CN202155061U - High vacuum distillation purification device - Google Patents
High vacuum distillation purification device Download PDFInfo
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- CN202155061U CN202155061U CN201120217305XU CN201120217305U CN202155061U CN 202155061 U CN202155061 U CN 202155061U CN 201120217305X U CN201120217305X U CN 201120217305XU CN 201120217305 U CN201120217305 U CN 201120217305U CN 202155061 U CN202155061 U CN 202155061U
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- liquid separator
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- high vacuum
- film evaporator
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Abstract
The utility model relates to a high vacuum distillation purification device, which comprises a falling film evaporator, a gas-liquid separator, a U-tube heater, a U-tube condenser, a material circulating pump, a liquid receiving tank, a cold trap and a vacuum pump unit (Microsoft user 1). The high vacuum distillation purification device is characterized in that the gas-liquid separator is directly connected with the falling film evaporator and the U-tube condenser, and the U-tube heater is arranged at the bottom of the gas-liquid separator. The high vacuum distillation purification device has the advantages that by the aid of a direct-connected compact structure, large-caliber heating tubes of the falling film evaporator and the internal condenser, the internal airflow resistance of the device is reduced, the quantity of leaked air of the device is decreased, high vacuum is ensured, materials evaporate by the aid of falling films so that the device is high in heat transfer efficiency, high in treatment capacity, not easy to scale and the like, thermal polymerization or thermal decomposition and the like are decreased effectively so that the device is high in product yield and quality, a certain energy-saving effect is achieved, and additionally the device is simple in structure, low in manufacturing cost, flexible in operation and capable of being operated continuously and intermittently.
Description
Technical field
The utility model relates to a kind of high vacuum distillation purifying plant, can be applied to the higher boiling in the medication chemistry industry, the distillation purification of heat-sensitive substance.
Background technology
At present, known high vacuum distillation device has molecular clock, short-path distillation etc., and the distillation that they are fit to below the vacuum 1.33Pa is purified.Need in vacuum 1.33～266Pa scope, distill the material of purifying, if use molecular clock, short course distillation device, then plant investment and operating cost are higher, and the disposal ability of above two kinds of devices is less than normal.The distillation of above-mentioned substance is purified and is adopted conventional vacuum still distillation device usually.Vacuum still distillation device generally has two kinds of forms.The first is made up of the distillation still, the condenser that separate, and distillation still is connected with pipeline with condenser, the subsidiary mechanical stirring device that has, and the gas-flow resistance of this kind form distilling apparatus is big, is difficult for reaching the condition of high vacuum degree requirement; It two is made up of distillation still and built-in condenser, and the gas-flow resistance of this kind form distilling apparatus has greatly improved than first kind.The normally intermittently operated of vacuum still distillation device, heat transfer efficiency is extremely low, and disposal ability is very little.For example proportion is 1100kg/m
3Material; The differential static pressure that the every 50mm of its liquid phase height is produced is about 4mmHg (50 * 1.1 ÷ 13.6=4.04); And this differential static pressure is 300 ℃ a material for boiling point under the normal pressure, and when gaseous pressure was 1mmHg, 50mm place boiling point elevation value was about 38 ℃ under its liquid level; That is to say that material below the liquid level 50mm is overheated serious and can not seethe with excitement, the conventional according to statistics effective heat transfer area of vacuum still distillation device has only 10～20% of total heat conduction area.In addition, because the material heated time is long, add that the liquid phase static pressure causes the material elevation of boiling point and causes material overheated serious, oxidation, polymerization, coking, carbonization or cracking take place in material easily, finally cause the yield of product and quality to descend.
Summary of the invention
The utility model technical problem to be solved is to propose a kind of high vacuum distillation purifying plant, exists yield and the low shortcoming of content that heat transfer efficiency is low, disposal ability is little, oxidation, polymerization, coking, carbonization or cracking and product take place material easily with the high vacuum distillation device that overcomes prior art.
The utility model is to solve the problems of the technologies described above the technical scheme that is adopted: the high vacuum distillation purifying plant includes falling film evaporator, gas-liquid separator, U type pipe heater, U type pipework condensation device, material circulating pump at least, receives flow container, cold-trap and vavuum pump unit; The charging aperture at described falling film evaporator top is connected with the outlet of material circulating pump; Material circulation pump intake is connected with the discharging opening of gas-liquid separator bottom; Be connected with the discharging opening of U type pipework condensation device by the charging aperture of flow container; Gas-liquid separator is connected with receiving flow container through balance pipe, and the air inlet of cold-trap is connected with the exhaust outlet of U type pipework condensation device, and the air inlet of vavuum pump unit is connected with the exhaust outlet of cold-trap; It is characterized in that described gas-liquid separator directly links to each other with U type pipework condensation device with falling film evaporator, the bottom of gas-liquid separator is provided with U type pipe heater.
Press such scheme, described falling film evaporator is a falling film evaporator in the vertical tube, and its primary structure includes a vertically arranged shell-and-tube heat exchanger, and described shell-and-tube heat exchanger adopts the heat exchanger tube of big caliber, and its draw ratio is 50～100.
Press such scheme, described gas-liquid separator is a horizontal vessel, and its diameter can guarantee that air velocity is at 5～15m/s.
Press such scheme, the housing diameter of described U type pipe heater is 1/2～1/3 of a gas-liquid separator diameter.
Press such scheme, described U type pipework condensation device includes one group of vertically arranged U type heat exchanger tube, and its diameter is 0.45～0.65 times of described gas-liquid separator diameter.
Press such scheme; The lower end of described U type pipework condensation device is provided with condensate liquid seal pot and following condensate liquid seal pot; The described diameter of going up the condensate liquid seal pot is 0.4～0.5 times of U type pipework condensation device diameter; Following seal pot diameter is 0.7～0.8 of a top seal pot diameter, and the spacing of last condensate liquid seal pot and following condensate liquid seal pot is 1.5～1.8 times of following condensate liquid seal pot diameter.
Introduce the structure and the function thereof of each parts of the utility model below in detail:
Falling film evaporator of the present invention is a falling film evaporator in the vertical tube, and its primary structure includes a vertically arranged shell-and-tube heat exchanger, falls for reducing pressure, adopts the heat exchanger tube of big caliber, and its draw ratio is 50～100.Because material is film forming evaporation in this falling film evaporation organ pipe, does not have the effect of liquid phase static pressure, its evaporation intensity can reach 10 times of conventional vacuum still distillation device.In addition,, can reduce the generation of situation such as oxidation, polymerization, coking, carbonization or cracking greatly, reach the purpose that improves product yield and quality because the material heated time is short.
The described gas-liquid separator of the utility model is a horizontal vessel, and the big I of its diameter guarantees that air velocity is at 5～15m/s.For reducing gas-flow resistance, guarantee vacuum, gas-liquid separator directly is connected with U type pipework condensation device with falling film evaporator, and its bottom is provided with U type pipe heater.Because the air velocity in this gas-liquid separator is low; Add with falling film evaporator and directly be connected with U type pipework condensation device; Do not had and conventional falling film evaporator and U type pipework condensation device between connecting line, reduced the gas-flow resistance of device, guaranteed the vacuum of device.
The described U type of the utility model pipe heater; Its housing diameter is 1/2～1/3 of a gas-liquid separator diameter; Be installed in the bottom of gas-liquid separator; Use in the distillation procedure later stage, be used for reclaiming the product of containing in the vinasse of above-mentioned gas-liquid separator bottom, to reach the purpose that improves product yield.
The U type pipework condensation device that the utility model adopted; Its primary structure includes one group of vertically arranged U type heat exchanger tube; Described U type pipework condensation device directly is connected with gas-liquid separator; Its diameter is 0.45～0.65 times of above-mentioned gas-liquid separator diameter; Its lower end is provided with condensate liquid seal pot and following condensate liquid seal pot, and the described diameter of going up the condensate liquid seal pot is 0.4～0.5 times of U type pipework condensation device diameter, and following seal pot diameter is 0.7～0.8 of a top seal pot diameter; The spacing of last condensate liquid seal pot and following condensate liquid seal pot is 1.5～1.8 times of time condensate liquid seal pot diameter, and U type pipework condensation device is that a kind of built-in condenser of distortion has pressure and falls little characteristics.
But but the both also intermittently operated of continued operation of the device of the utility model, specific operation process is following.
The batch distillation operating process:
At first a certain amount of material is placed the bottom of gas-liquid separator, liquid level is no more than the half the of gas-liquid separator height, starts the vavuum pump unit, restarts the material circulating pump, and recycle stock gets into from the top of falling film evaporator.In U type pipework condensation device, feed cooling water, feeding adds hot water and steam in the falling film evaporator shell then, and material is at the in-tube evaporation of falling film evaporator, and indirect steam gets into the condensation of U type pipework condensation device, and condensable product exports to through seal pot and receives flow container.Unevaporated material is got back to the gas-liquid separator bottom, constantly circulates through the material circulating pump again.When the gas phase temperature in the gas-liquid separator and pressure obviously reduce, turn off the water vapour in the falling film evaporator shell, in U type pipe heater, feed then and add hot water and steam, reclaim the product in the vinasse of gas-liquid separator bottom.
The continuous still operating process:
At first a certain amount of material is placed the gas-liquid separator bottom, start the vavuum pump unit, restart the material circulating pump, recycle stock gets into from the top of falling film evaporator.In U type pipework condensation device, feed cooling water, feeding adds hot water and steam in the falling film evaporator shell then, and the pending material of certain flow gets into gas-liquid separator continuously simultaneously.Material is at the in-tube evaporation of falling film evaporator, and indirect steam gets into the condensation of U type pipework condensation device, and condensable product exports to through seal pot and receives flow container.Unevaporated material is got back to the gas-liquid separator bottom, constantly circulates through the material circulating pump again.After pending material adds, when the gas phase temperature in the gas-liquid separator and pressure obviously reduce, turn off the water vapour in the falling film evaporator shell, in U type pipe heater, feed then and add hot water and steam, reclaim the product in the vinasse of gas-liquid separator bottom.
The device beneficial effect of the utility model is: the big caliber heating tube of direct-connected cramped construction and falling film evaporator, the employing of built-in condenser, reduced device internal gas flow resistance, and reduced the air capacity of device seepage, guaranteed the realization of condition of high vacuum degree; Material adopts falling film evaporation, has advantages such as heat transfer efficiency height, disposal ability are big, less scaling; The material heated time is short, not overheated, can reduce situation such as thermal polymerization or thermal decomposition effectively, has the high advantage of product yield and quality; Material only in gravity effect current downflow, is not to promote by high temperature difference in falling film evaporator, allows to use the more economical low temperature difference, has certain energy-saving effect; In addition, apparatus structure is simple, cheap, and flexible operation, but both continued operations, but intermittently operated again.
Description of drawings
Fig. 1 is the device technique flow process and the device construction sketch map of the utility model.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the device of the utility model is further specified.
Embodiment 1
Visible by figure below, the device of the utility model comprises falling film evaporator 1, gas-liquid separator 2, U type pipe heater 3, material circulating pump 4, seal pot 5, U type pipework condensation device 6 at least, receives flow container 7, cold-trap 8, vavuum pump unit 9 and be connected pipeline,
The charging aperture at described falling film evaporator 1 top is connected with the outlet of material circulating pump 4; The suction inlet of material circulating pump 4 is connected with the discharging opening of gas-liquid separator 2 bottoms; Be connected with the discharging opening of U type pipework condensation device 6 by the charging aperture of flow container 7; Gas-liquid separator 2 is connected with receiving flow container 7 through balance pipe, and the air inlet of cold-trap 8 is connected with the exhaust outlet of U type pipework condensation device 6, and the air inlet of vavuum pump unit 9 is connected with the exhaust outlet of cold-trap 8; Described gas-liquid separator 2 directly links to each other with U type pipework condensation device 6 with falling film evaporator 1, and the bottom of gas-liquid separator 2 is provided with U type pipe heater 3.
Described falling film evaporator is a falling film evaporator in the vertical tube, and its primary structure includes a vertically arranged shell-and-tube heat exchanger, and described shell-and-tube heat exchanger adopts the heat exchanger tube of big caliber, and its draw ratio is 60.
Described gas-liquid separator is a horizontal vessel, and its diameter can guarantee that air velocity is at 8m/s.
The housing diameter of described U type pipe heater is 1/3 of a gas-liquid separator diameter.
Described U type pipework condensation device includes one group of vertically arranged U type heat exchanger tube, and its diameter is 0.50 times of described gas-liquid separator diameter.
The lower end of described U type pipework condensation device is provided with condensate liquid seal pot and following condensate liquid seal pot; The described diameter of going up the condensate liquid seal pot is 0.4 times of U type pipework condensation device diameter; Following seal pot diameter is 0.7 of a top seal pot diameter, and the spacing of last condensate liquid seal pot and following condensate liquid seal pot is 1.6 times of following condensate liquid seal pot diameter.
The application implementation example
The maleimide resin additive product situation that distillation is purified in the device of the vacuum still distillation device of routine and the utility model respectively is following:
It is 13m that 800 kilograms of materials drop into heat exchange area
2Conventional vacuum still distillation device adopts Roots's water ring vacuum pump unit, and vacuum can only be controlled at 399～450Pa in the still, 130～135 ℃ of gas phase temperatures, and 150～160 ℃ of liquidus temperatures, disposing needs 10 hours.Product yield 93%, content 98%.
It is 6.5m that 800 kilograms of materials drop into the falling film evaporator heat exchange area
2The device of the utility model adopts Roots's water ring vacuum pump unit, and vacuum can be controlled in below the 266Pa in the gas-liquid separator, 115～120 ℃ of gas phase temperatures, and liquidus temperature is identical with gas phase temperature, and disposing only needs 2 hours.Product yield 97%, content 99.9%.
Claims (6)
1. the high vacuum distillation purifying plant includes falling film evaporator (1), gas-liquid separator (2), U type pipe heater (3), U type pipework condensation device (6), material circulating pump (4) at least, receives flow container (7), cold-trap (8) and vavuum pump unit (9); The charging aperture at described falling film evaporator (1) top is connected with the outlet of material circulating pump (4); The suction inlet of material circulating pump (4) is connected with the discharging opening of gas-liquid separator (2) bottom; Be connected with the discharging opening of U type pipework condensation device (6) by the charging aperture of flow container (7); Gas-liquid separator (2) is connected with receiving flow container (7) through balance pipe; The air inlet of cold-trap (8) is connected with the exhaust outlet of U type pipework condensation device (6), and the air inlet of vavuum pump unit (9) is connected with the exhaust outlet of cold-trap (8); It is characterized in that described gas-liquid separator (2) directly links to each other with U type pipework condensation device (6) with falling film evaporator (1), the bottom of gas-liquid separator (2) is provided with U type pipe heater (3).
2. by the described high vacuum distillation purifying plant of claim 1; It is characterized in that described falling film evaporator is a falling film evaporator in the vertical tube; Its primary structure includes a vertically arranged shell-and-tube heat exchanger; Described shell-and-tube heat exchanger adopts the heat exchanger tube of big caliber, and its draw ratio is 50～100.
3. by claim 1 or 2 described high vacuum distillation purifying plants, it is characterized in that described gas-liquid separator is a horizontal vessel, its diameter can guarantee that air velocity is at 5～15m/s.
4. by claim 1 or 2 described high vacuum distillation purifying plants, the housing diameter that it is characterized in that described U type pipe heater is 1/2～1/3 of a gas-liquid separator diameter.
5. by claim 1 or 2 described high vacuum distillation purifying plants, it is characterized in that described U type pipework condensation device includes one group of vertically arranged U type heat exchanger tube, its diameter is 0.45～0.65 times of described gas-liquid separator diameter.
6. by claim 1 or 2 described high vacuum distillation purifying plants; The lower end that it is characterized in that described U type pipework condensation device is provided with condensate liquid seal pot and following condensate liquid seal pot; The described diameter of going up the condensate liquid seal pot is 0.4～0.5 times of U type pipework condensation device diameter; Following seal pot diameter is 0.7～0.8 of a top seal pot diameter, and the spacing of last condensate liquid seal pot and following condensate liquid seal pot is 1.5～1.8 times of following condensate liquid seal pot diameter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120217305XU CN202155061U (en) | 2011-06-24 | 2011-06-24 | High vacuum distillation purification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120217305XU CN202155061U (en) | 2011-06-24 | 2011-06-24 | High vacuum distillation purification device |
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| Publication Number | Publication Date |
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| CN202155061U true CN202155061U (en) | 2012-03-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201120217305XU Expired - Fee Related CN202155061U (en) | 2011-06-24 | 2011-06-24 | High vacuum distillation purification device |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102266677A (en) * | 2011-06-24 | 2011-12-07 | 刘元 | High vacuum distillation purification device |
| CN103695167A (en) * | 2014-01-07 | 2014-04-02 | 常州市百得来生物科技有限公司 | Purification device and purification method for removing impurities in oil liquids |
| CN105289020A (en) * | 2015-11-23 | 2016-02-03 | 梁锋 | Ethanol solution low temperature vacuum purification device |
| CN106924983A (en) * | 2017-05-05 | 2017-07-07 | 江苏格桑花涂料有限公司 | A kind of anticorrosive paint production enrichment facility |
| CN108865202A (en) * | 2018-06-27 | 2018-11-23 | 安徽省建辉生物质能发展有限公司 | A kind of bamboo and wood vinegar liquid distilation device |
-
2011
- 2011-06-24 CN CN201120217305XU patent/CN202155061U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102266677A (en) * | 2011-06-24 | 2011-12-07 | 刘元 | High vacuum distillation purification device |
| CN103695167A (en) * | 2014-01-07 | 2014-04-02 | 常州市百得来生物科技有限公司 | Purification device and purification method for removing impurities in oil liquids |
| CN105289020A (en) * | 2015-11-23 | 2016-02-03 | 梁锋 | Ethanol solution low temperature vacuum purification device |
| CN106924983A (en) * | 2017-05-05 | 2017-07-07 | 江苏格桑花涂料有限公司 | A kind of anticorrosive paint production enrichment facility |
| CN108865202A (en) * | 2018-06-27 | 2018-11-23 | 安徽省建辉生物质能发展有限公司 | A kind of bamboo and wood vinegar liquid distilation device |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120307 Termination date: 20140624 |
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| EXPY | Termination of patent right or utility model |