CN107365253A - A kind of propylene glycol methyl ether acetate distillation system and its rectificating method - Google Patents

A kind of propylene glycol methyl ether acetate distillation system and its rectificating method Download PDF

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Publication number
CN107365253A
CN107365253A CN201710584100.7A CN201710584100A CN107365253A CN 107365253 A CN107365253 A CN 107365253A CN 201710584100 A CN201710584100 A CN 201710584100A CN 107365253 A CN107365253 A CN 107365253A
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tower
light component
refined
pipeline
return tank
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Inventor
曹圣平
孙百亚
赵跃
陈电华
姜伟伟
肖春生
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Rugao Ran Chemical Materials Co Ltd
WUXI BAICHUAN CHEMICAL INDUSTRIAL Co Ltd
BAICHUAN CHEMICAL (RUGAO) Co Ltd
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Rugao Ran Chemical Materials Co Ltd
WUXI BAICHUAN CHEMICAL INDUSTRIAL Co Ltd
BAICHUAN CHEMICAL (RUGAO) Co Ltd
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Priority to CN201710584100.7A priority Critical patent/CN107365253A/en
Publication of CN107365253A publication Critical patent/CN107365253A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/52Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C67/54Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The present invention relates to a kind of propylene glycol methyl ether acetate distillation system and its rectificating method, compression rectification tower is entered by the de- thick finished product continuous conveying gently handled of preceding step, material into tower heats by tower reactor reboiler, gas phase is then condensed by top gaseous phase pipe by double-effect heat exchanger, and liquid is presented and enters refined return tank;Phegma is refluxed into compression rectification tower by a refined reflux pump part in refined return tank, a part of then be cooled within 40 DEG C by finished product cooler and adopted as finished product into finished pot;Save the light component that packed tower is used to be enriched with thick finished product, i.e. water, acetic acid and propylene glycol monomethyl ether in refined return tank top one.The advantage of the invention is that:On the one hand rectification process of the present invention reaches energy-conservation purpose by the way of energy-saving dual-purpose and flash distillation combine;Still further aspect can reduce light component in finished product using flash distillation plant, so as to reach the purpose for improving product purity.

Description

A kind of propylene glycol methyl ether acetate distillation system and its rectificating method
Technical field
The invention belongs to fine chemicals production field, more particularly to a kind of propylene glycol methyl ether acetate distillation system and its Rectificating method.
Background technology
Propylene glycol methyl ether acetate is the less toxic advanced industrial solvent of function admirable, is had to polarity and nonpolar material Very strong solvability, suitable for high-grade paint, the solvent of the various polymer of ink, including it is amino methyl acid esters, vinyl, poly- Ester, cellulose acetate, alkyd resin, acrylic resin, epoxy resin and nitrocellulose etc..Wherein.Propylene glycol monomethyl ether third Acid esters is solvent best in coating, ink, suitable for unsaturated polyester (UP), polyurethane based resin, acrylic resin, epoxy resin Deng.
With the continuous development of market economy, the technical threshold and fund threshold of all kinds of chemical products are relatively more and more lower, Market tends to saturation, basically reaches supply and marketing balance, or even drug on the market, and the profit of product increasingly tends to equalize, the past that The kind sudden huge profits epoch have not been existed, and this is also wanted to the enterprise that produces or will invest with bigger pressure, enterprise The market of keen competition obtains one seat and original technique is transformed, it is necessary to put into substantial amounts of technical force and fund, On the one hand it is energy consumption and the material consumption for reducing product, is exactly the quality for improving product in addition, the competitiveness of product in market could be improved.
According to traditional propylene glycol methyl ether acetate product processes, mainly existed with raw material propylene glycol monomethyl ether and acetic acid The mixture of synthesizing propylene glycol monomethyl ether acetate under acidic catalyst effect, then it is not engaged in the third of reaction by pretreatment removing Glycol methyl ether and acetic acid, crude product is finally entered into rectifying column, in process of production, tower top is cold for the product tower in distillation process The condensate liquid of condenser is recirculated water, and because tower operation is atmospheric operation, gaseous substance is condensed in all towers, finally Condensate liquid participates in reflux in tower, and it is consistent with extraction composition to flow back, and the charging of the product tower is the mixed of propylene glycol methyl ether acetate Compound, after the processing of preceding process, still there is the light component that part is lighter than product, be to remove to finishing column, final Product purity maximum can only achieve 98.5%, and impurity is light component and mass content is more than 1%(Water, acetic acid, propylene glycol monomethyl ether).Root According to the requirement of HG/T3940-2007 standards, the purity requirement to propylene glycol methyl ether acetate is more than 99.5%, therefore only will be light Component eliminates from product, could improve the content of product to reach the requirement of standard.
Using current conventional atmospheric distillation process, such as accompanying drawing 1, it is necessary to equipment have:Tower reactor reboiler 1,, atmospheric distillation Tower 2,, reflux pump 3,, overhead condenser 4,, return tank 5,;By the way of rectifying is illustrated, through taking off the half of light component processing into Product continuously enter rectifying column 2 by metering,, tower reactor reboiler 1,Heated using steam, most of material in tower is steamed with gas phase Tower top is distillated, then through overhead condenser 4,Condense within 40 DEG C, enter return tank 5,, then be back to through a reflux pump part Tower 2,Interior, a part of qualified product then produces system, into finished pot.Whole distillation process, on the one hand need that tower will be entered Interior all materials are all heated to be gas phase, then condensed device is all condensed into liquid phase, this completely heated up and total condensation Mode is a kind of waste to the energy;Still further aspect takes off the treated material of light component still also containing micro light due to preceding step Component, it is to remove on the basis of existing process, because light component is(Water, acetic acid, propylene glycol monomethyl ether), in distillation process Return tank is brought into as condensate liquid is condensed together, so to solve product quality problem in traditional handicraft is to be difficult to 's.
Understand by analysis, the rectifier unit in existing propylene glycol methyl ether acetate production technology, it is difficult to which finished product is pure Degree brings up to HG/T3940-2007 standard requirement, i.e., final product quality content is more than 99.5%, and existing process energy consumption is big, and having must Studying a kind of process route reduces propylene glycol methyl ether acetate lmpurities content so as to reach the mesh of raising product purity 's.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of propylene glycol methyl ether acetate distillation system and its rectificating method, On the one hand the rectification process reaches energy-conservation purpose by the way of energy-saving dual-purpose and flash distillation combine;Still further aspect utilizes flash distillation Device can reduce light component in finished product, so as to reach the purpose for improving product purity.
In order to solve the above technical problems, the technical scheme is that:A kind of propylene glycol methyl ether acetate distillation system, its Innovative point is:The distillation system includes compression rectification tower, reboiler, double-effect heat exchanger and refined return tank;
One side wall of the compression rectification tower is disposed with the material inlet A of connection compression rectification tower from top to bottom and gas enters Mouthful, the bottom of the compression rectification tower is respectively arranged with the material outlet A and heavy constituent extraction mouth of connection compression rectification tower;
The upper portion side wall of the reboiler is provided with the gas vent of a connection reboiler, and the bottom centre of the reboiler is provided with one The material inlet B of reboiler is connected, and gas feed is connected with gas vent by pipeline A, material outlet A and material inlet B Connected by pipeline B;
The top of the compression rectification tower connects double-effect heat exchanger by gas phase pipe, and the lower sides of the double-effect heat exchanger are provided with The liquid outlet of one connection double-effect heat exchanger;
The top of the refined return tank is provided with the liquid-inlet of the refined return tank of a connection, the liquid outlet and liquid-inlet Connected by pipeline C, and the light component flash column that a connection refines return tank is additionally provided with the top of refined return tank;It is described light Component flash column connects light component cooler by pipeline D, and extraction regulating valve, the extraction regulating valve are provided with pipeline D Flowmeter is also connected by pipeline E, and flowmeter is arranged in parallel with light component cooler;
The refined return tank is also connected by pipeline F with the top of compression rectification tower, and has also been arranged in series essence on pipeline F Reflux pump processed;The pipeline F also connects a finished product cooler by pipeline G.
A kind of method for carrying out rectifying with above-mentioned propylene glycol methyl ether acetate distillation system, its innovative point are:It is described Method comprises the following steps:
(1)Compression rectification tower is delivered into by the de- thick finished product gently handled of preceding step, after more than 50% liquid level is reached in tower, Stop charging, start to convey steam to tower reactor reboiler, material in tower is heated, progressively vaporized material in tower, pass through Refined return tank is entered after double-effect heat exchanger condensation;
(2)When starting operation, extraction regulating valve at the top of light component flash column is closed, in the way of conventional distillation, is opened refined Reflux pump carries out forced refluence, is stepped up reboiler steam supply, tower temperature and tower pressure will be progressively enhanced, rectifying to be pressurised When tower tower pressure reaches more than 0.35MPa, extraction regulating valve to be opened, carries out emptying processing to system, systems stabilisation pressure is 0.3~ 0.4MPa;
(3)After rectifying column charging to be pressurised is normal, steam supply amount progressively tends towards stability, and it is 2/ to control compression rectification tower reflux ratio 1~3/1, extraction governor valve control light component extraction flow FI1 adopt with cooling down the finished product adopted into finished pot through light component cooler Outflow FI2 ratios are 1/20~1/5.
The advantage of the invention is that:
(1)Propylene glycol methyl ether acetate distillation system of the present invention, double-effect heat exchanger has been used in the distillation system, the heat exchanger one Aspect is used for the condenser of compression rectification tower, can be used in addition as the reboiler of the atmospheric tower in preceding step process, main Purpose can be arrived to energy-conservation, temperature control function;That is the heat that the gas phase of compression rectification tower is condensed can be for step tower apparatus before doing Thermal source, preceding step tower need then to be conserved by steam-heated cost originally;Furthermore make economic benefits and social benefits because overhead condenser changes, originally Substantial amounts of recirculated water is needed as low-temperature receiver to condense, and this programme only needs two small heat exchangers, i.e. finished product cooler and light component Condenser, it is necessary to recirculated water then be former heat exchanger half size, low-temperature receiver can be saved herein, that is, saved electric energy;
(2)Propylene glycol methyl ether acetate distillation system of the present invention, wherein, refined return tank plays two works in this distillation system With, be on the one hand as return tank, still further aspect be then as flash tank use, for the flash distillation to light component, so as to reach Improve the purpose of product purity;Verified by actual production, after this programme is implemented, the product purity of propylene glycol methyl ether acetate by More than 99% is brought up within 98.5% originally, impurity is then accordingly reduced, especially moisture and acidity, has reached 300ppm Within, even if product quality has reached the requirement of HG/T3940-2007 standards;
(3)The method that the present invention uses propylene glycol methyl ether acetate distillation system rectifying, employs double-effect heat exchanger so that this technology Condensate liquid in scheme need not be condensed into 40 DEG C, it is only necessary to 130 can be condensed under the conditions of 0.3MPa pressure above DEG C, the phegma of same flow, which is refluxed, enters compression rectification tower, 40 DEG C of traditional handicraft with 130 DEG C in this programme Compared to, it is necessary at least 90 DEG C of vaporization sensible heat, and it is final all by as the cost of product, and then rectificating method of the present invention is used, The finished product of product can also be substantially reduced.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the structural representation that propylene glycol methyl ether acetate produces traditional distillation system.
Fig. 2 is the structural representation of propylene glycol methyl ether acetate distillation system of the present invention.
Embodiment
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this It is bright to be limited among described scope of embodiments.
Propylene glycol methyl ether acetate distillation system of the present invention, as shown in Fig. 2 including compression rectification tower 2, reboiler 1, economic benefits and social benefits Heat exchanger 4 and refined return tank 5.
One side wall of compression rectification tower 2 is disposed with the material inlet A and gas of connection compression rectification tower 2 from top to bottom Import, the bottom of compression rectification tower 2 are respectively arranged with the material outlet A and heavy constituent extraction mouth of connection compression rectification tower 2.
The upper portion side wall of reboiler 1 is provided with the gas vent of a connection reboiler 1, and the bottom centre of reboiler 1 is provided with one The material inlet B of reboiler 1 is connected, and gas feed is connected with gas vent by pipeline A, material outlet A and material inlet B Connected by pipeline B.
The top of compression rectification tower 2 connects double-effect heat exchanger 4 by gas phase pipe 9, and the lower sides of double-effect heat exchanger 4 are provided with The liquid outlet of one connection double-effect heat exchanger 4.
The top of refined return tank 5 is provided with the liquid-inlet of the refined return tank 5 of a connection, and liquid outlet leads to liquid-inlet Piping C is connected, and the light component flash column 6 that a connection refines return tank 5 is additionally provided with the top of refined return tank 5;Light group Divide flash column 6 to connect light component cooler 8 by pipeline D, and extraction regulating valve 10 is provided with pipeline D, produce regulating valve 10 Flowmeter 11 is also connected by pipeline E, and flowmeter 11 is arranged in parallel with light component cooler 8.
Refined return tank 5 is also connected by pipeline F with the top of compression rectification tower 2, and has also been arranged in series on pipeline F Refined reflux pump 3;Pipeline F also connects a finished product cooler 7 by pipeline G.
Propylene glycol methyl ether acetate rectifying is carried out with above-mentioned propylene glycol methyl ether acetate distillation system, is comprised the following steps:
(1)Compression rectification tower 2 is delivered into by the de- thick finished product gently handled of preceding step, after more than 50% liquid level is reached in tower, Stop charging, start to convey steam to tower reactor reboiler 1, material in tower is heated, progressively vaporized material in tower, pass through Double-effect heat exchanger 4 enters refined return tank 5 after condensing;
(2)When starting operation, the top of light component flash column 6 extraction regulating valve is closed, in the way of conventional distillation, is opened refined Reflux pump 3 carries out forced refluence, is stepped up the steam supply amount of reboiler 1, tower temperature and tower pressure will be progressively enhanced, essence to be pressurised When evaporating the tower pressure of tower 2 and reaching more than 0.35MPa, extraction regulating valve 10 is opened, emptying processing is carried out to system, systems stabilisation pressure is 0.3~0.4MPa;
(3)Rectifying column 2 to be pressurised feed it is normal after, steam supply amount progressively tends towards stability, and controls the reflux ratio of compression rectification tower 2 to be 2/1~3/1, extraction regulating valve 10 control light component extraction flow FI1 with through light component cooler 8 cooling adopt into finished pot into Product extraction flow FI2 ratios are 1/20~1/5.
Propylene glycol methyl ether acetate rectificating method of the present invention is described in detail below by specific embodiment:
Embodiment 1
The present embodiment propylene glycol methyl ether acetate rectificating method, comprises the following steps:
(1)Compression rectification tower 2 is delivered into by the de- thick finished product gently handled of preceding step, after more than 50% liquid level is reached in tower, Stop charging, start to convey steam to tower reactor reboiler 1, material in tower is heated, progressively vaporized material in tower, pass through Double-effect heat exchanger 4 enters refined return tank 5 after condensing;
(2)When starting operation, the top of light component flash column 6 extraction regulating valve is closed, in the way of conventional distillation, is opened refined Reflux pump 3 carries out forced refluence, is stepped up the steam supply amount of reboiler 1, tower temperature and tower pressure will be progressively enhanced, essence to be pressurised When evaporating the tower pressure of tower 2 and reaching more than 0.35MPa, extraction regulating valve 10 is opened, emptying processing is carried out to system, systems stabilisation pressure is 0.3~0.4MPa;
(3)Rectifying column 2 to be pressurised feed it is normal after, steam supply amount progressively tends towards stability, and controls the reflux ratio of compression rectification tower 2 to be 2/1~3/1, extraction regulating valve 10 control light component extraction flow FI1 with through light component cooler 8 cooling adopt into finished pot into Product extraction flow FI2 ratios are 1/20;
(4)Tower is pressed with after tower temperature stabilization, and continuous feed and continuous extraction operation 1 hour, 2 hours, 3 hours, 4 hours are respectively to adopting Go out finished product and extraction light component is sampled and analyzes and try to achieve average content.
The specific energy consumption of the present embodiment contrast past technique, reduces 13%, the analysis of propylene glycol methyl ether acetate finished product content It is 99% to obtain average value, and especially light component content is down to 0.53%;The light component of extraction is analyzed to contain propane diols in light component Methyl ether acetate mass content is 20%.
Embodiment 2
The present embodiment propylene glycol methyl ether acetate rectificating method, comprises the following steps:
(1)Compression rectification tower 2 is delivered into by the de- thick finished product gently handled of preceding step, after more than 50% liquid level is reached in tower, Stop charging, start to convey steam to tower reactor reboiler 1, material in tower is heated, progressively vaporized material in tower, pass through Double-effect heat exchanger 4 enters refined return tank 5 after condensing;
(2)When starting operation, the top of light component flash column 6 extraction regulating valve is closed, in the way of conventional distillation, is opened refined Reflux pump 3 carries out forced refluence, is stepped up the steam supply amount of reboiler 1, tower temperature and tower pressure will be progressively enhanced, essence to be pressurised When evaporating the tower pressure of tower 2 and reaching more than 0.35MPa, extraction regulating valve 10 is opened, emptying processing is carried out to system, systems stabilisation pressure is 0.3~0.4MPa;
(3)Rectifying column 2 to be pressurised feed it is normal after, steam supply amount progressively tends towards stability, and controls the reflux ratio of compression rectification tower 2 to be 2/1~3/1, extraction regulating valve 10 control light component extraction flow FI1 with through light component cooler 8 cooling adopt into finished pot into Product extraction flow FI2 ratios are 1/18;
(4)Tower is pressed with after tower temperature stabilization, and continuous feed and continuous extraction operation 1 hour, 2 hours, 3 hours, 4 hours are respectively to adopting Go out finished product and extraction light component is sampled and analyzes and try to achieve average content.
The specific energy consumption of the present embodiment contrast technique in the past, reduces 13.1%, and embodiment 1 is 13%, is slightly changed, and the third two It is 99.2% that the analysis of alcohol methyl ether acetate finished product content, which obtains average value, and especially light component content is down to 0.453%;What is produced is light It is 30% that component analysis, which obtains mass content containing propylene glycol methyl ether acetate in light component,.
Embodiment 3
The present embodiment propylene glycol methyl ether acetate rectificating method, comprises the following steps:
(1)Compression rectification tower 2 is delivered into by the de- thick finished product gently handled of preceding step, after more than 50% liquid level is reached in tower, Stop charging, start to convey steam to tower reactor reboiler 1, material in tower is heated, progressively vaporized material in tower, pass through Double-effect heat exchanger 4 enters refined return tank 5 after condensing;
(2)When starting operation, the top of light component flash column 6 extraction regulating valve is closed, in the way of conventional distillation, is opened refined Reflux pump 3 carries out forced refluence, is stepped up the steam supply amount of reboiler 1, tower temperature and tower pressure will be progressively enhanced, essence to be pressurised When evaporating the tower pressure of tower 2 and reaching more than 0.35MPa, extraction regulating valve 10 is opened, emptying processing is carried out to system, systems stabilisation pressure is 0.3~0.4MPa;
(3)Rectifying column 2 to be pressurised feed it is normal after, steam supply amount progressively tends towards stability, and controls the reflux ratio of compression rectification tower 2 to be 2/1~3/1, extraction regulating valve 10 control light component extraction flow FI1 with through light component cooler 8 cooling adopt into finished pot into Product extraction flow FI2 ratios are 1/15;
(4)Tower is pressed with after tower temperature stabilization, and continuous feed and continuous extraction operation 1 hour, 2 hours, 3 hours, 4 hours are respectively to adopting Go out finished product and extraction light component is sampled and analyzes and try to achieve average content.
The specific energy consumption of the present embodiment contrast technique in the past, reduces 12.8%, and embodiment 1 is 13%, and change increases, and the third two It is 99.5% that the analysis of alcohol methyl ether acetate finished product content, which obtains average value, and especially light component content is down to 0.25%;What is produced is light It is 50% that component analysis, which obtains mass content containing propylene glycol methyl ether acetate in light component,.
Embodiment 4
The present embodiment propylene glycol methyl ether acetate rectificating method, comprises the following steps:
(1)Compression rectification tower 2 is delivered into by the de- thick finished product gently handled of preceding step, after more than 50% liquid level is reached in tower, Stop charging, start to convey steam to tower reactor reboiler 1, material in tower is heated, progressively vaporized material in tower, pass through Double-effect heat exchanger 4 enters refined return tank 5 after condensing;
(2)When starting operation, the top of light component flash column 6 extraction regulating valve is closed, in the way of conventional distillation, is opened refined Reflux pump 3 carries out forced refluence, is stepped up the steam supply amount of reboiler 1, tower temperature and tower pressure will be progressively enhanced, essence to be pressurised When evaporating the tower pressure of tower 2 and reaching more than 0.35MPa, extraction regulating valve 10 is opened, emptying processing is carried out to system, systems stabilisation pressure is 0.3~0.4MPa;
(3)Rectifying column 2 to be pressurised feed it is normal after, steam supply amount progressively tends towards stability, and controls the reflux ratio of compression rectification tower 2 to be 2/1~3/1, extraction regulating valve 10 control light component extraction flow FI1 with through light component cooler 8 cooling adopt into finished pot into Product extraction flow FI2 ratios are 1/12;
(4)Tower is pressed with after tower temperature stabilization, and continuous feed and continuous extraction operation 1 hour, 2 hours, 3 hours, 4 hours are respectively to adopting Go out finished product and extraction light component is sampled and analyzes and try to achieve average content.
The specific energy consumption of the present embodiment contrast past technique, reduces 12.5%, propylene glycol methyl ether acetate finished product content point Extract average value be 99.6%, especially light component content is down to 0.15%;The light component of extraction is analyzed to contain third in light component Glycol methyl ether acetate mass content is 65%.
Embodiment 5
The present embodiment propylene glycol methyl ether acetate rectificating method, comprises the following steps:
(1)Compression rectification tower 2 is delivered into by the de- thick finished product gently handled of preceding step, after more than 50% liquid level is reached in tower, Stop charging, start to convey steam to tower reactor reboiler 1, material in tower is heated, progressively vaporized material in tower, pass through Double-effect heat exchanger 4 enters refined return tank 5 after condensing;
(2)When starting operation, the top of light component flash column 6 extraction regulating valve is closed, in the way of conventional distillation, is opened refined Reflux pump 3 carries out forced refluence, is stepped up the steam supply amount of reboiler 1, tower temperature and tower pressure will be progressively enhanced, essence to be pressurised When evaporating the tower pressure of tower 2 and reaching more than 0.35MPa, extraction regulating valve 10 is opened, emptying processing is carried out to system, systems stabilisation pressure is 0.3~0.4MPa;
(3)Rectifying column 2 to be pressurised feed it is normal after, steam supply amount progressively tends towards stability, and controls the reflux ratio of compression rectification tower 2 to be 2/1~3/1, extraction regulating valve 10 control light component extraction flow FI1 with through light component cooler 8 cooling adopt into finished pot into Product extraction flow FI2 ratios are 1/10;
(4)Tower is pressed with after tower temperature stabilization, and continuous feed and continuous extraction operation 1 hour, 2 hours, 3 hours, 4 hours are respectively to adopting Go out finished product and extraction light component is sampled and analyzes and try to achieve average content.
The specific energy consumption of the present embodiment contrast past technique, reduces 11%, the analysis of propylene glycol methyl ether acetate finished product content It is 99.61% to obtain average value, and especially light component content is down to 0.14%;The light component of extraction analyze in light component containing the third two Alcohol methyl ether acetate mass content is 85%.
Embodiment 1~5 carries out data comparison and understood, the light component extraction regulating valve 10 in this programme is unlimited to be opened greatly preferably, Especially comparing embodiment 4 and embodiment 5 are understood, when increasing light component produced quantity, will be produced ratio with finished product and are adjusted to 1/ by 1/12 When 10, although finished product purity is still improved, simultaneously unobvious, and the finished product content in corresponding extraction light component rises very It hurry up, step reaction system, this aspect add side reaction before being recycled into due to the light component produced in this programme, last anti- And it is unfavorable for the purity of product;The energy consumption of step, is exactly finally the energy unit consumption for improving product before adding in addition.Pass through unit consumption Data will also realize that as the increase of light component produced quantity, energy unit consumption are stepping up.In summary embodiment, it is known that touch at present The light component produced quantity and finished product produced quantity ratio of rope are proper in 1/15~1/12 scope, so both ensure that product quality Preferably, it in turn ensure that energy unit consumption is proper.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The skill of the industry For art personnel it should be appreciated that the present invention is not limited to the above embodiments, described in above-described embodiment and specification is explanation The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and Its equivalent thereof.

Claims (2)

  1. A kind of 1. propylene glycol methyl ether acetate distillation system, it is characterised in that:The distillation system includes compression rectification tower, boiled again Device, double-effect heat exchanger and refined return tank;
    One side wall of the compression rectification tower is disposed with the material inlet A of connection compression rectification tower from top to bottom and gas enters Mouthful, the bottom of the compression rectification tower is respectively arranged with the material outlet A and heavy constituent extraction mouth of connection compression rectification tower;
    The upper portion side wall of the reboiler is provided with the gas vent of a connection reboiler, and the bottom centre of the reboiler is provided with one The material inlet B of reboiler is connected, and gas feed is connected with gas vent by pipeline A, material outlet A and material inlet B Connected by pipeline B;
    The top of the compression rectification tower connects double-effect heat exchanger by gas phase pipe, and the lower sides of the double-effect heat exchanger are provided with The liquid outlet of one connection double-effect heat exchanger;
    The top of the refined return tank is provided with the liquid-inlet of the refined return tank of a connection, the liquid outlet and liquid-inlet Connected by pipeline C, and the light component flash column that a connection refines return tank is additionally provided with the top of refined return tank;It is described light Component flash column connects light component cooler by pipeline D, and extraction regulating valve, the extraction regulating valve are provided with pipeline D Flowmeter is also connected by pipeline E, and flowmeter is arranged in parallel with light component cooler;
    The refined return tank is also connected by pipeline F with the top of compression rectification tower, and has also been arranged in series essence on pipeline F Reflux pump processed;The pipeline F also connects a finished product cooler by pipeline G.
  2. 2. a kind of method that propylene glycol methyl ether acetate distillation system with described in claim 1 carries out rectifying, it is characterised in that: Methods described comprises the following steps:
    (1)Compression rectification tower is delivered into by the de- thick finished product gently handled of preceding step, after more than 50% liquid level is reached in tower, Stop charging, start to convey steam to tower reactor reboiler, material in tower is heated, progressively vaporized material in tower, pass through Refined return tank is entered after double-effect heat exchanger condensation;
    (2)When starting operation, extraction regulating valve at the top of light component flash column is closed, in the way of conventional distillation, is opened refined Reflux pump carries out forced refluence, is stepped up reboiler steam supply, tower temperature and tower pressure will be progressively enhanced, rectifying to be pressurised When tower tower pressure reaches more than 0.35MPa, extraction regulating valve to be opened, carries out emptying processing to system, systems stabilisation pressure is 0.3~ 0.4MPa;
    (3)After rectifying column charging to be pressurised is normal, steam supply amount progressively tends towards stability, and it is 2/ to control compression rectification tower reflux ratio 1~3/1, extraction governor valve control light component extraction flow FI1 adopt with cooling down the finished product adopted into finished pot through light component cooler Outflow FI2 ratios are 1/20~1/5.
CN201710584100.7A 2017-07-18 2017-07-18 A kind of propylene glycol methyl ether acetate distillation system and its rectificating method Pending CN107365253A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN107827778A (en) * 2017-10-30 2018-03-23 烟台国邦化工机械科技有限公司 A kind of continuous rectification refines cyanoacetate compound device and its technique
CN110668926A (en) * 2019-11-25 2020-01-10 南通百川新材料有限公司 Propylene glycol methyl ether rectification purification system and method thereof
WO2020019283A1 (en) * 2018-07-27 2020-01-30 南通百川新材料有限公司 Propylene glycol methyl ether acetate rectification system and rectification method
CN113185390A (en) * 2021-04-07 2021-07-30 厦门中坤化学有限公司 Method for continuously separating propylene glycol methyl ether, cyclopentanone and propylene glycol methyl ether acetate
CN113599851A (en) * 2021-08-19 2021-11-05 南通百川新材料有限公司 Novel light component removal and rectification system and method for propylene glycol methyl ether acetate
CN115784851A (en) * 2022-10-28 2023-03-14 南通百川新材料有限公司 Novel propylene glycol methyl ether rectification production method

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CN205653372U (en) * 2016-04-18 2016-10-19 百川化工(如皋)有限公司 Take off light system in propylene glycol methyl ether acetate production

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CN101172934A (en) * 2006-12-05 2008-05-07 褚雅志 Device and method for co-production or single production of refined methanol with rough methanol
CN205653372U (en) * 2016-04-18 2016-10-19 百川化工(如皋)有限公司 Take off light system in propylene glycol methyl ether acetate production

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107827778A (en) * 2017-10-30 2018-03-23 烟台国邦化工机械科技有限公司 A kind of continuous rectification refines cyanoacetate compound device and its technique
WO2020019283A1 (en) * 2018-07-27 2020-01-30 南通百川新材料有限公司 Propylene glycol methyl ether acetate rectification system and rectification method
CN110668926A (en) * 2019-11-25 2020-01-10 南通百川新材料有限公司 Propylene glycol methyl ether rectification purification system and method thereof
CN113185390A (en) * 2021-04-07 2021-07-30 厦门中坤化学有限公司 Method for continuously separating propylene glycol methyl ether, cyclopentanone and propylene glycol methyl ether acetate
CN113599851A (en) * 2021-08-19 2021-11-05 南通百川新材料有限公司 Novel light component removal and rectification system and method for propylene glycol methyl ether acetate
CN115784851A (en) * 2022-10-28 2023-03-14 南通百川新材料有限公司 Novel propylene glycol methyl ether rectification production method
CN115784851B (en) * 2022-10-28 2024-04-05 南通百川新材料有限公司 Propylene glycol methyl ether rectification production method

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