CN102266677A - High vacuum distillation purification device - Google Patents
High vacuum distillation purification device Download PDFInfo
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- CN102266677A CN102266677A CN2011101726765A CN201110172676A CN102266677A CN 102266677 A CN102266677 A CN 102266677A CN 2011101726765 A CN2011101726765 A CN 2011101726765A CN 201110172676 A CN201110172676 A CN 201110172676A CN 102266677 A CN102266677 A CN 102266677A
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- gas
- liquid separator
- diameter
- falling film
- film evaporator
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- 238000005292 vacuum distillation Methods 0.000 title claims abstract description 14
- 238000000746 purification Methods 0.000 title abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 73
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000011552 falling film Substances 0.000 claims abstract description 37
- 238000009833 condensation Methods 0.000 claims description 34
- 230000005494 condensation Effects 0.000 claims description 34
- 238000007599 discharging Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 2
- 238000012719 thermal polymerization Methods 0.000 abstract description 2
- 230000007423 decrease Effects 0.000 abstract 1
- 238000004821 distillation Methods 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 3
- 238000004939 coking Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 238000010276 construction Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000000998 batch distillation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000526 short-path distillation Methods 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to a high vacuum distillation purification device which comprises a falling film evaporator, a gas-liquid separator, a U-shaped tube heater, a U-shaped tube condenser, a material circulating pump, a liquid-accepting tank, a cold trap, and a vacuum pump unit, and is characterized in that the gas-liquid separator is directly connected to the falling film evaporator and the U-shaped tube condenser, and the U-shaped tube heater is disposed at the bottom of the gas-liquid separator. The beneficial effect of the device of the invention is that: the adoption of a directly-connected compact structure, a large-diameter heating tube of the falling film evaporator, and a built-in condenser reduces the airflow resistance inside the device, decreases the air capacity leaked by the device, and guarantees the realization of a high vacuum degree; the material is evaporated by a falling film, which has the advantages of high heat transfer efficiency, great processing capacity, difficult scaling, and the like; situations such as thermal polymerization or thermal decomposition are effectively reduces, and the device has the advantages of high product yield and quality; the device has certain energy saving effect; in addition, the device has a simple structure, low cost, and flexible operation, and is applicable to both continuous operation and intermittent operation.
Description
Technical field
The present invention 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 they are fit to the following distillation of vacuum 1.33Pa and purify.Need distill the material of purifying in vacuum 1.33～266Pa scope, 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 ℃ material for boiling point under the normal pressure, when gaseous pressure is 1mmHg, 50mm place boiling point elevation value is about 38 ℃ under its liquid level, that is to say that the following material of liquid level 50mm is overheated serious and can not seethe with excitement, the Chang Gui effective heat transfer area of vacuum still distillation device has only 10～20% of total heat conduction area according to statistics.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
Technical problem to be solved by this invention 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 present invention solves 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, is subjected to 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 being subjected to flow container by balance pipe, 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 present invention 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 situations 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.
Gas-liquid separator of the present invention 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.
U type pipe heater of the present invention, its housing diameter is 1/2～1/3 of a gas-liquid separator diameter, is installed in the bottom of gas-liquid separator, uses 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.
U type pipework condensation device of the present invention, 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, 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, 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 both also intermittently operated of continued operation of device of the present invention, specific operation process is as follows.
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 half of gas-liquid separator height, starts the vavuum pump unit, restarts the material circulating pump, and recycle stock enters from the top of falling film evaporator.Feed cooling water in U type pipework condensation device, 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 enters the condensation of U type pipework condensation device, and condensable product exports to through seal pot and is subjected to 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 enters from the top of falling film evaporator.Feed cooling water in U type pipework condensation device, feeding adds hot water and steam in the falling film evaporator shell then, and the pending material of certain flow enters gas-liquid separator continuously simultaneously.Material is at the in-tube evaporation of falling film evaporator, and indirect steam enters the condensation of U type pipework condensation device, and condensable product exports to through seal pot and is subjected to 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.
Device beneficial effect of the present invention 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 situations 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 device technique flow process of the present invention and device construction schematic diagram.
The specific embodiment
Below in conjunction with drawings and Examples device of the present invention is further specified.
Embodiment 1
By figure below as seen, device of the present invention 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, is subjected to flow container 7, cold-trap 8, vavuum pump unit 9 and connecting pipe,
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 being subjected to flow container 7 by balance pipe, the air inlet of cold-trap 8 is connected with the exhaust outlet of U type pipework condensation device 6, 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.
Application Example
The maleimide resin additive product situation that distillation is purified in the vacuum still distillation device of routine and device of the present invention respectively is as follows:
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
2Device of the present invention 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, is subjected to 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 being subjected to flow container (7) by 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 |
|---|---|---|---|
| CN 201110172676 CN102266677B (en) | 2011-06-24 | 2011-06-24 | High vacuum distillation purification device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110172676 CN102266677B (en) | 2011-06-24 | 2011-06-24 | High vacuum distillation purification device |
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| CN102266677A true CN102266677A (en) | 2011-12-07 |
| CN102266677B CN102266677B (en) | 2013-07-17 |
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| CN 201110172676 Expired - Fee Related CN102266677B (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 |
|---|---|---|---|---|
| CN102908794A (en) * | 2012-09-04 | 2013-02-06 | 吴国存 | Tank condensation, diversion and pressure reduction distillator |
| CN103160334A (en) * | 2013-03-14 | 2013-06-19 | 济钢集团有限公司 | Method and device for separation of benzene and water in debenzolized rich oil |
| CN104326520A (en) * | 2014-10-29 | 2015-02-04 | 宝鸡忠诚制药机械有限责任公司 | Horizontal pipe falling-film thermo-compression water distiller |
| CN106422378A (en) * | 2012-01-11 | 2017-02-22 | 张惠明 | Methods and Apparatuses for Water Purification |
| CN111003866A (en) * | 2019-12-06 | 2020-04-14 | 安徽晨晰洁净科技有限公司 | Waste salt concentration treatment device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101099905A (en) * | 2006-07-09 | 2008-01-09 | 蒋建君 | Pointed bottom distilling device |
| CN202155061U (en) * | 2011-06-24 | 2012-03-07 | 刘元 | High vacuum distillation purification device |
-
2011
- 2011-06-24 CN CN 201110172676 patent/CN102266677B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101099905A (en) * | 2006-07-09 | 2008-01-09 | 蒋建君 | Pointed bottom distilling device |
| CN202155061U (en) * | 2011-06-24 | 2012-03-07 | 刘元 | High vacuum distillation purification device |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106422378A (en) * | 2012-01-11 | 2017-02-22 | 张惠明 | Methods and Apparatuses for Water Purification |
| CN106422378B (en) * | 2012-01-11 | 2019-10-01 | 张惠明 | Method and apparatus for Water warfare |
| CN102908794A (en) * | 2012-09-04 | 2013-02-06 | 吴国存 | Tank condensation, diversion and pressure reduction distillator |
| CN102908794B (en) * | 2012-09-04 | 2015-07-29 | 唐山山岛石油化学有限公司 | Condensation diversion reduced pressure distiller in tank |
| CN103160334A (en) * | 2013-03-14 | 2013-06-19 | 济钢集团有限公司 | Method and device for separation of benzene and water in debenzolized rich oil |
| CN104326520A (en) * | 2014-10-29 | 2015-02-04 | 宝鸡忠诚制药机械有限责任公司 | Horizontal pipe falling-film thermo-compression water distiller |
| CN111003866A (en) * | 2019-12-06 | 2020-04-14 | 安徽晨晰洁净科技有限公司 | Waste salt concentration treatment device |
| CN111003866B (en) * | 2019-12-06 | 2024-05-17 | 安徽晨晰洁净科技有限公司 | Waste salt concentration treatment device |
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| CN102266677B (en) | 2013-07-17 |
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Effective date of registration: 20160721 Address after: 430332 Hubei Province, Wuhan city Huangpi District Cai Zha Zhen new avenue Patentee after: Wuhan Huazhong chemical and medical equipment Engineering Co., Ltd. Address before: 430077 Hubei city of Wuhan province Wuchang Oriole Road No. 25 Wuhan Pharmaceutical Design Institute Patentee before: Liu Yuan |
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