CN101412653A - Method for preparing phenylethylene by ethylbenzene gas-phase dehydrogenation and refining product of phenylethylene - Google Patents
Method for preparing phenylethylene by ethylbenzene gas-phase dehydrogenation and refining product of phenylethylene Download PDFInfo
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- CN101412653A CN101412653A CNA2007100471955A CN200710047195A CN101412653A CN 101412653 A CN101412653 A CN 101412653A CN A2007100471955 A CNA2007100471955 A CN A2007100471955A CN 200710047195 A CN200710047195 A CN 200710047195A CN 101412653 A CN101412653 A CN 101412653A
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The invention relates to a method for preparing styrene through the gas-phase dehydrogenation of ethylbenzene and refining a product. The method comprises the following steps: ethylbenzene as a raw material is heated and gasified in the presence of water; the ethylbenzene is subjected to gas-phase catalytic dehydrogenation reaction; the product of dehydrogenation reaction is condensed and is subjected to oil-water separation to obtain a coarse product; the coarse product is rectified to remove light composition impurities; the coarse product is rectified to remove the ethylbenzene; the ethylbenzene returns to a dehydrogenation material system for recycling; and the coarse product is rectified to remove heavy composition impurities so as to obtain the refined product of the ethylbenzene. The method is characterized in that a gas-phase material in the top of a tower for rectification and ethylbenzene removal is used as a heating medium and carries out heating on the ethylbenzene as the raw material and water so as to gasify the ethylbenzene. Compared with the prior method of multistage transformation heat integration for reclaiming heat energy, the method has the advantages that in the process of rectification and ethylbenzene removal, the reclaiming rate of heat energy is higher and can generally reach between 60 and 90 percent; and the method adopts single-tower operation for the ethylbenzene removal, and has simple process control as well as easy and stable operation. The method is in particular suitable for reconstructing the prior device.
Description
Technical field
The present invention relates to a kind of by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, particularly adopt the sequential method separation process carry out product purification by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method.
Background technology
Vinylbenzene is important basic organic, with fields such as device, weaving, building materials, light industry, toys important purposes is all arranged at automobile making, household electrical appliances by its material that makes.By ethyl benzene dehydrogenation preparation of styrene is leading at present industrialized preparing process, and material ethylbenzene gasifies in the presence of water (as thermal barrier), and further provides the required heat of reaction to carry out the vapor catalytic dehydrogenation reaction with water vapor.Usually adopt fixed-bed reactor, the active ingredient of dehydrogenation catalyst commonly used mainly comprises the oxide compound of ferric oxide and basic metal and alkaline-earth metal etc.Contain benzene, toluene and other light constituent impurity of by-product, unreacted ethylbenzene in the product of dehydrogenation reaction and, be necessary so will obtain the separation and purification of qualified styrene product dehydrogenation product based on the heavy constituent impurity of tar.In the prior art, vinylbenzene dehydrogenation product separation and purification mainly comprises and once takes off light method and two kinds of technical process of sequential method.Once take off light method with ethylbenzene with removed by a rectifying in the lump based on the light constituent of by product benzene and toluene, sequence rule is first to remove light constituents such as benzene and toluene by rectifying separation, and then rectifying separation removes ethylbenzene.Both respectively have its characteristics, and sequential method technology is applicable to the product purification process that dehydrogenation product light constituent content is more.
In the separation and purification process of products of dehydrogenation reactions, because the boiling-point difference very little (only being 9 ℃ under the normal pressure) of vinylbenzene and ethylbenzene, remove the ethylbenzene process and adopt precise distillation usually, Rectification Column's Theoretical Plate Number generally needs about 90, reflux ratio is generally about 7, thermal load is very high, and its energy consumption accounts for 3/4ths of whole separation and purification process total energy consumption.Therefore, the energy recovery that removes the ethylbenzene rectifying is to reduce the key of ethylbenzene gas-phase dehydrogenation preparation of styrene energy consumption.In the prior art, people adopt the integrated technology of stage variable pressure heat to reclaim this heat energy morely, the rectifying separation process that removes ethylbenzene is carried out in plural tower, the working pressure of tower reduces step by step, the cat head material of the tower that previous stage pressure is higher relatively is as the material of the back one-level tower heating medium that boils again, is that 99807390.3 Chinese patent, application number are the technical scheme that 200510083832.5 Chinese patent application all discloses this type of as the patent No..What of employing progression are the rate of recovery of the integrated recovery rectifying separation heat energy of stage variable pressure heat depend on, the many more rate of recovery of progression are high more in theory.But in fact too much progression causes the reduction of practical value because the complicacy of equipment and operating procedure greatly increases, the general integrated heat energy that reclaim ethylbenzene and vinylbenzene sepn process of two-stage transformation heat that adopt in the prior art more, be that the rectifying separation process is carried out in two rectifying tower, the rate of recovery of its heat energy can reach 40～50% at the most.
Summary of the invention
The invention provides a kind ofly by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, the technical problem that it will solve is further to improve the rate of recovery that removes ethylbenzene rectifying heat energy in the separation and purification of products of dehydrogenation reactions.
Below be the technical scheme that the present invention solves the problems of the technologies described above:
A kind of by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, this method may further comprise the steps:
1) material ethylbenzene heating and gasifying in the presence of water;
2) Qi Hua ethylbenzene and water mixture carry out the vapor catalytic dehydrogenation reaction;
3) products of dehydrogenation reactions condensation liquefaction, getting oil phase material after oily water separation is the thick product of vinylbenzene;
4) the thick product of vinylbenzene carries out rectifying by rectifying tower, and cat head is discharged based on the benzene of dehydrogenation reaction by-product and the light constituent impurity of toluene;
5) the tower still material of step 4) carries out rectifying by rectifying tower, discharges unreacted ethylbenzene after the condensation of overhead gas phase materials, and ethylbenzene returns the reuse of dehydrogenation feed system;
6) the tower still material of step 5) carries out rectifying by rectifying tower, and cat head gets the vinylbenzene purified product, and the tower still is discharged the heavy constituent impurity based on tar.
Above-mentioned steps 1) in, described material ethylbenzene and water are heated as heating medium by the overhead gas phase materials of step 5) and to make it gasification, material ethylbenzene and water cool off the overhead gas phase materials of step 5) as heat-eliminating medium and make it condensation simultaneously.
In step 1), generally material ethylbenzene and water are heated by reboiler, reboiler can comprise main reboiler and auxiliary reboiler, both are arranged side by side mutually, the heating medium of main reboiler is the described overhead gas phase materials of step 5), auxiliary reboiler then adopts the heating medium of outer confession, as the water vapor from general facilities.
In order to guarantee the fully condensation of overhead gas phase materials quilt in the step 5), overhead gas phase materials in the step 5) and the material ethylbenzene in the step 1) and water can be again through second stage condensations after carrying out heat exchange, second stage condenser condensing adopts the heat-eliminating medium of outer confession, as the water coolant from general facilities.
Generally, above-mentioned steps 1) the quality feed ratio of described material ethylbenzene and water is 1.8～2.2: 1; The working pressure of the described rectifying of step 5) is 20～100KPa absolute pressure, is preferably 30～50KPa absolute pressure; The reflux ratio of the described rectifying of step 5) is 4～17; Be preferably 6～10.
In the present invention, the dehydrogenation product treating process adopts sequential method technology, the main technical process of reaction of the vapor catalytic dehydrogenation of ethylbenzene and product treating process thereof and parameter and traditional method are basic identical, and the required heat energy of the heat energy that its key is rectifying separation in the dehydrogenation product treating process is removed ethylbenzene and material gasification is mutually integrated.
The contriver analyzes by vapor catalytic dehydrogenation reaction and the refining full-range energy consumption of product thereof to ethylbenzene, and carry out finding after the corresponding heat calculation, the boiling point of the azeotropic system of material ethylbenzene and water is 92 ℃, and the condensing temperature that removes the rectifying tower overhead gas phase materials of ethylbenzene is 105 ℃, its temperature difference is 13 ℃, is that heating medium heats to make it to gasify to the former and has enough thermal driving forces with the latter; In addition, generally speaking by producing per kilogram vinylbenzene purified product, the heat energy that condensation produced that removes the rectifying tower overhead gas phase materials of ethylbenzene is about the 590kw/kg product, the required energy consumption of material ethylbenzene and aqueous vaporization is about the 630kw/kg product, in theory, the heat energy that condensation produced that removes the rectifying tower overhead gas phase materials of ethylbenzene under perfect condition can 100% obtains reclaiming.The contriver finds that by test its rate of recovery is at least 60%, can reach 90% at most.
Compared with prior art, the invention has the advantages that the rectifying heat energy recovery rate that removes ethylbenzene in the separation and purification of products of dehydrogenation reactions significantly improves, and generally can reach 60～90%.The rectifying that removes ethylbenzene adopts single tower operation, and technology controlling and process is simple, and the device operation is easier steadily.Another advantage of the present invention is to be fit to very much conventional apparatus is transformed, and the equipment of main flow and operating procedure need not change, only can realize the energy-saving and cost-reducing of whole device significantly to part interchanger and relevant pipeline adjustment.
To come below that the invention will be further described by embodiment, as previously mentioned, the required heat energy of the heat energy that key of the present invention is rectifying separation in the dehydrogenation product treating process is removed ethylbenzene and material gasification is mutually integrated, the main technical process of reaction of the vapor catalytic dehydrogenation of ethylbenzene and product treating process thereof and parameter and traditional method are basic identical, and these are well known to those of ordinary skill in the art.Therefore, in order technical scheme more of the present invention to be described, embodiment will pay attention to the displaying of required mutually integrated this details of heat energy of heat energy that rectifying separation in the dehydrogenation product treating process removes ethylbenzene and material gasification.Be understood that for those of ordinary skills, the omission of other parts details does not influence the full implementation of technical solution of the present invention.
Description of drawings
Accompanying drawing is the thick product purification process of the vinylbenzene of an embodiment of the invention schema.
Each mark is defined as in the accompanying drawing:
1---lightness-removing column; 2---take off ethylbenzene tower; 3---weight-removing column; 4---the dehydrogenation reaction head tank; 5---dehydrogenation reaction head tank master reboiler; 6---the dehydrogenation reaction head tank is assisted reboiler; 7---take off ethylbenzene tower cat head material second stage condenser; M1---the thick product of vinylbenzene; M2---lightness-removing column tower still material; M3---based on the light constituent impurity of benzene and toluene; M4---take off ethylbenzene Tata still material; M5---take off ethylbenzene tower overhead gas phase materials; M5-1---take off ethylbenzene tower overhead condensation backflow material; M5-2---cyclically utilizing ethylbenzene; M6---vinylbenzene purified product; M7---based on the heavy constituent impurity of tar; RM1---material ethylbenzene; RM2---water; RM3---the circulation of dehydrogenation reaction raw material is boiled and is added thermal material; The dehydrogenation reaction raw material of RM4---gasification.
Embodiment
Below in conjunction with accompanying drawing embodiment is described:
Material ethylbenzene RM1 and RM2 water drop in the dehydrogenation reaction head tank 4, the quality feed ratio is controlled to be 2.0～2.1: 1, material ethylbenzene is heated gasification in the presence of water, the dehydrogenation reaction raw material of gasification (gas phase mixture of ethylbenzene and water) RM4 goes dehydrogenation reactor to carry out the vapor catalytic dehydrogenation reaction.Dehydrogenation reaction raw material circulation is boiled and is added thermal material RM3 by the heating of boiling again of main reboiler 5 arranged side by side mutually and auxiliary reboiler 6, wherein auxiliary reboiler employing 0.4kg/cm
2Low-pressure steam be heating medium.
Behind the products of dehydrogenation reactions condensation liquefaction, get oil phase material through oily water separation and obtain the thick product M1 of vinylbenzene, its composition sees the following form:
| Component | Content (weight %) |
| Vinylbenzene | 60.42 |
| Ethylbenzene | 37.61 |
| Benzene | 0.27 |
| Toluene | 1.18 |
| Tar | 0.26 |
| Other light constituent impurity | 0.14 |
| Other heavy constituent impurity | 0.02 |
| Water | Surplus |
The thick product M1 of vinylbenzene is introduced into lightness-removing column 1 and carries out rectifying, by the light constituent impurity M3 of cat head discharge based on benzene and toluene.The theoretical plate number of lightness-removing column 1 is 20～25, and working pressure is 25～30KPa absolute pressure, and reflux ratio is 25～30.The tower still material M2 rich in styrene of lightness-removing column, and contain unreacted ethylbenzene and heavy constituent impurity.
Lightness-removing column tower still material M2 enters and takes off ethylbenzene tower 2 and carry out precise distillation, and the theoretical plate number of taking off ethylbenzene tower 2 is 85～95, and working pressure is 30～50KPa absolute pressure, and reflux ratio is 6～9.Take off ethylbenzene tower overhead gas phase materials M5 and be introduced into dehydrogenation reaction head tank master reboiler 5, boil again with dehydrogenation reaction raw material circulation and to add thermal material RM3 and carry out heat exchange, the gas-liquid mixed material that goes out autonomous reboiler 5 is again through the 7 further condensations of second stage condenser, a part of M5-1 of condensation material returns and takes off ethylbenzene tower, another part M5-2 discharges and takes off ethylbenzene tower 2, returns the dehydrogenation reaction head tank as cyclically utilizing ethylbenzene.Tower still material M4 rich in styrene, and contain heavy constituent impurity.
Need to prove that second stage condenser 7 mainly act as replenishing of main reboiler 5 and standby, when driving to wait other working condition that fluctuation takes place, guarantee gaseous phase materials M5, thereby guarantee the device smooth running and have good turndown ratio by fully condensation.
Take off ethylbenzene Tata still material M4 and enter weight-removing column 3 at last and carry out rectifying, the theoretical plate number of weight-removing column 3 is 35～40, and working pressure is 10～15KPa absolute pressure, and reflux ratio is 0.6～1.0.Obtain vinylbenzene purified product M6 by cat head, the tower still is discharged the heavy constituent impurity M7 based on tar.
Embodiment is with the operation of above-mentioned technical process and parameter, is 75 tons/hour scale production by vinylbenzene output, and the inlet amount of the thick product M1 of vinylbenzene is 126 tons/hour.To produce the per kilogram styrene product, taking off the required energy consumption of ethylbenzene tower overhead gas phase materials M5 condensation is the 695kw/kg product, and wherein the energy of second stage condenser 7 consumption is the 106kw/kg product.Calculate by this, the heat energy recovery rate that takes off ethylbenzene tower is about 84.7%.
The calculation formula of the rate of recovery is:
Claims (8)
1, a kind of by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, this method may further comprise the steps:
1) material ethylbenzene heating and gasifying in the presence of water;
2) Qi Hua ethylbenzene and water mixture carry out the vapor catalytic dehydrogenation reaction;
3) products of dehydrogenation reactions condensation liquefaction, getting oil phase material after oily water separation is the thick product of vinylbenzene;
4) the thick product of vinylbenzene carries out rectifying by rectifying tower, and cat head is discharged based on the benzene of dehydrogenation reaction by-product and the light constituent impurity of toluene;
5) the tower still material of step 4) carries out rectifying by rectifying tower, discharges unreacted ethylbenzene after the condensation of overhead gas phase materials, and ethylbenzene returns the reuse of dehydrogenation feed system;
6) the tower still material of step 5) carries out rectifying by rectifying tower, and cat head gets the vinylbenzene purified product, and the tower still is discharged the heavy constituent impurity based on tar,
It is characterized in that above-mentioned steps 1) in, described material ethylbenzene and water are heated as heating medium by the overhead gas phase materials of step 5) and to make it gasification, material ethylbenzene and water cool off the overhead gas phase materials of step 5) as heat-eliminating medium and make it condensation simultaneously.
2, according to claim 1 by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, it is characterized in that in the described step 1), by reboiler material ethylbenzene and water are heated, reboiler comprises main reboiler and auxiliary reboiler, both are arranged side by side mutually, the heating medium of main reboiler is the described overhead gas phase materials of step 5), and auxiliary reboiler adopts the heating medium of outer confession.
3, according to claim 1 by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, it is characterized in that overhead gas phase materials in the described step 5) and the material ethylbenzene in the step 1) and water carry out after the heat exchange again through second stage condensation, second stage condenser condensing adopts the heat-eliminating medium of outer confession.
4, according to claim 1,2 or 3 described by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, the quality feed ratio that it is characterized in that described material ethylbenzene of step 1) and water is 1.8～2.2: 1.
5, according to claim 1,2 or 3 described by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, the working pressure that it is characterized in that the described rectifying of step 5) is 20～100KPa absolute pressure.
6, according to claim 5 by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, the working pressure that it is characterized in that the described rectifying of step 5) is 30～50KPa absolute pressure.
7, according to claim 1,2 or 3 described by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, the reflux ratio that it is characterized in that the described rectifying of step 5) is 4～17.
8, according to claim 7 by ethylbenzene gas-phase dehydrogenation preparation of styrene and products thereof purified method, the reflux ratio that it is characterized in that the described rectifying of step 5) is 6～10.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100471955A CN101412653A (en) | 2007-10-18 | 2007-10-18 | Method for preparing phenylethylene by ethylbenzene gas-phase dehydrogenation and refining product of phenylethylene |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100471955A CN101412653A (en) | 2007-10-18 | 2007-10-18 | Method for preparing phenylethylene by ethylbenzene gas-phase dehydrogenation and refining product of phenylethylene |
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| CNA2007100471955A Pending CN101412653A (en) | 2007-10-18 | 2007-10-18 | Method for preparing phenylethylene by ethylbenzene gas-phase dehydrogenation and refining product of phenylethylene |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102836559A (en) * | 2012-08-28 | 2012-12-26 | 南通宝钢钢铁有限公司 | Oil material light constituent separating and storing system |
| CN107454896A (en) * | 2015-03-31 | 2017-12-08 | 德希尼布工艺技术股份有限公司 | The method for preheating dehydrogenation reactor charging |
| CN107540510A (en) * | 2016-06-29 | 2018-01-05 | 中石化上海工程有限公司 | The energy-saving process method of styrene piece-rate system |
| CN113024345A (en) * | 2021-01-15 | 2021-06-25 | 宁波科元精化股份有限公司 | Tower recovery process for improving recovery rate of styrene |
| CN114685237A (en) * | 2022-03-16 | 2022-07-01 | 江苏常青树新材料科技股份有限公司 | Process method for preparing p-methylstyrene by reacting p-methyl-ethylbenzene |
-
2007
- 2007-10-18 CN CNA2007100471955A patent/CN101412653A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102836559A (en) * | 2012-08-28 | 2012-12-26 | 南通宝钢钢铁有限公司 | Oil material light constituent separating and storing system |
| CN102836559B (en) * | 2012-08-28 | 2014-07-30 | 南通宝钢钢铁有限公司 | Oil material light constituent separating device |
| CN107454896A (en) * | 2015-03-31 | 2017-12-08 | 德希尼布工艺技术股份有限公司 | The method for preheating dehydrogenation reactor charging |
| CN107454896B (en) * | 2015-03-31 | 2021-05-04 | 德希尼布工艺技术股份有限公司 | Method for preheating the feed of a dehydrogenation reactor |
| CN107540510A (en) * | 2016-06-29 | 2018-01-05 | 中石化上海工程有限公司 | The energy-saving process method of styrene piece-rate system |
| CN113024345A (en) * | 2021-01-15 | 2021-06-25 | 宁波科元精化股份有限公司 | Tower recovery process for improving recovery rate of styrene |
| CN114685237A (en) * | 2022-03-16 | 2022-07-01 | 江苏常青树新材料科技股份有限公司 | Process method for preparing p-methylstyrene by reacting p-methyl-ethylbenzene |
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Open date: 20090422 |