CN104974035B - Azeotropic distillation is used to process the acetic acid containing dialkyl aromatic hydrocarbons and water method - Google Patents
Azeotropic distillation is used to process the acetic acid containing dialkyl aromatic hydrocarbons and water method Download PDFInfo
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Abstract
The present invention can extract unreacted dialkyl aromatic hydrocarbons in azeotropy rectification column during preparing aromatic carboxylic acid continuously and recycle, and will not break production process set up concentration thus have influence on separating effect, continuous operation can be realized.The method of the invention is simple to operate, low cost, unreacted dialkyl aromatic hydrocarbons will not produce interference again to the rectification characteristic of azeotropy rectification column and the composition of system, so that the dehydration composition as the acetic acid of rectification target can keep stable, and then reduction tower top distillates the content of Organic substance in water.
Description
Technical field
The present invention relates to a kind of acetic acid and method of water reclaiming with azeotropic distillation in aromatic carboxylic acid produces and containing dialkyl aromatic hydrocarbons, particularly in the production process of p-phthalic acid, time in charging containing xylol, use azeotropic distillation purifying acetic acid and the process of water.
Background technology
Traditional aromatic carboxylic acid's production process, generally uses the liquid phase air oxidation adding pressure alkylaromatic hydrocarbon to obtain.Alkylaromatic hydrocarbon liquid phase oxidation is in the presence of acetate solvate and metal catalyst system, and the alkyl on aromatic hydrocarbons progressively aoxidizes generation aldehyde and carboxylic acid, finally gives aromatic carboxylic acid.
The oxidizing process of alkylaromatic hydrocarbon will generate water, simultaneously with substantial amounts of heat, in order to keep stablizing of water content in course of reaction temperature and reactor, generally use solvent evaporation mode to be removed by heat.The acetic acid of removal and water mixed vapour, condensed by condenser, there is the form of low-pressure steam, removal heat of reaction, then major part condensed fluid is back in reactor, and partial condensation liquid enters into solvent dehydration system, carry out the separation of acetic acid and water, by the acetic acid cycling and reutilization of isolated, a part of water is used as system dispensing or cleaning mixture, and major part enters water treatment system with sewage form.
Acetic acid separates common rectificating method, azeotropic distillation method and the liquid-liquid extraction method that generally use with water.Owing to acetic acid and water boiling point are closer to, when in acetic acid aqueous mixtures, acetic acid content is the lowest, both sharply increase by separating difficulty.Therefore, when low acetic acid content in separation requirement water, it has been recognized that heterogeneous azeotropic rectification distillation technology is a kind of more energy efficient, separation method that running cost is low.
Patent US2050234, GB298137, GB1576787 have invented separation acetic acid and the azeotropic distillation method of water, but have not accounted for the trace alkylbenzene impact on piece-rate system in aromatic carboxylic acid's production process.CN200810185619.9 has invented the azeotropic distillation method with n-butyl acetate as entrainer, simultaneously take account of production aromatic carboxylic acid's process, the alkylbenzene having trace enters into azeotropic distillation system, unreacted alkylbenzene forms azeotropic mixture due to entrainer or the acetic acid water that can and generally use, in azeotropy rectification column, stable separation can be produced impact, in order to reduce the alkylbenzene impact on lock out operation, and make alkylbenzene in azeotropy rectification column be reused, propose in azeotropic district, use interval or extract one material in batches out, by to the condensation of material and standing, separation and Extraction dialkyl benzene, and the standing liquid of the trace dialkyl benzene contained, again return to extract out near the position of material.Maximize to ensure to extract out the concentration of dialkyl benzene in material, the patent proposes the concentration ratio operating optimal temperature range and optimal dialkyl benzene with entrainer.The present invention is although it is contemplated that the impact of dialkyl benzene, but owing to aromatic carboxylic acid's production is the process of a serialization, use interval or the method in batches extracting dialkyl benzene, not only operate poor repeatability, labor intensity is big, also the concentration problems of on-line analysis dialkyl benzene can be related to, the delayed optimum efficiency that can affect this operation of concentration analysis.The fluctuation of azeotropy rectification column temperature all by time and the extraction amount of impact extraction material, increases the difficulty of operation.
CN95194732.X with reduce azeotropy rectification column number of theoretical plate as target, invented in the acetic acid with isobutyl acetate or n-propyl acetate as entrainer and the azeotropic distillation technique of water.During aoxidizing aromatic carboxylic acid processed, unconverted dialkyl benzene enters the impact after azeotropy rectification column on stable separation, patent uses on the lower position higher than azeotropic district, it is introduced into stream, control penetrating of entrainer, from tower, extract one material containing high concentration dialkyl benzene out in this region, for eliminating the impact of dialkyl benzene simultaneously.But, separate with entrainer for how the dialkyl benzene in stock being flowed in extraction, recycle, do not propose suitable method.
Above-mentioned patent consider unconverted dialkyl benzene azeotropy rectification column is stably separated when affecting, the most only determine the position (near the lower limit in azeotropic region) of extraction dialkyl benzene, aspect is utilized the material extracted is carried out separation, propose and first material is cooled down, then standing separation is carried out, and use on-line analysis, interval or the method for batch operation.Owing in actual production process, this region belongs to vapour, liquid composition change the most significantly stage, interval or batch operation will cause steam inside amount, the minor variations of amount of liquid material, the concentration balance making production process set up all is broken by these, eventually affect separating effect, therefore, be not suitable for serialization rectification and produce, simultaneously, also due to increase condenser and online analytical instrument, increasing cost of investment, operation easier is the biggest simultaneously.
Summary of the invention
For above-mentioned situation, the present invention is directed to the acetic acid containing dialkyl aromatic hydrocarbons and water, material composition and azeotropic distillation column overhead composition is extracted out by analyzing, extraction feed separation and utilization are studied, it was found that use following method to be possible not only to add condenser, reduce extract temperature, the separation of dialkyl aromatic hydrocarbons and other component can also be realized, it is achieved continuous operation；Enter azeotropic distillation column overhead by other component after making separation, control the stable operation of process the most further, also make these materials be separated further, utilize.
The inventive method provides a kind of and uses azeotropic distillation to process the acetic acid containing dialkyl aromatic hydrocarbons and water method, the present invention uses the method for azeotropic distillation method and the dialkyl aromatic hydrocarbons stream stock combination of enrichment, less than azeotropic district lower limit dialkyl aromatic hydrocarbons richness, the stream stock containing dialkyl benzene is amassed region in azeotropy rectification column tower extract out, aqueous phase mixing in the material containing high concentration dialkyl aromatic hydrocarbons extracted out from tower and two grades of decanters, oil phase after decant enters common rectifying tower separation dialkyl aromatic hydrocarbons and entrainer, entrainer is directly entered one-level decanter, recycle, and dialkyl aromatic hydrocarbons enters follow-up oxidation system and aoxidizes further.
The concrete technical scheme of the present invention is as follows:
A kind of acetic acid and the water method that use azeotropic distillation process to contain dialkyl aromatic hydrocarbons, comprise the steps:
(1) in aromatic carboxylic acid's production process, the material of the acetic acid containing dialkyl aromatic hydrocarbons and water being carried out azeotropic distillation and separated entering azeotropy rectification column higher than the position of azeotropic district lower limit, the entrainer that azeotropy rectification column uses is alkyl acetate；Azeotropy rectification column tower bottom liquid body material forms upflowing vapor by reboiler heating vaporization, and this steam contacts step by step at the material of Ta Nei with azeotropic rectifying tower top together with the material of the acetic acid containing dialkyl aromatic hydrocarbons and water, and carry out conducting heat, mass transfer；The acetate solvate being substantially free of entrainer can be produced at the bottom of azeotropy rectification column tower；
(2) after the steam condensation that azeotropic distillation column overhead flows out, one-level decanter is entered in liquid form, it is layered in one-level decanter, the oil phase on upper strata is back to azeotropic distillation column overhead together with supplementing stream stock with entrainer, the aqueous phase of lower floor is in addition to part flow to two grades of decanters, and remaining enters follow-up piece-rate system and separates；It flow to the quality of aqueous phase in two grades of decanters and account for the 10%-40% of aqueous phase gross mass；
(3) in azeotropy rectification column, amass region less than azeotropic district lower limit dialkyl aromatic hydrocarbons richness and extract a plume stock out, this stream stock mixes with the aqueous phase exited in two grades of decanters from one-level decanter, stratification again in two grades of decanters, in two grades of decanters, the oil phase on upper strata flow to common rectifying tower and separates further, and in two grades of decanters, the aqueous-phase reflux of lower floor is to azeotropic distillation column overhead；
(4) material flowed out from conventional distillation column overhead returns in one-level decanter, and the dialkyl aromatic hydrocarbons at the bottom of common rectifying tower tower enters follow-up oxidation system and carries out post processing.
Amassing region less than azeotropic district lower limit dialkyl aromatic hydrocarbons richness described in step (3) is that temperature is the region of 95 DEG C-110 DEG C in azeotropy rectification column, and in this region, the quality of dialkyl aromatic hydrocarbons accounts for the 5%-50% of liquid phase gross mass, preferably 20%--50%.
In azeotropy rectification column, amass region less than azeotropic district lower limit dialkyl aromatic hydrocarbons richness described in step (3) to extract a plume stock out and account for and enter the 50%-150%, preferably 60%-110% of dialkyl aromatic hydrocarbons gross mass azeotropy rectification column material；Extraction stream stock is selected in above-mentioned scope be to try to ensure that the dialkyl aromatic hydrocarbons accumulation total amount in azeotropy rectification column will not increase because stream stock enters the increase of the dialkyl aromatic hydrocarbons amount brought into.
In step (3), the temperature exiting into the aqueous phase in two grades of decanters from one-level decanter is 20 DEG C-80 DEG C, preferably 45 DEG C--60 DEG C；Above-mentioned aqueous phase temperature range advantageously reduces temperature of liquid in two grades of decanters, so that the layering of liquid liquid is more thorough.
In step (1), in acetic acid containing dialkyl aromatic hydrocarbons and the material of water, the quality of water accounts for the 15-50% of material gross mass；Water in above-mentioned scope makes whole process costs relatively low, economic and practical；If the content of water increases further, the economy using azeotropic distillation separating-purifying acetic acid would not be fairly obvious.
The one in n-propyl acetate, n-butyl acetate, isobutyl acetate, sec-Butyl Acetate of the alkyl acetate described in step (1).
Described in step (1), aromatic carboxylic acid is p-phthalic acid or M-phthalic acid.
Described in step (1), dialkyl aromatic hydrocarbons is xylol or meta-xylene.
The material of acetic acid containing dialkyl aromatic hydrocarbons of the present invention and water refers in aromatic carboxylic acid's production process, after using acetic acid and aqueous solvent, is evaporated by gas or the form of solid-liquor separation obtains rich in acetate solvate, and wherein acetic acid quality content is at 85-50%.The feed stream stock containing the acetic acid of dialkyl aromatic hydrocarbons and the material of water in the present invention can be one, it is also possible to is multiply.
According to the present invention, unreacted dialkyl aromatic hydrocarbons in azeotropy rectification column can be extracted during preparing aromatic carboxylic acid continuously and recycle, and will not break production process set up concentration thus have influence on separating effect, continuous operation can be realized.The method of the invention is simple to operate, low cost, unreacted dialkyl aromatic hydrocarbons will not produce interference again to the rectification characteristic of azeotropy rectification column and the composition of system, so that the dehydration composition as the acetic acid of rectification target can keep stable, and then reduction tower top distillates the content of Organic substance in water.
Accompanying drawing explanation
Fig. 1 is the material charging of the acetic acid containing 100ppm xylol and water, and the dynamic analog different time sections xylol after driving is along the concentration profile of azeotropy rectification column；
Fig. 2 is the material charging of the acetic acid containing 100ppm xylol and water, and the dynamic analog different time sections after driving is along the temperature profile of azeotropy rectification column；
Fig. 3 is that employing azeotropic distillation of the present invention processes the acetic acid containing dialkyl aromatic hydrocarbons and the flow chart of water.
Detailed description of the invention
The quality of " dialkyl aromatic hydrocarbons " of the present invention uses existing gas chromatography (external standard method) to measure.
The piece-rate system utilizing accompanying drawing that the present invention uses azeotropic distillation process the acetic acid containing dialkyl aromatic hydrocarbons and water illustrates.
Fig. 1 and Fig. 2 is that employing azeotropic distillation of the present invention processes in the acetic acid containing dialkyl aromatic hydrocarbons and water method, the entrainer used in azeotropic distillation is sec-Butyl Acetate, when in charging containing xylol, use the result that the multicomponent rectification of existing dynamic analog calcutation calculates.Fig. 1 reflect driving after different time sections xylol along azeotropy rectification column column plate concentration profile, Fig. 2 is different time azeotropy rectification column column plate variations in temperature scattergram.As can be seen from Figure 1, when in charging containing xylol (molar fraction of xylol is 0.010 in simulation), count from starting charging, xylol starts constantly to accumulate at the 8th and the 9th piece of tray location, migration over time, xylol concentration on this position is gradually increased, and then the system that affects separates and composition concentration distribution.Fig. 2 reflects corresponding different time, the temperature variations in tower.Along with xylol accumulation in azeotropy rectification column, the concentration of component distribution in tower changes, and Temperature Distribution change is more and more obvious, separates more and more unstable, have impact on the separating effect of azeotropic distillation top of tower and bottom in reflecting whole tower.
Fig. 3 is that the present invention uses azeotropic distillation to process containing the acetic acid of unreacted xylol, the flow chart of water.In the azeotropic distillation separation acetic acid of the present invention, water method, acetic acid and the material of water containing dialkyl aromatic hydrocarbons are respectively from and produce p-phthalic acid oxidation reactor top condensed fluid extraction section, crystallizer overhead vapor etc..Owing in material pending in different phase, water content is different, therefore, although the most only illustrate a feed stream stock 1, but can have other aqueous feed stream stock, as fed from crystallizer overhead vapor, the washing material etc. of high pressure absorber.They enter in tower along other position of azeotropy rectification column.And main feed stream stock comes automatic oxidation reaction cooler Extract and high pressure absorber, this burst of charging contains xylol and the water of high level.
After the steam stream stock 3 at azeotropy rectification column A top is condensed by condenser B, entering in one-level decanter (phase separator) C1, condensed fluid stands in this place, is again layered, and upper strata is organic facies, and lower floor is aqueous phase.Organic facies includes entrainer, methyl acetate, xylol and other organic compound, and containing water and a small amount of entrainer, methyl acetate in aqueous phase.Organic phase fluid stock 4b in one-level decanter and entrainer supplement stream stock 4a and form stream stock 5b, are back to azeotropy rectification column A tower top；Its aqueous phase stream stock has sub-fraction to pass through to flow stock 9 to enter in two grades of decanter C2, and major part is entered follow-up piece-rate system separated by stream stock 8, and the quality of stream stock 9 accounts for the 10%-40% of aqueous phase gross mass.
In azeotropy rectification column, amass region (in azeotropy rectification column, temperature is the region of 95 DEG C-110 DEG C) less than azeotropic district lower limit xylol richness extract a plume stock 6 out, the extracted amount of this stream stock accounts for and enters the 50%-150%, preferably 60%-110% of dialkyl aromatic hydrocarbons gross mass in azeotropy rectification column material.If it was found that one aqueous phase stream stock of addition is mixed, both can reduce temperature, and can reach again to separate purpose.Then, being mixed with stream stock 6 by the aqueous phase stream stock 9 exited into from one-level decanter in two grades of decanters, stratification again in two grades of decanter C2, the temperature of aqueous phase stream stock 9 is 20 DEG C-80 DEG C, preferably 45 DEG C--60 DEG C；By profit layering, the xylol in oil phase, entrainer are separated with methyl acetate.In two grades of decanter C2, the aqueous phase of lower floor is back to azeotropy rectification column A tower top by stream stock 5a, in two grades of decanter C2, the oil phase stream stock 7 on upper strata flow to common rectifying tower D and separates further, xylol is separated from entrainer and methyl acetate, xylol stream stock 11 at the bottom of common rectifying tower D tower enters follow-up oxidation system to carry out recycling after post processing, this makes it possible to ensure stablizing of the concentration in azeotropy rectification column tower and Temperature Distribution.Common rectifying tower D top separates in returning to one-level decanter C1 rich in the material stream 10 of entrainer and methyl acetate, forms oil phase and be back to azeotropy rectification column A tower top and utilize after layering.Xylol long-pending for richness can be extracted out by the present invention continuously, and makes in the xylol of extraction nearly 80% to obtain separation to reoxidize utilization, improve the yield of production process.
Hereinafter, the simulated conditions in the azeotropy rectification column of the present invention are illustrated in conjunction with the embodiments.The azeotropic distillation simulation of the present invention uses the actual p xylene oxidation of factory to produce the condition of p-phthalic acid, the feed entrance point of the azeotropy rectification column with sec-Butyl Acetate as entrainer enters the acetum of different moisture content, wherein contains trace xylol and methyl acetate.The parameter such as following table of component formation azeotropic mixture in this simulation:
| Bi-component | Azeotropic point | Composition |
| Water xylol | 92℃ | 45.1wt% |
| Water--sec-Butyl Acetate | 86.58℃ | 19.22 wt% |
| Water acetic acid methyl ester | 56.5℃ | 3.5wt% |
| Acetic acid xylol | 115℃ | 72.0wt% |
Embodiment
1
One acetic acid containing xylol and the feed stream stock 1 of water, enter azeotropy rectification column A with the flow of 5075.71kg/h from the 14th block of column plate, and in feed stream stock 1, acetate concentration is 54.6wt%, and xylol flow is 13.6kg/h, and azeotropy rectification column is 45 blocks of column plates.Meanwhile, extracting a plume stock 6 continuously out in long-pending the 10th piece of tray location side of (azeotropic region) lower limit of azeotropy rectification column xylol richness, its extracted amount is close to the flow of xylol, i.e. 15.92kg/h in feed stream stock 1.According to Fig. 2 Temperature Distribution it can be seen that temperature is at about 96.3 DEG C at this, in stream stock 6 corresponding component be respectively the concentration of xylol be 47.5wt%, sec-Butyl Acetate concentration 19.1wt%, water concentration 19.6wt%, acetate concentration 12wt% and methyl acetate 1.8wt%.The present invention is by stream stock 6 and exits into aqueous phase stream stock 9(aqueous phase stream stock 9 temperature 58.7 DEG C in two grades of decanters, flow 528kg/h from one-level decanter) hybrid cooling in two grades of decanter C2, control temperature is at 53 DEG C, and layering forms organic facies and aqueous phase again.Wherein the organic facies in two grades of decanter C2 enters common rectifying tower D with 210kg/h flow by stream stock 7.The component of stream stock 7 consists of para-xylene concentration 36wt%, sec-Butyl Acetate concentration 20.5wt%, methyl acetate concentration 41.2wt%, and remaining is acetic acid and water.Through the separation of common rectifying tower D, xylol stream stock 11 at the bottom of tower can obtain the xylol of purity 99.0wt% with 43kg/h flow, and xylol can enter follow-up oxidation system and aoxidize utilization further.
Common rectifying tower D headpiece stream stock 10 separates in returning to one-level decanter, and again forms oil phase after layering and be back to azeotropy rectification column A tower top and utilize.Xylol long-pending for richness can be extracted out by the present invention continuously, and makes nearly 70% the obtaining separation and reoxidize utilization of xylol of extraction, improves the yield of production process.
Embodiment
2
One acetic acid containing xylol and the feed stream stock 1 of water, azeotropy rectification column A is entered from the 22nd block of column plate with the flow of 5075.71kg/h, in feed stream stock 1, acetate concentration is 74.6wt%, and xylol flow is 13.6kg/h, and azeotropy rectification column rectifying column is 45 blocks of column plates.Meanwhile, extracting a plume stock 6 continuously out in long-pending the 18th piece of tray location side of (azeotropic region) lower limit of azeotropy rectification column xylol richness, its extracted amount is close to the flow of xylol, i.e. 14.62kg/h in feed stream stock 1.According to Fig. 2 Temperature Distribution it can be seen that temperature is at about 98.6 DEG C at this, in stream stock 6, corresponding component is concentration 40.5wt% of xylol respectively, sec-Butyl Acetate concentration 23.1wt%, water concentration 21.6wt%, acetate concentration 12.5wt% and methyl acetate 2.3wt%.The present invention is by stream stock 6 and exits into aqueous phase stream stock 9(aqueous phase stream stock 9 temperature 50 C in two grades of decanters, flow 500kg/h from one-level decanter) hybrid cooling in two grades of decanter C2, control temperature is at 58 DEG C, and layering forms organic facies and aqueous phase again.Wherein the organic facies in two grades of decanter C2 enters common rectifying tower D with 22.06kg/h flow by stream stock 7.The component of stream stock 7 consists of para-xylene concentration 34wt%, sec-Butyl Acetate concentration 21.2wt%, methyl acetate concentration 43.1wt%, and remaining is acetic acid and water.Through the separation of common rectifying tower D, xylol stream stock 11 at the bottom of tower can obtain the xylol of purity 99.0wt% with 46kg/h flow, and xylol can enter follow-up oxidation system and aoxidize utilization further.
Common rectifying tower D headpiece stream stock 10 separates in returning to one-level decanter, and again forms oil phase after layering and be back to azeotropy rectification column A tower top and utilize.Xylol long-pending for richness can be extracted out by the present invention continuously, and makes nearly 80% the obtaining separation and reoxidize utilization of xylol of extraction, improves the yield of production process.
Claims (7)
1. one kind uses azeotropic distillation to process the acetic acid containing dialkyl aromatic hydrocarbons and water method, it is characterised in that comprise the steps:
1) in aromatic carboxylic acid's production process, the material of the acetic acid containing dialkyl aromatic hydrocarbons and water being carried out azeotropic distillation and separated entering azeotropy rectification column higher than the position of azeotropic district lower limit, the entrainer that azeotropy rectification column uses is alkyl acetate；Azeotropy rectification column tower bottom liquid body material forms upflowing vapor by reboiler heating vaporization, and this steam contacts step by step at the material of Ta Nei with azeotropic rectifying tower top together with the material of the acetic acid containing dialkyl aromatic hydrocarbons and water, and carry out conducting heat, mass transfer；The acetate solvate being substantially free of entrainer can be produced at the bottom of azeotropy rectification column tower；
2) after the steam condensation that azeotropic distillation column overhead flows out, one-level decanter is entered in liquid form, it is layered in one-level decanter, the oil phase on upper strata is back to azeotropic distillation column overhead together with supplementing stream stock with entrainer, the aqueous phase of lower floor is in addition to part flow to two grades of decanters, and remaining enters follow-up piece-rate system and separates；It flow to the quality of aqueous phase in two grades of decanters and account for the 10%-40% of aqueous phase gross mass；
3) in azeotropy rectification column, amass region less than azeotropic district lower limit dialkyl aromatic hydrocarbons richness and extract a plume stock out, this stream stock mixes with the aqueous phase exited in two grades of decanters from one-level decanter, stratification again in two grades of decanters, in two grades of decanters, the oil phase on upper strata flow to common rectifying tower and separates further, and in two grades of decanters, the aqueous-phase reflux of lower floor is to azeotropic distillation column overhead；
4) material flowed out from conventional distillation column overhead returns in one-level decanter, and the dialkyl aromatic hydrocarbons at the bottom of common rectifying tower tower enters follow-up oxidation system and carries out post processing；
Described in step (1), alkyl acetate is sec-Butyl Acetate.
Method the most according to claim 1, it is characterized in that amassing region less than azeotropic district lower limit dialkyl aromatic hydrocarbons richness described in step (3) is that temperature is the region of 95 DEG C-110 DEG C in azeotropy rectification column, in this region, the quality of dialkyl aromatic hydrocarbons accounts for the 5%-50% of liquid phase gross mass.
Method the most according to claim 2, it is characterised in that amass region lower limit less than azeotropic district dialkyl aromatic hydrocarbons richness in azeotropy rectification column described in step (3) and extract a plume stock out and account for and enter the 50%-150% of dialkyl aromatic hydrocarbons gross mass azeotropy rectification column material.
Method the most according to claim 3, it is characterised in that in step (3), the temperature exiting into the aqueous phase in two grades of decanters from one-level decanter is 20 DEG C-80 DEG C.
In method the most according to claim 4, it is characterised in that in step (1), acetic acid containing dialkyl aromatic hydrocarbons and the material of water, the quality of water accounts for the 15-50% of material gross mass.
Method the most according to claim 1, it is characterised in that described in step (1), aromatic carboxylic acid is p-phthalic acid or M-phthalic acid.
Method the most according to claim 1, it is characterised in that described in step (1), dialkyl aromatic hydrocarbons is xylol or meta-xylene.
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|---|---|---|---|---|
| CN1161686A (en) * | 1994-08-23 | 1997-10-08 | 帝国化学工业公司 | Dehydration of acetic acid by azeotropic distillation in the prodn. of aromatic acid |
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| CN101986320A (en) * | 2010-08-23 | 2011-03-16 | 华东理工大学 | Modeling method for heterogeneous azeotropic rectification solvent dehydrating tower of industrial purified terephthalic acid (PTA) device |
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| CN1161686A (en) * | 1994-08-23 | 1997-10-08 | 帝国化学工业公司 | Dehydration of acetic acid by azeotropic distillation in the prodn. of aromatic acid |
| CN1696098A (en) * | 2005-03-25 | 2005-11-16 | 扬子石油化工股份有限公司 | Method for recovering raw material, solvent and by-product generated in procedure of producing aromatic carboxylic acid |
| CN101986320A (en) * | 2010-08-23 | 2011-03-16 | 华东理工大学 | Modeling method for heterogeneous azeotropic rectification solvent dehydrating tower of industrial purified terephthalic acid (PTA) device |
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