CN208917099U - A kind of 2,3- dichloropyridine preparation separating methanol reclaimer - Google Patents
A kind of 2,3- dichloropyridine preparation separating methanol reclaimer Download PDFInfo
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- CN208917099U CN208917099U CN201821168737.4U CN201821168737U CN208917099U CN 208917099 U CN208917099 U CN 208917099U CN 201821168737 U CN201821168737 U CN 201821168737U CN 208917099 U CN208917099 U CN 208917099U
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- reclaimer
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Abstract
The utility model discloses one kind 2,3- dichloropyridine preparation separating methanol reclaimer, it is characterized by comprising thin film evaporators and condenser, the thin film evaporator includes evaporator tube, the evaporator tube is externally provided with upper chuck and lower chuck, upper steam heating cavity and lower steam heating cavity are formed between the upper chuck and lower chuck and evaporator tube difference, the evaporator tube is provided with shaft, scraper plate is provided in the shaft, distributing device and gas-liquid separator are set in the evaporator tube, which is equipped with material inlet and secondary steam exports；The condenser includes condenser cylinder, intake antrum, heat exchange chamber and water chamber are set in the condenser cylinder, convection tube is set in the heat exchange chamber, which is equipped with methanol steam import and methanol liquid outlet and the methanol steam import connects with secondary steam outlet.The utility model after separating in generation mixed liquor for recycling methanol in 2,3- dichloropyridine preparation process.
Description
Technical field
The utility model belongs to a kind of 2,3- dichloropyridine preparation separating methanol reclaimer.
Background technique
When being prepared to 2,3- dichloropyridine, following technique can be used: in the presence of solvent and acid binding agent, with 2,
3,6- trichloropyridines are original in 250ml autoclave, put into 30g2,3,6- trichloropyridines, 90g methanol (solvent), 30g tri-
Ethamine (acid binding agent), 0.2g tri- (triphenylphosphine) radium chloride (I), 0.4g triphenylphosphine are passed through in nitrogen replacement reaction kettle empty
Gas, replacement completion, logical hydrogen are simultaneously warming up to 75 DEG C and are reacted (i.e. hydrogenation reaction), in reaction process reaction pressure gradually under
Drop fills into hydrogen and maintains reaction pressure between 2.0~2.2MPa, and successive reaction 18h, reaction terminates.
Since production object resulting after above-mentioned hydrogenation reaction is methanol (solvent), 2- chloropyridine, 2,3- dichloropyridine, water etc.
The generation mixture (liquid) of composition, in order to obtain target product 2,3- dichloro pyrrole, the generation mixture is after reaction kettle discharge
Need variant component separation.And the existing methanol isolated can generally mix that (hereinafter referred to as " methanol is mixed containing moisture content and a little impurity
Close liquid "), it is therefore necessary to further purification, in favor of recycling.
Utility model content
In order to which in view of one or more defects existing in the prior art, the utility model provides one kind 2,3- dichloro
Pyridine preparation separating methanol reclaimer.
To achieve the above object, the utility model provides the recycling of one kind 2,3- dichloropyridine preparation separating methanol and sets
It is standby, it is characterised in that: including thin film evaporator (1) and condenser (2)；The thin film evaporator (1) includes evaporator tube (1-
1) it, is arranged with upper chuck (1-2) and lower chuck (1-3) outside the evaporator tube (1-1), upper chuck (1-2) inner wall and the steaming
It sends out and forms upper steam heating cavity (1-4) between device cylinder (1-1) outer wall, the lower chuck (1-3) and the evaporator tube (1-1) are outside
It is formed between wall lower steam heating cavity (1-5), is rotatably provided with shaft (1-6) in the evaporator tube (1-1), the shaft
Scraper plate (1-7) is provided on (1-6), the upper end shaft (1-6) be pierced by after the evaporator tube (1-1) again with motor (1-8)
Connection is located at the shaft (1-6) above the scraper plate (1-7) and is equipped with distributing device (1-9) and gas-liquid separator (1-10), the gas
Liquid/gas separator (1-10) is located above the distributing device (1-9), the lower chuck (1-3) be equipped be lauched steam inlet (1-11),
Lower steam outlet (1-12) and down blow mouth (1-13), the upper chuck (1-2) be equipped with upper water vapour import (1-14),
Upper steam outlet (1-15) and upper sewage draining exit (1-16), the evaporator tube bottom (1-1) are equipped with discharge port (1-17), should
Evaporator tube (1-1) is equipped with material inlet (1-18) and secondary steam outlet (1-19), the material inlet (1-18) and cloth
The glassware position (1-9) is corresponding, and secondary steam outlet (1-19) is located above the gas-liquid separator (1-10)；The condenser
It (2) include condenser cylinder (2-1), the radial partition (2-2) in the inner cavity condenser cylinder (2-1) two is successively divided into water
Chamber (2-3), heat exchange chamber (2-4) and water chamber (2-5), the heat exchange chamber (2-4) is interior to be provided with multiple convection tubes (2-6), should
Convection tube one end (2-6) is connected to intake antrum (2-3), which is connected to water chamber (2-5), which hands over
It changes chamber (2-4) and exports (2-8) equipped with methanol steam import (2-7) and methanol liquid, the methanol steam import (2-7) and institute
It states secondary steam outlet (1-19) to connect, which is equipped with water inlet (2-9), which is equipped with water outlet
(2-10)。
Using the above scheme, when work, methyl alcohol mixed liquor enters in condenser cylinder (2-1) from material inlet (1-18),
And distributing device (1-9) of the methyl alcohol mixed liquor through rotation status acts on and on evaporator tube (1-1) inner wall is in continuous uniform
Circumferential waterfall so that methyl alcohol mixed liquor is being evenly heated by evaporator cylinder (1-1) inner wall membrane mode, heat transference efficiency
Greatly, heating surface is big, and evaporation intensity is high, and the overcurrent time is short；At work, the high-temperature water vapor from upper water vapour import (1-14) into
Enter by being formed between the upper chuck (1-2) inner wall and evaporator tube (1-1) outer wall in steam heating cavity (1-4), on this
High-temperature water vapor in steam heating cavity (1-4) is circumferentially evenly heated evaporator tube (1-1) upper inside wall, with realization pair
Methyl alcohol mixed liquor heating in the top evaporator tube (1-1), is evaporated methanol；In addition, can be by high-temperature water vapor from being lauched
Steam inlet (1-11) enters by forming down steam heating between lower chuck (1-3) inner wall and evaporator tube (1-1) outer wall
In chamber (1-5), the high-temperature water vapor in the lower steam heating cavity (1-5) is circumferentially equal to evaporator tube (1-1) lower inner wall
Even heating heats the methyl alcohol mixed liquor in the lower part evaporator tube (1-1) with realizing, is evaporated methanol；Due to steaming on this
Vapour heating chamber (1-4) and lower steam heating cavity (1-5) are provided separately, and steam will not be mutually mixed, it can be achieved that upper and lower temperature difference control
System makes steam heating cavity on this (1-4) interior vapor (steam) temperature that can reduce moisture evaporation lower than lower steam heating cavity (1-5) temperature, mention
High methanol vapour concentration can improve evaporation effect；Since the motor driven shaft (1-6) rotates, the shaft (1-6) drive is scraped
Plate (1-7), distributing device (1-9) and gas-liquid separator (1-10) rotation, due to the uniform rotation of scraper plate, by methyl alcohol mixed liquor object
Material constantly spreads to film on evaporator tube (1-1) inner wall evaporating surface, to achieve the effect that thin film evaporation, the evaporator cylinder
After methanol steam rising after being heated up evaporation in body (1-1) after gas-liquid separator (1-10) separation, the methanol of steam state
Then it can enter in heat exchange chamber (2-4) through methanol steam import (2-7) by convection current again through secondary steam outlet (1-19) discharge
It manages (2-6) heat exchange and is condensed into methyl alcohol mixed liquor, and be discharged in storage tank through methanol liquid outlet (2-8), purity can be high
Up to 98.5% or more, circular response utilization can be made.
Further, the evaporator tube (1-1) is equipped with Butterworth Hatch (1-20), the Butterworth Hatch (1-20) and cloth
The device position (1-9) is corresponding.The Butterworth Hatch (1-20) can avoid impurity from remaining convenient for the distributing device (1-9) processing of cleaning in time
And it blocks.
Further, radial baffle (2-11) is equipped in the heat exchange chamber (2-4).The radial baffle (2-11) limit
The methanol steam has been determined in heat exchange chamber (2-4) interior motion path, high/low temperature methanol steam is avoided to be mutually mixed, and prevents mixing dry
It disturbs, while increasing the methanol steam heat exchange residence time, improve condensation efficiency.
Further, the radial baffle (2-11) has multiple and axially hands in upper and lower along evaporator tube (1-1)
Mistake distribution.Since increasing methanol steam in heat exchange chamber (2-4) interior motion path, while resistance is generated to methanol vapor flow
And slow down, the methanol steam heat exchange residence time is greatly increased, condensation efficiency is improved.
Further, the scraper plate (1-7) is affixed by two crossbeams (1-71) and shaft (1-6) and two crossbeams
(1-71) is between the upper and lower every setting.Scraper plate (1-7) bearing up-down force support, intensity is reliable, is not easy to loosen and damage, extends and use the longevity
Life.
Further, the scraper plate (1-7) has multiple and is axially to be interspersed in left and right along the shaft (1-6).
Resistance when methyl alcohol mixed liquor flows down can be reduced, flow velocity is improved, evaporation time can be shortened.
Further, the scraper plate (1-7) uses fixed scraper plate and centrifugal scraper plate mixed configuration.
Further, on this steam outlet (1-15) be lauched steam inlet (1-11) and connected by outer tube (1-21).
Steam heating cavity (1-4) and lower steam heating cavity (1-5) tandem working, make high temperature section steam in upper steam heating cavity (1- on this
4) utilization is heated in, low-temperature zone is heated utilization in lower steam heating cavity (1-5), to realize different temperature zones to steam heat
The reasonable utilization of amount, can reduce heat waste, economical environment-protective.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model.
Specific embodiment
The utility model is described in further detail with reference to the accompanying drawings and examples:
It is shown in Figure 1: one kind 2,3- dichloropyridine preparation separating methanol reclaimer comprising thin film evaporator 1
With condenser 2；The thin film evaporator 1 includes evaporator tube 1-1, and upper chuck 1-2 is arranged with outside evaporator tube 1-1
With lower chuck 1-3, upper steam heating cavity 1-4 is formed between upper chuck 1-2 inner wall and evaporator tube 1-1 outer wall, under this
Lower steam heating cavity 1-5 is formed between collet 1-3 and evaporator tube 1-1 outer wall, is rotatably set in evaporator tube 1-1
Be equipped with shaft 1-6, be provided with scraper plate 1-7 on shaft 1-6, the upper end shaft 1-6 be pierced by after the evaporator tube 1-1 again with
Motor 1-8 connection, the shaft 1-6 above the scraper plate 1-7 are equipped with distributing device 1-9 and gas-liquid separator 1-10, the gas
Liquid/gas separator 1-10 is located above distributing device 1-7, and the lower chuck 1-3 is equipped with and is lauched steam inlet 1-11, lower water vapour
Export 1-12 and down blow mouth 1-13, the upper chuck 1-2 be equipped with upper water vapour import 1-14, upper steam outlet 1-15 and
Upper sewage draining exit 1-16, the bottom evaporator tube 1-1 are equipped with discharge port 1-17, and evaporator tube 1-1 is equipped with material inlet
1-18 and secondary steam export 1-19, and material inlet 1-18 is corresponding with the position distributing device 1-9, which exports 1-19
Above the gas-liquid separator 1-10；The condenser 2 includes condenser cylinder 2-1, the inner cavity condenser cylinder 2-1 two
A radial direction partition 2-2 is successively divided into intake antrum 2-3, heat exchange chamber 2-4 and water chamber 2-5, is provided in heat exchange chamber 2-4
Multiple convection tube 2-6, the one end convection tube 2-6 are connected to intake antrum 2-3, and the convection tube 2-6 other end and water chamber 2-5 connect
Logical, heat exchange chamber 2-4 is equipped with methanol steam import 2-7 and methanol liquid exports 2-8, the methanol steam import 2-7 and institute
It states and is connected between secondary steam outlet 1-19 by pipeline 2-12, intake antrum 2-3 is equipped with water inlet 2-9, and water chamber 2-5 is set
There is water outlet 2-10.
When work, first, methyl alcohol mixed liquor enters in condenser cylinder 2-1 from material inlet 1-18, and methyl alcohol mixed liquor
Distributing device 1-9 through rotation status acts on and is on evaporator tube 1-1 inner wall the circumferential waterfall of continuous uniform, so that first
Alcohol mixed liquor is being evenly heated by evaporator cylinder 1-1 inner wall membrane mode, and heat transference efficiency is big, and heating surface is big, evaporation intensity
Height, overcurrent time are short；Second, at work, which enters from upper water vapour import 1-14 by upper chuck 1-2
It is formed between wall and evaporator tube 1-1 outer wall in upper steam heating cavity 1-4, the high-temperature water on this in steam heating cavity 1-4
Steam is circumferentially evenly heated evaporator tube 1-1 upper inside wall, mixed to the methanol in the top evaporator tube 1-1 to realize
Liquid heating is closed, methanol is evaporated；Third can enter high-temperature water vapor by lower chuck 1-3 from steam inlet 1-11 is lauched
It is formed between wall and evaporator tube 1-1 outer wall in lower steam heating cavity 1-5, the high-temperature water in the lower steam heating cavity 1-5
Steam is circumferentially evenly heated evaporator tube 1-1 lower inner wall, mixed to the methanol in the lower part evaporator tube 1-1 to realize
Liquid heating is closed, methanol is evaporated；Since steam heating cavity 1-4 on this and lower steam heating cavity 1-5 are provided separately, steam will not
It is mutually mixed, it can be achieved that upper and lower temperature difference controls, makes on this that vapor (steam) temperature can be lower than lower steam heating cavity 1- in steam heating cavity 1-4
5 temperature can improve evaporation effect, energy saving, and the 4th, since motor driven shaft 1-6 is rotated, shaft 1-6 drive is scraped
Plate 1-7, distributing device 1-9 and gas-liquid separator 1-10 rotation, due to the uniform rotation of scraper plate, constantly by methyl alcohol mixed liquor material
Film is spread on evaporator tube 1-1 inner wall evaporating surface, to achieve the effect that thin film evaporation, quilt in evaporator tube 1-1
After methanol steam rising after heat temperature raising evaporation after gas-liquid separator 1-10 separation, the methanol of steam state can go out through secondary steam
Then mouth 1-19 discharge enters in heat exchange chamber 2-4 through methanol steam import 2-7 again is condensed into first by convection tube 2-6 heat exchange
Alcohol mixed liquor, and be discharged in storage tank through methanol liquid outlet 2-8, to recycle.
Further, the evaporator tube 1-1 be equipped with Butterworth Hatch 1-20, Butterworth Hatch 1-20 with distributing device 1-7
Set correspondence.Butterworth Hatch 1-20 can avoid impurity from remaining and block convenient for handling distributing device 1-7 cleaning in time.
Further, radial baffle 2-11 is equipped in the heat exchange chamber 2-4.Radial baffle 2-11 is defined
Methanol steam motion path in heat exchange chamber 2-4, avoids high/low temperature methanol steam from being mutually mixed, and prevents mixing from interfering, together
The Shi Zengjia methanol steam heat exchange residence time, improve condensation efficiency.
Further, the radial baffle 2-11 has multiple and is axially in staggeredly to divide up and down along evaporator tube 1-1
Cloth.Since increasing methanol steam motion path in heat exchange chamber 2-4, while resistance is generated to methanol vapor flow and is subtracted
Speed greatly increases the methanol steam heat exchange residence time, improves condensation efficiency.
Further, the scraper plate 1-7 is affixed by two crossbeam 1-71 and shaft 1-6 and two crossbeam 1-71 on
Lower interval setting.The support of scraper plate 1-7 bearing up-down force, intensity is reliable, is not easy to loosen and damage, prolongs the service life.
Further, the scraper plate 1-7 have it is multiple and for along the shaft 1-6 axially be in left and right be interspersed.It can subtract
Resistance when few methyl alcohol mixed liquor flows down, improves flow velocity, can shorten evaporation time.
Further, the scraper plate 1-7 uses fixed scraper plate and centrifugal scraper plate mixed configuration.Due to fixed scraper plate
Gap with evaporation stack shell inner wall is only 1-2mm, it is desirable that higher processing and installation accuracy are particularly suitable for extra-high viscosity and easily rise
Evaporation and concentration, precipitation or the purification of foam material.Using centrifugal scraper plate, can radially be slided when in scraper plate installation shaft, it should
When shaft drives scraper plate rotation, scraper plate is acted in centrifugal force and is radially got rid of to evaporator tube inner wall, while with shaft one
It rises and circles, and this of scraper plate scrapes, and makes methyl alcohol mixed liquor material on evaporator tube inner wall in membranaceous turbulent flow
State greatly improves heat transfer coefficient, at the same it is this continuously scrape, effectively inhibit overheat, dry wall and the knot of material
Phenomena such as dirty.The two mixed configuration can meet economic benefits and social benefits fruit, and overcome single function insufficient and reduce performance.
Further, on this steam outlet 1-15 be lauched steam inlet 1-11 and connected by outer tube 1-21.Steaming on this
Vapour heating chamber 1-4 and lower steam heating cavity 1-5 tandem working, steam heating cavity (1-4) and lower steam heating cavity 1-5 series connection on this
Work can enter back into quilt in the lower steam heating cavity 1-5 after high-temperature steam is heated utilization in upper steam heating cavity 1-4
Reheating utilizes, and since high temperature section steam heats evaporator tube 1-1 internal upper part, low-temperature zone steam is to evaporator tube 1-
Lower part is heated in 1, therefore high-temperature steam heating source is graded utilization, to realize different temperature zones to the reasonable abundant of steam heat
It utilizes, heat waste can be reduced, it is energy saving.
The preferred embodiments of the present invention have been described in detail above.It should be appreciated that the ordinary skill people of this field
Member according to the present utility model can conceive without creative work makes many modifications and variations.Therefore, all this technology necks
Technical staff passes through logic analysis, reasoning or limited reality according to the design of the utility model on the basis of existing technology in domain
Available technical solution is tested, it all should be within the scope of protection determined by the claims.
Claims (8)
1. one kind 2,3- dichloropyridine preparation separating methanol reclaimer, it is characterised in that: including thin film evaporator (1) and cold
Condenser (2)；
The thin film evaporator (1) includes evaporator tube (1-1), is arranged with upper chuck (1-2) outside the evaporator tube (1-1)
With lower chuck (1-3), upper steam heating cavity (1- is formed between upper chuck (1-2) inner wall and evaporator tube (1-1) outer wall
4) lower steam heating cavity (1-5), the evaporator tube, are formed between the lower chuck (1-3) and evaporator tube (1-1) outer wall
It is rotatably provided with shaft (1-6) in (1-1), is provided with scraper plate (1-7) in the shaft (1-6), which is pierced by
It is connect again with motor (1-8) after the evaporator tube (1-1), is located at the shaft (1-6) above the scraper plate (1-7) and is equipped with
Distributing device (1-9) and gas-liquid separator (1-10), which is located above the distributing device (1-9), under described
Collet (1-3) is equipped with and is lauched steam inlet (1-11), lower steam outlet (1-12) and down blow mouth (1-13), the upper folder
It covers (1-2) and is equipped with upper water vapour import (1-14), upper steam outlet (1-15) and upper sewage draining exit (1-16), the evaporator cylinder
The body bottom (1-1) is equipped with discharge port (1-17), which is equipped with material inlet (1-18) and secondary steam goes out
Mouth (1-19), the material inlet (1-18) is corresponding with the distributing device position (1-9), and secondary steam outlet (1-19) is located at the gas
Above liquid/gas separator (1-10)；
The condenser (2) includes condenser cylinder (2-1), the radial partition (2-2) in the inner cavity condenser cylinder (2-1) two
Successively it is divided into intake antrum (2-3), heat exchange chamber (2-4) and water chamber (2-5), is provided in the heat exchange chamber (2-4) multiple
Convection tube (2-6), the convection tube one end (2-6) are connected to intake antrum (2-3), convection tube (2-6) other end and water chamber (2-
5) be connected to, which is equipped with methanol steam import (2-7) and methanol liquid and exports (2-8), the methanol steam into
Mouth (2-7) connects with secondary steam outlet (1-19), which is equipped with water inlet (2-9), the water chamber (2-
5) it is equipped with water outlet (2-10).
2. one kind 2,3- dichloropyridine preparation separating methanol reclaimer as described in claim 1, it is characterised in that: described
Evaporator tube (1-1) is equipped with Butterworth Hatch (1-20), and the Butterworth Hatch (1-20) is corresponding with the distributing device position (1-9).
3. one kind 2,3- dichloropyridine preparation separating methanol reclaimer as described in claim 1, it is characterised in that: described
Radial baffle (2-11) is equipped in heat exchange chamber (2-4).
4. one kind 2,3- dichloropyridine preparation separating methanol reclaimer as claimed in claim 3, it is characterised in that: described
Radial baffle (2-11) has multiple and is axially in be interspersed up and down along evaporator tube (1-1).
5. special such as a kind of 2,3- dichloropyridine preparation separating methanol reclaimer of any of claims 1-4
Sign is: the scraper plate (1-7) is affixed by two crossbeams (1-71) and shaft (1-6) and two crossbeams (1-71) between the upper and lower
Every setting.
6. one kind 2,3- dichloropyridine preparation separating methanol reclaimer as claimed in claim 5, it is characterised in that: described
Scraper plate (1-7) has multiple and is axially to be interspersed in left and right along the shaft (1-6).
7. one kind 2,3- dichloropyridine preparation separating methanol reclaimer as claimed in claim 5, it is characterised in that: described
Scraper plate (1-7) uses fixed scraper plate and centrifugal scraper plate mixed configuration.
8. one kind 2,3- dichloropyridine preparation separating methanol reclaimer as described in claim 1, it is characterised in that: on this
Steam outlet (1-15) be lauched steam inlet (1-11) and connected by outer tube (1-21).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821168737.4U CN208917099U (en) | 2018-07-24 | 2018-07-24 | A kind of 2,3- dichloropyridine preparation separating methanol reclaimer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821168737.4U CN208917099U (en) | 2018-07-24 | 2018-07-24 | A kind of 2,3- dichloropyridine preparation separating methanol reclaimer |
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| Publication Number | Publication Date |
|---|---|
| CN208917099U true CN208917099U (en) | 2019-05-31 |
Family
ID=66694477
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201821168737.4U Active CN208917099U (en) | 2018-07-24 | 2018-07-24 | A kind of 2,3- dichloropyridine preparation separating methanol reclaimer |
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| CN (1) | CN208917099U (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110947195A (en) * | 2019-12-30 | 2020-04-03 | 无锡市志成生化工程装备有限公司 | Multi-jacket evaporator |
| CN111013172A (en) * | 2019-12-25 | 2020-04-17 | 李武林 | Wiped film evaporator |
| CN112755556A (en) * | 2021-01-06 | 2021-05-07 | 扬州大学 | Wiped film evaporator and using method thereof |
| CN112807712A (en) * | 2021-01-05 | 2021-05-18 | 中国神华煤制油化工有限公司 | Evaporator with a heat exchanger |
-
2018
- 2018-07-24 CN CN201821168737.4U patent/CN208917099U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013172A (en) * | 2019-12-25 | 2020-04-17 | 李武林 | Wiped film evaporator |
| CN110947195A (en) * | 2019-12-30 | 2020-04-03 | 无锡市志成生化工程装备有限公司 | Multi-jacket evaporator |
| CN112807712A (en) * | 2021-01-05 | 2021-05-18 | 中国神华煤制油化工有限公司 | Evaporator with a heat exchanger |
| CN112807712B (en) * | 2021-01-05 | 2023-05-02 | 中国神华煤制油化工有限公司 | Evaporator |
| CN112755556A (en) * | 2021-01-06 | 2021-05-07 | 扬州大学 | Wiped film evaporator and using method thereof |
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