifying still, the rectifying column, institute
To state condenser and the return tank is sequentially connected, the return tank is communicated to the tower top of the rectifying column by reflux line, its
It is characterised by, the first temperature sensor for determining temperature in the rectifying column is provided with the top of the rectifying column, it is described
The bottom of return tank is provided with the second temperature sensor for determining the return tank inner condensat liquid temperature.
2. distillation system according to claim 1, it is characterised in that first temperature sensor is apart from the rectifying column
The distance on top is the 5~10% of the rectifying tower height degree.
3. distillation system according to claim 2, it is characterised in that first temperature sensor is included along the rectifying
The distance between the spaced two sensitive measurement plates of tower length direction, two described sensitive measurement plates are the rectifying tower height
The 0.5~3% of degree.
4. distillation system according to claim 1, it is characterised in that the bottom of the return tank is provided with phegma outlet
And product outlet, the phegma outlet connect with the reflux line, the product outlet connects with finished pot, the backflow
Liquid outlet is higher than the product outlet, and the phegma outlet is provided with extraction valve.
5. distillation system according to claim 4, it is characterised in that the reflux line includes one section of U-shaped liquid sealing pipe.
6. distillation system according to claim 5, it is characterised in that the distillation system is also included to control described adopt
Go out the first controller of valve opening and closing, first controller electrically connects with first temperature sensor.
7. distillation system according to claim 1, it is characterised in that exhaust outlet, institute are provided with the top of the return tank
The input that exhaust outlet is stated with molecular sieve adsorption post connects, and the output end of the molecular sieve adsorption post is provided with motor-driven valve.
8. distillation system according to claim 7, it is characterised in that between the exhaust outlet and the molecular sieve adsorption post
It is provided with and regards cup for holding discoloration silica gel.
9. distillation system according to claim 1, it is characterised in that the distillation system also includes carrying for the condenser
Cold medium feedway for refrigerant and the second controller for controlling refrigerant flow, the second controller with
The second temperature sensor electrical connection.
10. a kind of solvent purification system, it is characterised in that including the distillation system as described in any one of claim 1~9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710755870.3A CN107362567A (en) | 2017-08-29 | 2017-08-29 | A kind of distillation system and solvent purification system |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710755870.3A CN107362567A (en) | 2017-08-29 | 2017-08-29 | A kind of distillation system and solvent purification system |
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| CN201710755870.3A Pending CN107362567A (en) | 2017-08-29 | 2017-08-29 | A kind of distillation system and solvent purification system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096169A (en) * | 2018-09-29 | 2018-12-28 | 天津科林泰克科技有限公司 | A kind of purification alpha-pyrrolidone steams the device and method of slag |
| CN109157860A (en) * | 2018-09-17 | 2019-01-08 | 大丰跃龙化学有限公司 | A kind of negative pressure rectifying still condensing reflux structure |
| CN110559677A (en) * | 2019-09-25 | 2019-12-13 | 南通百川新材料有限公司 | Efficient trimethylolpropane synthetic solvent rectification tail gas recovery device |
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| CN102432769A (en) * | 2011-07-25 | 2012-05-02 | 漳州亚邦化学有限公司 | Unsaturated polyester resin and production method thereof |
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| CN109157860A (en) * | 2018-09-17 | 2019-01-08 | 大丰跃龙化学有限公司 | A kind of negative pressure rectifying still condensing reflux structure |
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| CN110559677A (en) * | 2019-09-25 | 2019-12-13 | 南通百川新材料有限公司 | Efficient trimethylolpropane synthetic solvent rectification tail gas recovery device |
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