CN103977592B - The method of light naphtha is removed with the rectifier unit comprising two reboiler - Google Patents

The method of light naphtha is removed with the rectifier unit comprising two reboiler Download PDF

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Publication number
CN103977592B
CN103977592B CN201410239635.7A CN201410239635A CN103977592B CN 103977592 B CN103977592 B CN 103977592B CN 201410239635 A CN201410239635 A CN 201410239635A CN 103977592 B CN103977592 B CN 103977592B
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reboiler
extraction
rectifying column
tower reactor
tower
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CN103977592A (en
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张燕
王凌燕
张春灵
殷欣欣
毛学峰
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YANTAI GUOBANG CHEMICAL MACHINE TECHNOLOGY Co Ltd
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YANTAI GUOBANG CHEMICAL MACHINE TECHNOLOGY Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/10Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

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  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The invention provides and a kind ofly comprise the rectifier unit of two reboiler and remove the method for light naphtha with this device, this device comprises rectifying column, circulation reboiler, extraction reboiler, heat exchanger, condenser, reflux-withdrawal control system and product pans, circulation reboiler is connected with the tower reactor of rectifying column respectively with extraction reboiler, extraction reboiler liquid-phase tube and extraction reboiler gas phase pipe is provided with between extraction reboiler and rectifying column, raw material heat exchanger and condenser is provided with between described rectifying column and reflux-withdrawal control system, product pans are connected with reflux-withdrawal control system.The method can, according to liquid level gauge height in tower reactor liquid thermometer and rectifying column, judge whether to run extraction reboiler.The invention solves the halfway problem of traditional reboiler flush distillation, the light component content in tower bottom of rectifying tower extraction material is reduced, improves the yield of product.

Description

The method of light naphtha is removed with the rectifier unit comprising two reboiler
Technical field
The present invention relates to technical field of chemical separation, particularly relate to and a kind ofly comprise the rectifier unit of two reboiler and remove the method for light naphtha with this device.Particularly utilization comprises the rectifier unit of two reboiler by the raw material containing trace and the thing that heavily boils on a small quantity, completes removing further of kettle material light component by twice evaporation, makes to obtain higher concentration in tower reactor and heavily to boil the equipment of thing and method.It belongs to the category of chemical separating, is particularly useful for the occasion containing trace and heavily boil on a small quantity thing material and light component separation of products.
Background technology
Usually the occasion of heavily boil thing material and light component separation of products can be related in the industry such as chemical industry, pharmacy.When the contained thing material that heavily boils is micro-or a small amount of, need the thing that heavily boils to be separated through long-time high-temperature heating rectifying, in distillation process due to the heat time lengthen, temperature is too high, tower reactor reboiler heat exchange tube wall has the coking of the thing that heavily boils, glutinous wall, even may block heat exchanger tube, the efficiency of heating surface of reboiler is reduced.Heat according to single reboiler and the technique of extraction continuously, the material of tower reactor extraction is the heavy constituent containing a large amount of light component, will certainly cause the loss of light component like this, reduces separative efficiency.
Based on above problem, consider how high concentration heavily to be boiled thing as early as possible and to take out rectifier unit be thoroughly extend heat exchanger tube blocking, improve the key point of methyl esters yield.
How to found new the comprising the rectifier unit of two reboiler and remove the method for light naphtha with this device, one of current important research and development problem of real genus that a kind of structure is simple, replacing heat-exchange tube number of times is few, separative efficiency is high.
Summary of the invention
The technical problem to be solved in the present invention is to provide and a kind ofly comprises the rectifier unit of two reboiler and remove the method for light naphtha with this device, make that its structure is simple, replacing heat-exchange tube number of times is few, separative efficiency is high, thus solve existing rectifier unit heavily boil thing flush distillation not thoroughly, heat exchanger tube easily blocks, separative efficiency is low deficiency.
For solving the problems of the technologies described above, the invention provides a kind of rectifier unit comprising two reboiler, its special character is: comprise rectifying column, circulation reboiler, extraction reboiler, heat exchanger, condenser, reflux-withdrawal control system and product pans, circulation reboiler is connected with the tower reactor of rectifying column respectively with extraction reboiler, extraction reboiler liquid-phase tube and extraction reboiler gas phase pipe is provided with between extraction reboiler and rectifying column, raw material heat exchanger and condenser is provided with between described rectifying column and reflux-withdrawal control system, product pans are connected with reflux-withdrawal control system.
As a modification of the present invention, described rectifying column takes into account the tower reactor gas phase temperature detector for detecting tower reactor gas phase temperature in the tower reactor tower reactor liquid level be provided with for detecting tower reactor liquid level.
Further, described circulation reboiler is connected with the tower reactor of rectifying column by tower reactor circulating pump.
Further, described rectifying column feeding line is provided with feed rate control system.
Further, described circulation reboiler is forced circulating reboiler, forces falling-film reboiler, thermosyphon reboiler or a through type reboiler, the polishing of described circulation reboiler heat exchanger tube inwall.
Further, described extraction reboiler is immersion shell and tube reboiler, the polishing of described immersion shell and tube reboiler heat exchanger tube inwall, and heat medium adopts Steam Heating or heat-conducting oil heating.
Further, described extraction reboiler is positive displacement formula reboiler, the polishing of described positive displacement reboiler cylinder inboard wall, and heat medium adopts Steam Heating or heat-conducting oil heating.
Further, bottom described extraction reboiler, bobbin carriage is provided with extraction reboiler liquidus temperature mouth and tower reactor extraction pipeline.
The invention still further relates to a kind of method that said apparatus removes light naphtha, adopt rectifying column, circulation reboiler, extraction reboiler, reflux-withdrawal control system, condenser, product receiving tank and between connecting line etc. jointly remove light component in tower reactor extraction fraction, its step is as follows:
(1) raw material needing to be separated is controlled feed rate by feed rate control system, raw material flows through tower top heat exchanger and overhead vapours carries out heat exchange, charging in the middle part of rectifying column;
(2) to circulation reboiler supply heating agent, start to heat material in rectifying column, make the steam of light component increase, control feed back by overhead reflux extraction control system and return rectifying column, withdrawing fluid makes the filler complete wetting of full tower;
(3) when tower reactor liquid level in rectifying column is higher than restriction liquid level, open the valve of extraction reboiler gas phase pipe, make extraction reboiler and tower bottom of rectifying tower pressure balance, then extraction reboiler liquid-phase tube is opened, in rectifying column, liquid flow in extraction reboiler, to extraction reboiler supply heating agent, the light component entering into extraction reboiler is continued heating evaporation, after the liquidus temperature of extraction reboiler reaches the saturation temperature of the thing mixture that heavily boils, close extraction reboiler liquid-phase tube valve, continue to be heated to extraction reboiler and reach high some temperature, to open on tower reactor extraction pipeline valve by outside kettle material extraction battery limit (BL).
Further, the feeding manner of described rectifying column is continuous feed mode, and the extraction of tower reactor can adopt continuous extraction mode or interval extraction mode.
The invention has the beneficial effects as follows:
The present invention had both been applicable to atmospheric operation and had also been applicable to decompression and pressurized operation, and simple to operate, applied range, applicability is strong.By arranging two covers for providing the heater of heat to rectifying column, solving the halfway problem of traditional reboiler flush distillation, the light component content in tower bottom of rectifying tower extraction material being reduced greatly, improves the yield of product.Method of the present invention is mainly used in the distillation operation of the material containing micro-or a small amount of thing that heavily boils.
Accompanying drawing explanation
Above-mentioned is only the general introduction of technical solution of the present invention, and in order to better understand technological means of the present invention, below in conjunction with accompanying drawing and detailed description of the invention, the present invention is described in further detail.Example, only for explaining the present invention, is not intended to limit scope of the present invention.
Fig. 1 is a kind of structural representation comprising the rectifier unit of two reboiler of the present invention.
Fig. 2 is the structural representation of the device described in the embodiment of the present invention 2.
Wherein, 1, rectifying column; 2, tower reactor gas phase temperature detector; 3, extraction reboiler gas phase pipe; 4, extraction reboiler liquid-phase tube; 5, extraction reboiler; 6, extraction reboiler liquidus temperature; 7, tower reactor extraction pipeline; 8, tower reactor circulating pump; 9, circulation reboiler; 10, tower reactor liquid level gauge; 11, raw material heat exchanger; 12, condenser; 13, reflux-withdrawal control system; 14, product receiving tank; 15, feedstock control system; 16, tower reactor liquid phase temperature monitor.
Detailed description of the invention
Embodiment 1
With reference to shown in Fig. 1, the invention provides a kind of rectifier unit comprising two reboiler, comprise rectifying column 1, circulation reboiler 9, extraction reboiler 5, heat exchanger 11, condenser 12, reflux-withdrawal control system 13 and product pans 14; Circulation reboiler 9 is connected with the tower reactor of rectifying column 1 respectively with extraction reboiler 5, is provided with extraction reboiler liquid-phase tube 4 and extraction reboiler gas phase pipe 3 between extraction reboiler 5 and rectifying column 1; Be provided with raw material heat exchanger 11 and condenser 12 between described rectifying column 1 and reflux-withdrawal control system 13, product pans 14 are connected with reflux-withdrawal control system 13.
Circulation reboiler 9 can be connected with rectifying column 1 by tower reactor circulating pump 8, and extraction reboiler 5 is directly connected with rectifying column by pipeline.Described circulation reboiler 9 one end is connected with rectifying column 1 tower reactor gas-phase space, and the other end is connected with tower reactor circulating pump 8.
Described rectifying column 1 feed end is provided with feed rate control system 15.
Described rectifying column 1 tower reactor is provided with tower reactor gas phase temperature detector 2, tower reactor liquid thermometer 16 and the tower reactor liquid level gauge 10 for detecting tower reactor liquid level.
Described circulation reboiler 9 can be forced circulating reboiler or force falling-film reboiler, and circulation reboiler 9 can adopt Steam Heating also can be heat-conducting oil heating; The heat exchanger tube inwall polishing of circulation reboiler, be conducive to preventing heavily boiling the coking of material on tube wall or glutinous wall, cramming.
Described extraction reboiler 5 is preferably the shell and tube reboiler of immersion; Extraction reboiler 5 can adopt Steam Heating also can be heat-conducting oil heating; The heat exchanger tube specification of extraction reboiler 5 adopts Large Diameter Pipeline heat exchanger tube, at least selects Ф 32 or Ф 38 heat exchanger tube and its heat exchanger tube inwall polishing; Extraction reboiler 5 arranges four process stream contact mouths of pipe: process stream liquid-inlet, gas-liquid equilibrium mouth, process stream extraction mouth, liquidus temperature detect mouth.
Bottom described extraction reboiler 5, bobbin carriage is provided with extraction reboiler liquidus temperature mouth 6.
Bottom described extraction reboiler 5, bobbin carriage is also provided with tower reactor extraction pipeline 7, for the extraction of tower reactor qualified material.
Embodiment 2
With reference to shown in Fig. 2, the difference of the present embodiment and above-described embodiment is, described circulation reboiler 9 is directly connected with rectifying column 1 by pipeline, and described circulation reboiler 9 is thermosiphon reboiler or a through type reboiler; Extraction reboiler is positive displacement reboiler, cylinder inboard wall polishing.
The present invention also provides a kind of and adopts the above-mentioned rectifier unit comprising two reboiler to remove the method for light naphtha, main employing rectifying column, circulation reboiler, extraction reboiler, reflux-withdrawal control system, condenser, product receiving tank and between connecting line etc. jointly remove light component in tower reactor extraction fraction, its step is as follows:
(1) raw material needing to be separated is controlled feed rate by feed rate control system, raw material flows through tower top heat exchanger and overhead vapours carries out heat exchange, charging in the middle part of rectifying column;
(2) raw material of described rectifying column charging can be the raw material of alcohols, ester class, organic acid etc. containing micro-heavy constituent.
(3) to circulation reboiler supply heating agent, start to heat material in rectifying column, make the steam of light component increase, control feed back by overhead reflux extraction control system and return rectifying column, withdrawing fluid makes the filler complete wetting of full tower;
(4) when liquid level in rectifying column higher than total liquid level 2/3 time, open the valve of extraction reboiler gas phase pipe, make extraction reboiler and tower bottom of rectifying tower pressure balance, then extraction reboiler liquid-phase tube is opened, in rectifying column, liquid flow in extraction reboiler, to extraction reboiler supply heating agent, the light component entering into extraction reboiler is continued heating evaporation, after the liquidus temperature of extraction reboiler reaches suitable temperature, close extraction reboiler liquid-phase tube valve, continue to be heated to extraction reboiler and reach high some temperature, to open on tower reactor extraction pipeline valve by outside kettle material extraction battery limit (BL).
Method removing light naphtha may be used for atmospheric operation, decompression operation also may be used for pressurized operation for this; The medium higher for atmospheric boiling point adopts decompression operation, for reducing the operating temperature of tower reactor, in case the pyrolytic of material or coking; The material lower for atmospheric boiling point adopts atmospheric operation.
Raw material handled by described rectificating method is the material containing trace or the thing that heavily boils on a small quantity.The charging of described rectifying column is continuous feed mode, and the extraction of tower reactor can adopt continuation mode also can adopt interval extraction mode.
Embodiment 3
Remove heavy component for fatty acid methyl ester below, be further explained the present invention, the material composition in the present embodiment is mass fraction.
Mixture to be separated is the fatty acid methyl ester solution containing the thing that heavily boils, and wherein, the mass fraction of fatty acid methyl ester is 95%, and other are methyl alcohol and the thing that heavily boils on a small quantity.Raw material is with in a continuous fashion 20 blocks of plates of the rectifying column 1 of 28 pieces of numbers of plates through feedstock pump pressurization.The inbound traffics that add being controlled raw material by feed rate control system 15 are 1250kg/h.
In the operating condition of rectifying column 1, the operating temperature of tower top is 190 DEG C, and operating pressure is 5Kpa, and the operating temperature of rectifying column 1 tower reactor is 230 DEG C, and extraction reboiler 5 liquidus temperature is about 245 DEG C ± 10 DEG C.The thermal fluid inlet of heat exchanger 11 is connected with the gas phase of rectifying column, to be supplied raw materials preheating energy by the steam of tower top fatty acid methyl ester, and temperature when raw material enters rectifying column 1 is 170 DEG C.
Material carries out gas-liquid Mass and heat transfer in rectifying column 1, obtains qualified fatty acid methyl ester product at rectifying column 1 tower top, and flow is 1200kg/h.
Circulation reboiler 9 is for forcing falling-film reboiler, circulation is completed by circulating pump 8, the recycle stock of tower reactor circulating pump 8 is the tower reactor material being rich in fatty acid methyl ester, circulating temperature is 230 DEG C, internal circulating load is 20 tons/h, the extraction of extraction reboiler bottoms material interval, once, in extraction material, fatty acid methyl ester component content is 5%-10% in extraction in about every 8 hours.
Circulation reboiler adopts heat-conducting oil heating, and extraction reboiler adopts heat-conducting oil heating.
Embodiment 4
Take off heavy component to remove propyl acetate below, be further explained the present invention, the material composition in the present embodiment is mass fraction.
Mixture to be separated is the propyl acetate solution containing the thing that heavily boils, and wherein, the mass fraction of propyl acetate is 97.5%, and other are ethanol alcohol and the thing that heavily boils on a small quantity.Raw material is with in a continuous fashion 22 blocks of plates of the rectifying column 1 of 32 pieces of numbers of plates through feedstock pump pressurization.The inbound traffics that add being controlled raw material by feed rate control system 15 are 2300kg/h.
In the operating condition of rectifying column 1, the operating temperature of tower top is 102 DEG C, and operating pressure is normal pressure, and the operating temperature of rectifying column 1 tower reactor is 125 DEG C, and extraction reboiler 5 liquidus temperature is about 130 DEG C ± 5 DEG C.The thermal fluid inlet of heat exchanger 11 is connected with the gas phase of rectifying column, to be supplied raw materials preheating energy by the steam of tower top propyl acetate, and temperature when raw material enters rectifying column 1 is 90 DEG C.
Material carries out gas-liquid Mass and heat transfer in rectifying column 1, obtains qualified propyl acetate product at rectifying column 1 tower top, and flow is 2250kg/h.
Circulation reboiler 9 is thermosyphon reboiler, and recycle stock is the tower reactor material being rich in propyl acetate, and circulating temperature is 125 DEG C, internal circulating load is 25.8 tons/h, the extraction of extraction reboiler bottoms material interval, once, in extraction material, propyl acetate component content controls within 5% in extraction in about every 10 hours.
Circulation reboiler 9 adopts Steam Heating, and extraction reboiler 5 adopts Steam Heating.
The above; it is only preferred embodiment of the present invention; not do any pro forma restriction to the present invention, those skilled in the art utilize the technology contents of above-mentioned announcement to make a little any amendment, equivalent variations or modification, all drop in protection scope of the present invention.

Claims (5)

1. one kind removes the method for light naphtha with the rectifier unit comprising two reboiler, it is characterized in that: described rectifier unit comprises rectifying column, circulation reboiler, extraction reboiler, heat exchanger, condenser, reflux-withdrawal control system and product pans, circulation reboiler is connected with the tower reactor of rectifying column respectively with extraction reboiler, extraction reboiler liquid-phase tube and extraction reboiler gas phase pipe is provided with between extraction reboiler and rectifying column, raw material heat exchanger and condenser is provided with between described rectifying column and reflux-withdrawal control system, product pans are connected with reflux-withdrawal control system, described rectifying column takes into account the tower reactor gas phase temperature detector for detecting tower reactor gas phase temperature in the tower reactor tower reactor liquid level be provided with for detecting tower reactor liquid level, described circulation reboiler is connected with the tower reactor of rectifying column by tower reactor circulating pump, described rectifying column feeding line is provided with feed rate control system, bottom described extraction reboiler, bobbin carriage is provided with extraction reboiler liquidus temperature mouth and tower reactor extraction pipeline,
The method adopting above-mentioned rectifier unit to remove light naphtha is:
(1) raw material needing to be separated is controlled feed rate by feed rate control system, raw material flows through tower top heat exchanger and overhead vapours carries out heat exchange, charging in the middle part of rectifying column;
(2) to circulation reboiler supply heating agent, start to heat material in rectifying column, make the steam of light component increase, control feed back by overhead reflux extraction control system and return rectifying column, withdrawing fluid makes the filler complete wetting of full tower;
(3) when tower reactor liquid level in rectifying column is higher than restriction liquid level, open the valve of extraction reboiler gas phase pipe, make extraction reboiler and tower bottom of rectifying tower pressure balance, then extraction reboiler liquid-phase tube is opened, in rectifying column, liquid flow in extraction reboiler, to extraction reboiler supply heating agent, the light component entering into extraction reboiler is continued heating evaporation, after the liquidus temperature of extraction reboiler reaches the saturation temperature of the thing mixture that heavily boils, close extraction reboiler liquid-phase tube valve, continue to be heated to extraction reboiler and reach high some temperature, to open on tower reactor extraction pipeline valve by outside kettle material extraction battery limit (BL).
2. the rectifier unit with comprising two reboiler according to claim 1 removes the method for light naphtha, it is characterized in that: described circulation reboiler is forced circulating reboiler, forces falling-film reboiler, thermosyphon reboiler or a through type reboiler, the polishing of described circulation reboiler heat exchanger tube inwall.
3. the rectifier unit with comprising two reboiler according to claim 1 removes the method for light naphtha, it is characterized in that: described extraction reboiler is immersion shell and tube reboiler, the polishing of described immersion shell and tube reboiler heat exchanger tube inwall, heat medium adopts Steam Heating or heat-conducting oil heating.
4. the rectifier unit with comprising two reboiler according to claim 1 removes the method for light naphtha, it is characterized in that: described extraction reboiler is positive displacement reboiler, the polishing of described positive displacement reboiler cylinder inboard wall, heat medium adopts Steam Heating or heat-conducting oil heating.
5. the rectifier unit with comprising two reboiler according to claim 1 removes the method for light naphtha, it is characterized in that: the feeding manner of described rectifying column is continuous feed mode, and the extraction of tower reactor adopts continuous extraction mode or interval extraction mode.
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