CN1456382A - Packed tower top gas-liquid splite-flow reflux balancing distributing distilling producing process devics - Google Patents

Packed tower top gas-liquid splite-flow reflux balancing distributing distilling producing process devics Download PDF

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Publication number
CN1456382A
CN1456382A CN 02111619 CN02111619A CN1456382A CN 1456382 A CN1456382 A CN 1456382A CN 02111619 CN02111619 CN 02111619 CN 02111619 A CN02111619 A CN 02111619A CN 1456382 A CN1456382 A CN 1456382A
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liquid
packed tower
splite
distilling
phegma
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周增龙
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Abstract

A distillation equipment for purifying the thermosensitive substance, such as vitamines, is composed of a forced raw liquid evaporator set which consists of raw liquid evaporator, raw liquid circulating pump and spray distributor, and a filler tower whose top has an equalizing distributor of return liquid in vapor-liquid branching mode. Its advantages are simple system, low cost and high output and quality of product, and low energy consumption.

Description

Packed tower top gas-liquid splite-flow reflux balancing Fabric material distilling producing process device
The present invention's ' the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device ' (figure one is for being used for the schematic diagram of gap rectifying) is a kind of thermal release that is used for liquid mixture, purify, concentrate, subtractive process, at normal pressure, gap distillation or continuous rectification (figure five) production technology device schematic diagram under decompression or the high vacuum condition, compare with packed tower gap distillation (figure two) or continuous still (figure three) system that present conventional design is used, great difference is arranged, particularly in packed tower, fill equal regular wire packing, high vacuum condition (the thermal release of 1~100Pa) time processing heat sensitivity liquid mixture, purify, concentrate, in the purification operations system production process, more obvious by contrast.
The separation of liquid mixture material, concentrated, purification, be to utilize each component volatilization degree difference in the mixture liquid, be the different character of vapour pressure of each component under the same temperature, mostly under decompression distillation or high vacuum state, method with packed column distillation system carries out gap distillation or continuous rectification reaches the purpose that liquid mixture separates, concentrates, makes with extra care, purifies.Distilling producing process device to the heat sensitivity mixture material that need separate, concentrate, make with extra care, purify by distillating method, often need be under higher vacuum condition (1~100Pa), with alap heating-up temperature, short as far as possible heated time, make heat sensitivity mixture material, in the unit interval, obtain meeting the maximum throughput of product quality, to avoid the heat sensitivity mixture, the amount that produces qualitative change or appearance luster because of being heated is too much, and influences product quality or output capacity by the gross.Thereby design one and overlap the thermal release distilling apparatus, make particularly heat sensitivity mixture feed liquid class material of mixture feed liquid, separative efficiency height in the scope of broad, unit interval product fraction output capacity height, fall little in the peak load downforce, reduce the feed liquid heated time, under alap heating-up temperature condition, finish feed liquid processing procedure by the gross with the minimum time, can both in package unit, show, largely put to death in the structure of different tower internals and evaporation reboiler, the thermal release method of purification comparatively meticulous to some heat sensitivity liquid mixture, generally need under higher vacuum state, realize with the packed column distillation system of the regular wire mesh packing of filling, this is at chemical industry, pharmaceuticals industry, the light industry industry, food industry, be common in the industrial circles such as bioengineering, the energy consumption maximum, it is again extremely important production technology device, comparatively the typical case also is that design is used comparatively general at present, distillation of high vacuum distillation packed tower gap or continuous rectification production technology system, with the distillation schematic diagram of gap shown in the figure two is example: it is generally by distillation still or falling liquid film, climbing-film evaporation-reboiler (2-1), distilling filled tower and the condenser (2-5) formed by stripping section (2-2) rectifying section (2-3) phegma Fabric glassware (2-4), vapor-liquid separation current divider (2-6), the sampling or at thread detector (2-7), condensate cooler (2-8), cold hydrazine vacuum system (2-9), distillate storage tank (2-10), reflux ratio R regulation and control system (2-11), feed liquid preheated feed device compositions such as (using in the 3-12 continuous rectification conventional design), and in the continuous rectification conventional design, remove in the zone of packed tower stripping section shown in the figure three, increase is given the next feed liquid of hot device (3-12) in the interval charging of packed tower stripping section by the feed liquid intermediate feed, evaporation-reboiler (3-1) is put on also useful side, and P ' shown in the figure three is heavy component material Continuous Flow outlet in the continuous rectification process.In present gap rectifying conventional design or continuous rectification conventional design Distallation systm process, obtain maximum output capacity when improving the distillate product content as far as possible, optimize vapour-liquid mass process in the tower, under the least possible time, alap temperature conditions, strengthen the material evaporating capacity, so that under minimum energy consumption, obtain the highest distillation efficiency and minimum investment and operating cost.This is to the separation of heat sensitivity liquid mixture material, refining, concentrate, the purification process influence is very big, therefore except various dissimilar fillers are researched and developed, to reflux ratio regulation and control system (2-11) or (3-11), reflux in tower Fabric glassware (2-4) or (3-4) and evaporation-reboiler (2-1) or (3-1) all have more research and development to use, from present report and should be used for seeing as yet not disengaging figure two, the mode of basic production technological process shown in the figure three, particularly in order to make tower internals-backflow Fabric glassware (2-4) or (3-4) (reflux in tower distributing device illustration structure and its allocation position schematic diagram in tower that figure four uses for report up to the present, D is the vaporizer outlet, the diagram direction of arrow is removed high-level condenser, R is that high-order current divider phegma adjusting device and process duct flow to, R ' is the import of phegma Fabric glassware, Q for calandria phegma Fabric glassware commonly used to packing layer Fabric liquid status.From diagram as can be known, owing to be subjected to spatial constraints in the tower, the phegma Fabric glassware structure (figure four) of current application is difficult under the capacity of returns situation that varies in size, make phegma form balanced drop or liquid flows equal Fabric in the whole circular section of packed tower) at place, the whole circular section of packed tower, allow the phegma flow regulate size and balanced as far as possible Fabric material according to the R reflux ratio, and substantially constant, to reach moistening inner-tower filling material to best vapour-liquid mass process, expect to inner-tower filling material Fabric in order to make phegma enter Fabric glassware (2-4 or 3-4) simultaneously, must be with condenser (2-5 or 3-5), a vapour-liquid current divider or liquid-liquid current divider (2-6 or 3-6) and a cover reflux ratio R regulate control process piping systems (2-11 or 3-11), be placed in the height that exceeds the packed tower cat head, so that utilize the height potential difference to make phegma enter packed tower tower internals-backflow Fabric glassware (2-4 or 3-4), it is necessary that this will increase the high-order equipment of this class of location again, complementary elevated frame shelf structure device, thus investment and operating cost increased.In order to reach the state that phegma place, whole circular section in tower accomplishes balanced Fabric material and do not influence vapour locking in the tower, the evaporation-reboiler (2-1 or 3-1) of packed tower tower internals-phegma Fabric glassware (2-4 or 3-4) and Distallation systm all there is more Application and Development research.
The present invention's " the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device " is on the basis of the multiple evaporimeter that is suitable for the different feed liquid characteristic of Application and Development, utilize the technological process of the characteristic configuration of packed tower top gas-liquid splite-flow reflux balancing Fabric glassware (application for a patent for invention number :), the novel packed tower vapour-liquid shunting that composite design forms, balanced Fabric material continuous rectification of phegma or gap rectifying production technology device, the present invention's " the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device " both can be according to mixture feed liquid characteristic, also can be used as continuous rectification as gap rectifying and be used for production process, be specially adapted to heat sensitivity mixture feed liquid class material, ((figure one is a gap rectifying schematic diagram for 1~100Pa) packed tower continuous rectification or gap rectifying production process under decompression or the high vacuum condition, figure five is the continuous rectification schematic diagram), the balanced Fabric material of packed tower vapour-liquid shunting phegma of the present invention distilling producing process device is made up of two parts:
One. can select and fixed forced-circulation evaporation reboiler group according to mixture feed liquid rerum natura, it by (can be according to the different evaporation reboiler of feed liquid characteristic configuration: as accepting application for a patent for invention number: bottom rotary vertical falling-film thin-film evapovator, centrifugally distributing falling-film evaporator etc., figure one schematic diagram be built-in shell and tube heating falling film evaporation-reboiler configuration mode in the still) evaporation-reboiler (1-1), high vacuum distillation feed liquid circulating pump (1-2), spray the heat sensitivity liquid mixture carburation by evaporation assembly of Fabric glassware (1-3) composition.After the mixture feed liquid enters evaporation reboiler (1-1), start feed liquid circulating pump (1-2), force feed liquid to utilize pump pressure when nozzle (1-3) tubulation internal face in evaporation reboiler device sprays the evaporation of Fabric material formation falling-film by circulating pump, form a large amount of drops in the space and strengthen the feed liquid vaporescence, make mixture feed liquid a large amount of carburation by evaporations under short as far as possible time, alap heating-up temperature condition, and make the mixture vaporizer that becomes steam state enter the packed tower distillation system.
Two. after mixture feed liquid steam enters packed tower, by rectifying column filler stripping section (1-4), rectifying section (1-5) rises to top gas-liquid splite-flow reflux balancing Fabric glassware (1-6 accepted application for a patent for invention number :), because the architectural characteristic of top gas-liquid splite-flow reflux balancing Fabric glassware (1-6), can be according to the distillate sampling or at thread detector (1-7) feedack, regulate temperature (application for a patent for invention number :) thus reach the balanced Fabric glassware of control top gas-liquid splite-flow reflux phegma flow, and no matter the flow size all can reach phegma to the balanced Fabric liquid (picture one) of rectifying section filler, after the gas that cat head D outlet is obtained by light component distillate purity enters condenser (1-8) heat release, become liquid phase to flow into distillate basin (1-10), (distillation packed tower interval, gap generally is regardless of stripping section and rectifying section to finish liquid mixture thermal release gap rectification and purification or continuous rectification process, in fact owing in gap rectifying and the continuous rectification packed tower phegma Fabric glassware need be set all, make the moistening filler of phegma optimize vapour-liquid mass process in the tower, so the gap distillation also can be appointed for there being stripping section).
" the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device is " if as packed tower continuous rectification production process (figure five) in the present invention, only need intermediate feed to be set and give hot device (5-11) in packed tower stripping section zone, and intermediate feed is given hot device outlet be connected with packed tower intermediate feed mouth, as mixture feed liquid charging aperture, in addition will be according to the selected bottom rotary vertical falling-film thin-film evapovator of feed liquid characteristic (application for a patent for invention number :), bottom rotary vertical falling-film thin-film evapovator (application for a patent for invention number :) waits evaporimeter lower curtate heavy component distillate to export (5-1) B to be connected with the heavy component basin, make light component and heavy component respectively continuously at the bottom of cat head and the tower evaporation reboiler bottom flow out, schematic flow sheet is the balanced Fabric of packed tower vapour-liquid shunting phegma and expects continuous rectification production technology device schematic diagram shown in figure five.
The present invention's " the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device " and present similar heat sensitivity liquid mixture gap rectifying or the continuous rectification distillation system handled shown in figure two figure three, after the interior filling of tower same size and woven wire structured packing that same factory produces is compared, the difference of highly significant is arranged:
One. the present invention's " the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device " because top gas-liquid splite-flow reflux balancing Fabric glassware (application for a patent for invention number :) can reach the function that balanced Fabric spills drop and is not subjected to the influence of flow size at place, the whole circular section of packed tower, thereby optimized vapour-liquid mass process in the packed tower, the control system of distillate content is become only to be needed by sampling or behind the thread detector feedack, manually or automatically regulate the temperature that top gas-liquid splite-flow reflux balancing Fabric glassware refrigerant medium is imported and exported, can adjust Fabric material amount balanced in the tower automatically, thereby stably obtain the distillate of required quality standard, make operating process more simple and reliable, and no matter all can obtain effect same as using in gap rectifying (figure one) or continuous rectification (figure five) production process
Two. the backflow volume process pipelines is regulated in the no high-level condenser of the present invention's " the balanced Fabric of packed tower vapour-liquid shunting phegma expects the distilling producing process device ", high-order current divider, the high-order shunting of phegma, an expensive high position is shunted high-order equipment such as electric valve, thereby need not high-order frame structure positioner, not only optimize the interior vapour-liquid mass process of tower and also simplified Process configuration, optimized operating system, and reduced investment cost and relevant stop production to overhaul operation operating cost
Three. the present invention's " the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device " can be according to the feed liquid characteristic, (figure one to dispose different high vacuum feed liquid circulating evaporator groups, the evaporator bank of still formula shown in the figure five), under lower temperature conditions (as XX factory before 1997, XX factory is originally with the same intermediate of figure two class high vacuum packed tower gaps distillation XX product, the production technology device need be used the hot oil boiler heat supply, and temperature can not be lower than 220C, not only product has peculiar smell, and the feed liquid heated time is long, the raffinate amount reaches more than 10%, opened in 1998 make use the present invention's " the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device " after, heating condition changes steam 160C~170C into, the unit interval evaporating capacity is 2~3 times of original devices, the batch processing time shortened to 15~16 hours from nearly 40 hours, the raffinate amount from falling more than 10% at the end to 3%, the present of application) greatly improved mixture feed liquid carburation by evaporation amount, shortened heat sensitivity mixture feed liquid class material heated time, it is nearly more than 10% also to improve efficiency of pcr product when improving the quality of products, and has not only reduced unit cost but also improved operating environment.
Since nineteen ninety-eight existing more than the 10 cover production technology devices of the present invention's " the balanced Fabric material of packed tower vapour-liquid shunting phegma distilling producing process device " are applied to XX factory of XX factory heat sensitivity mixture material Distallation systm, obtain good benefit.

Claims (2)

  1. One. with " packed tower top gas-liquid splite-flow reflux balancing Fabric glassware " (application for a patent for invention number :) configuration, no high-level condenser, high-order vapour-liquid current divider, high-order frame structure, the high-order shunting of phegma is regulated backflow volume R and is compared process piping systems, only need to regulate between packed tower top gas-liquid splite-flow reflux balancing Fabric glassware pipe and import and export medium temperature, can realize Fabric material backflow volume in the filler Tata, change the interior vapour-liquid mass condition of tower with the control distillate quality, and both can be applicable to the packed tower normal pressure that simple rectifying also can be used for continuous rectification simultaneously, decompression, the distilling producing process device of high vacuum distillation heat sensitivity mixture material.
  2. Two. with " bottom rotary vertical falling-film thin-film evapovator " (application for a patent for invention number: 02110628.2), or with " centrifugally distributing falling-film evaporator " (application for a patent for invention number: 02110768.2), or invent other type distiller of design with me, evaporimeter, evaporator bank, the gap distilling apparatus that the distiller group is formed, continuous distillation plant, or above device and feed liquid circulating pump formation fortified mixture feed liquid, the packed tower normal pressure that is applied to simple rectifying or continuous rectification of heat sensitivity mixture material-evaporating carburetor group, decompression, the distilling producing process device of high vacuum distillation heat sensitivity mixture material.
CN 02111619 2002-05-09 2002-05-09 Packed tower top gas-liquid splite-flow reflux balancing distributing distilling producing process devics Pending CN1456382A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914077A (en) * 2010-09-13 2010-12-15 东瑞(南通)医药科技有限公司 Recovery process of tetrahydrofuran
CN105920861A (en) * 2016-06-08 2016-09-07 燕山大学 Spray distillation device
CN106422390A (en) * 2016-12-02 2017-02-22 山东海昆化工技术有限公司 Heat-sensitive material separating rectification device and rectification method thereof
CN108607232A (en) * 2018-07-10 2018-10-02 常州市九洲干燥设备有限公司 A kind of distilling apparatus
CN115155093A (en) * 2022-08-09 2022-10-11 山东蓝湾新材料有限公司 Distillation column is used in production of dimethylamino ethyl acrylate

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914077A (en) * 2010-09-13 2010-12-15 东瑞(南通)医药科技有限公司 Recovery process of tetrahydrofuran
CN105920861A (en) * 2016-06-08 2016-09-07 燕山大学 Spray distillation device
CN106422390A (en) * 2016-12-02 2017-02-22 山东海昆化工技术有限公司 Heat-sensitive material separating rectification device and rectification method thereof
CN108607232A (en) * 2018-07-10 2018-10-02 常州市九洲干燥设备有限公司 A kind of distilling apparatus
CN108607232B (en) * 2018-07-10 2024-04-02 常州市九洲干燥设备有限公司 Distillation device
CN115155093A (en) * 2022-08-09 2022-10-11 山东蓝湾新材料有限公司 Distillation column is used in production of dimethylamino ethyl acrylate

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