• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to the production of phthalic acid esters, in particular the preparation of dimethyl terephthalate used for the polymerization and the manufacture of polymeric materials. Synthesis is carried out by liquid-phase oxidation of a mixture of p-xylene and a fraction containing p-toluic acid methyl ester, with air at a temperature of 140-170 ° C and a pressure of 4-8 bar in the presence of dissolved heavy metal compounds. The esterification of the product obtained is then carried out with methanol, which becomes a liquid product by increasing the pressure, and then it is evaporated. Esterification proceeds at a temperature of 220–280 ° C and a pressure of 20–25 bar. To reduce energy consumption, the product is esterified with methanol-containing steam, brought to a compression ratio @ (1.25 - 15): 1 with a pressure of 25 - 30 bar and evaporated at 180 - 300 ° C It is obtained by evaporation of the filtrate of recrystallization of crude dimethyl terephthalate or by distillation of methanol-containing secondary steam under a pressure of 2-20 bar. The methanol-containing vapor released during compression is used to superheat this vapor to the esterification temperature. The resulting crude ester fraction and the methanol-containing secondary vapor fraction are withdrawn from the esterification stage and separated by distillation to isolate the p-toluic acid methyl ester fraction (which is recycled for oxidation), the crude dimethyl terephthalate fraction (which is then recrystallized from methanol) and the residue. The secondary vapors removed from the esterification stage should be washed with an aqueous phase followed by depressurization to 0.1–8 bar in the turbo-expander and recycling them to the process.
    公开号:SU1545938A3
    申请号:SU853856864
    申请日:1985-02-18
    公开日:1990-02-23
    发明作者:Модик Рудольф；Поршен Ерг；Шенген Антон；Виргес Ральф
    申请人:Динамит Нобель Аг (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to an improved process for the preparation of dimethyl terephthalate.
    The aim of the invention is to reduce energy costs.
    one
    FIG. 1 shows a flow chart of the process for the production of dimethyl terephthalate; in fig. 2-4 - a device used in the implementation process in examples 1-9.

    cm
    According to the technological scheme (fig. 1) nl, the oxidation of T, carried out at 140-170 ° C and a pressure of 4-8 ba, is fed through pipelines 1-4 p-xychol, recirculating methyl ester of n-toluic acid, air and cobalt - manganese catalyst, respectively.
    Oxidation stages I are discharged through pipelines 5-7 to off-gas, off-water, and oxidation product, respectively.
    The oxidation product is fed to etherification of TT with methanol at a temperature of 180-300 ° C and a pressure of 25-30 bar supplied through pipelines 8 and 9. From the esterification stage, the sterification product is withdrawn through pipe 10 to discharge stage III. as well as methanol-containing secondary steam, which is also fed through pipe 11 to pressure release stage I.
    At the IIT stage, a methanol-containing fraction is supplied via pipeline I2 to the rectification IV carried out under a pressure of 2-20 bar, where pipeline 13 also supplies the liquid phase obtained in stage V of oxidation exhaust gas I condensation, the secondary fraction fed through the pipeline 14 in the collection of 15 complex methyl ester of n-toluic acid, where the pipelines 16 and 17 also served containing the specified ester fraction obtained in stage VI distillation of the filtrate and rectification IV, as well as the main fraction of the crude ether, we submit via pipeline 18 to distillation VII, where the fraction is divided into the phase containing the specified ester, part of which is fed via pipeline 19 to collector 15, and the remainder via pipeline 20 to the filtrate collector 21, and to the raw dimethyl terephthalate fraction supplied 22 for VTTT distillation, where the fraction is divided into a target product fed through line 23 to purification IX by recrystallization from fresh methanol fed through line 24 to the methanol-containing phase fed through line 25 from rectification IV, and methanol containing phase supplied through the pipeline 26 of the collection0
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    n) 27, in which the pipeline
    28 submit methanol obtained at stage VT distillation of the filtrate, and the residue supplied through the pipeline
    29 into stage X of the treatment with methanol supplied via conduit 30, where a fraction containing g-toluic acid methyl ester is supplied, the fraction supplied via conduit 31 to collection 15, the methanol-containing fraction supplied via conduit 32 to rectification IV, and the residue withdrawn from the process via conduit 33. Purified target product is withdrawn through conduit 34, and recrystallization filtrate IX is fed via conduit 35 to collector 21, from which methanol-containing phase is conveyed through conduit 36
    device 37 (Fig. 2-4).
    In device 37, a condensed methanol-containing filtrate is obtained, which is fed through conduit 38 to a distillation VT, where it is separated into a methanol-containing fraction withdrawn from conduit 28 containing p-toluic acid methyl ester fraction withdrawn through conduit 16 and the residue withdrawn from the process through the pipeline 39. The off-gases of the V concentration are withdrawn through the pipeline 40, and the residual fraction obtained on rectification IV is withdrawn through the pipeline 41.
    The process in the device 37 is carried out as follows (Fig. 2).
    The methanol-containing filtrate is supplied through conduit 36 to collector 42, from which the filtrate is withdrawn through conduit 43 by means of a pump 44 and fed to a circulating conduit 45, in which an evaporator 46 is heated, heated by low-pressure steam produced during the process, and separation tank 48, from which part of methanol in the form of steam is removed through conduit 30 and, after overheating, is fed to stage X of processing the residue of distillation of crude dimethylterephthalate, and the residue of steam methanol is withdrawn through conduit 49 and fed to the compressor 50, in which methanol in a ratio of 1, .5: 1-15: 1 is compressed to 25-30 bar, with simultaneous overheating to 180-300 ° C. Methanol is then supplied to pipeline 9.
    on the esterification of TT. The bottom product of vessel 48 is withdrawn through conduit 38 and is fed to distillation VI. The excess filtrate fed through conduit 36 through the collector 42 is withdrawn through conduit 51.
    In the device 37 of FIG. 3, the secondary vapors of the IT esterification column 52, discharged through line 11, are subjected to the following pre-treatment before being fed to step TI7.
    They are washed in the apparatus 53 with hot water supplied through conduit 54 or with a condenser of a reflux condenser 55 fed through conduit 56. Purified secondary steam coming out of the upper part of the apparatus 53 is fed directly through heater 57 through a heater 58 to a turbine detander 59, where secondary vapors are reduced, for example, to 0.1-8 bar, after which they are fed to stage III, the stream containing the by-product obtained in apparatus 53 is recycled through conduit 60 via pump 61.
    In the device 37 of FIG. 4, methanol in the form of steam discharged through conduit 49 is fed to condenser 62 operating on cooling water supplied via conduit 63 by means of a pump 64. The resulting liquid methanol is fed to reservoir 65, from which methanol, required at stage X for treating the residue of distillation of dimethyl terephthalate, is methanol taken through line 66, when pump help 67 is adjusted to slightly increased pressure, e.g. 3 bar, and through line 68 and fed into circulation pipe 69, in which the evaporator 70 is placed, heated by the steam produced low pressure rum; and separation tank 71, from which methanol vapor is removed through conduit 30 and, after overheating, is fed to stage X.
    Methanol required for esterification II in column 52 is taken through conduit 72, brought to esterification pressure using a pump 73, heated in a low-pressure heated steam from an apparatus (heater) 74, and fed to a circulation conduit 75, in which an evaporator 76 is placed heated by high pressure steam, and
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    separation tank 77, from which pipe 78 removes methanol vapor, the latter is brought to an esterification temperature in an apparatus (heater) 79 heated with high-temperature oil before being fed to the esterification.
    Example 1 (Fig. 1 and 2). A mixture of 17825 kg / h of n-xnolol and 50105 kg / h of mixture, wt%: methyl p-toluic acid methyl ester (MEPTA) 67.1; dimethyl ortho phthalate (DMO), dimethyl isophthalate (DMI) and dimethyl terephthalate (DMT.) 19; benzoic acid methyl ester (MEBK) 8.3; terephthalaldehyde acid methyl ester (METAC) 2.8; p-Toluic acid (PTC) 0.7 and unidentified by-products (NLP) 1.8, oxidize 96612 kg / h of air in the presence of 333 kg / h of a catalyst based on cobalt and manganese (10: 1) in the form of acetates dissolved in water. The oxidation is carried out in a cascade of three reactors at a temperature increasing from 140 to 170 ° C and a pressure increasing from 4 to 8 bar. 74925 kg / h of oxidation product are obtained, wt.%: MEPTK 24; PTK 18.4; monomethyl terephthalate (MMT) 21.4; DME, DMI and DMT 12.7; terephthalic acid (TFA) 13; MEBK 5.5; high boiling components (VK) 2.8; METAK 1.8 and NPP 0.4, which is subjected to esterification of 35549.1 kg / h of methanol obtained in the process at a pressure of 25 bar. In addition, 89950 kg / h of exhaust gases are removed from the oxidation stage, from which 37089 kg / h of the aqueous phase are separated by condensation, wt%: 92.3; methanol 3.1; MEPTK 0.4 and NPP 4.2, supplied to the separation of methanol from it by rectification. As a result of esterification, 83420 kg / h of esterification product are obtained, wt%: DME, DMI and DMT 44.5; MEPTK 37,4; H, 0 7; MEBK - 4.6; VK 2.5; METAK 1.6, MMT 0.8; PTC 0.4; TPA 0.2 and NPP 1, which is fed to the depressurization stage, and 28180 kg / h of the methanol-containing fraction of the composition, wt.%: Methanol 67.8; H70 20.7; MEPTK 5.8; DME, DMI and DMT 1,3; OIEBK 1.1 and NPP 3.3, which is also fed to the depressurization stage, from the latter, 63969 kg / h under a pressure of 1.1 bar were discharged and having a temperature of 190 ° D, composition fraction, wt.%: DME, DMI and DMT 53.5; MEPTK 35; MEBK 3.6; VK 3.3; MMT I; METAK 2; PTC 0.5; TPA 0.2 and NPP 0.9 supplied to the MEPTA distillation unit, 1498 kg / h, having a temperature of 185 ° C, pressure of 1.1 bar and containing MEPTA fraction of composition, wt%: MEPTA -65.2; DME, DMI and DMT 21.8; MEBK 10.4; MMT 0.2 $ METAK 0.8; PTC 0.2 and NPP 1.6, recycled for oxidation, and 32650 kg / h, having a temperature of 80 ° C and a pressure of 1.1 bar, of the methanol-containing fraction of the composition, wt%: methanol 74.9; 18.5; MEBK 0.9; MEPTK 2; DME, DMI and DMT 0.1 and NPP 3.6, fed to the separation from it by rectification of MEPTK, recycled to oxidation, and from methanol, are supplied in the amount of 33838 kg / h to clear the target product by recrystallization.
    From the separation stage by distillation of the f-IPPC, 37086 kg / h of the fraction of the crude ether having the temperature of 235 ° C, wt.%: DME, DMI, DMT 89.7; VK 5.6; METAK 1.8; PC 1.7; PTC 0.7; TFA 0.4 and NPP 0.1, fed to the distillation, 21740 kg / h with a temperature of 130 ° C fraction MEPTK composition, wt.%: MEPTK 82.9; MEBK 8.5; DME, DMI and DMT 3,5; METAK 2.2; PTC 0.2 and NPP 2.7, recycled for oxidation, and 5143 kg / h with a temperature of 130 ° C fraction MEPTK composition, wt.%: MEPTK 85; OIE 8.7; DME, DMI and DMT 3,5; METAK 2.2; PTC 0.2 and NPP 0.4 combined with 77407 kg / h of the filtrate of the recrystallization stage of the target product, having the composition, wt%: methanol 90.9; DME, DMI and DMT 4.8; METAK 0.9, NgO 0.5; PTK 0.3; MMT 0.2 and NPP 2.4. As a result of the distillation, the fraction of the crude ether of the indicated composition gives 3,086 kg / h having a temperature of 160 ° C and a pressure of 1.1 bar of the target product composition, wt%: DME, DMI and DMT 96.9; METAK 2; PTC 0.7 and MMT 0.4, fed to the purification by recrystallization from methanol, fed to the recrystallization in the form of 10427 kg / h of fresh methanol and 62177 kg / h of recycled methanol composition, wt.%: Methanol 96.6; H: 0 0.4 and NPP 3, and 3000 kg / n having a temperature of 140 ° C and a pressure of 3 bar residual fraction composition
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    methanol-methanol
    WA, wt.%: VK 68.3; 17; DME, DMI and DMT 10; TPA 4 and NPP 0.7, applied for treatment of 9000 kg / h of the methanol fraction obtained in the process, wt%: methanol 96.9, Н.20 0.46 and NPP 2.64, having a temperature of 95 ° С and pressure 3 bar. As a result of the treatment, 2727 kg / h are obtained having a temperature of 140 ° C and a pressure of 1.1 bar of the composition fraction, wt%: DME, DMI and DMT 69; MEPTK 29.5 and NPP 1.5, recycled for oxidation, 8691 kg / h, having a temperature of 60 C fraction of the composition, May, 95.4; And, 0 1.9 and the RPE 2.7, recycled to the rectification, and 582 kg / h of the residue that is removed from the process. From the recrystallization stage, 29,223 kg / h of DMT with a purity level of 99.99% was recovered.
    The stream consisting of 77407 kg / h of recrystallization filtrate of the target product and 5143 kg / h of the MEPTA fraction removed from the MEPTA distillation stage is brought to a pressure of 6 bar and evaporated at 120 ° C. As a result of the evaporation, 9000 kg / h of the methanol vapor fraction of the specified composition, obtained for treating the residue of the crude DMT distillation, 40550 kg / h of the condensed methanol fraction of the composition, wt.%: Methanol 73.2; MEPTK 10,8; DME, DMI and DMT 9.7; METAK 2; MEBK 1.1; PTC 0.7; 0.5, MMT 0.3 and NPP 1.7 fed to distillation, and 33,000 kg / h by steam of the methanol fraction of the composition, wt.%: Methanol 96.9; H., 0 0.46, and NPP 2.64, which is adjusted to a pressure of 28 bar by compression and a ratio of 4.67: 1 and fed to a stage of esterification with a temperature of 250 ° C.
    I
    In the distillation of the condensed methanol fraction get 30544 kg / h having a temperature of 60 ° C methanol fraction composition, wt.%: Methanol 97.2; 0.7 and NPP 2.1, part of which (26869 kg / h) is recirculated for recrystallization, and the remainder (3675 kg / h) is fed to the esterification of the oxidation product, and also 9674 kg / h with a temperature of 185 ° C and pressure 1.1 bar fraction composition, wt.%: MEPTK 45.6; DME, DMI and DMT 37.1; METAK 8.2; OIEB 4.6; Mmt 1,2; VK 0.4 and NPP 0.1, recycled for oxidation.
    Example 2 (Fig. 1 and 3). Example 1 is repeated with the difference that the secondary esterification vapors are washed with 1430 kg / h of the aqueous phase obtained at the stage of condensation of exhaust gases, having a temperature of 100 C. The purified secondary vapors with a temperature of 192 ° C and a pressure of 25 bar are fed to a heater 58, in which they are dried using high-temperature oil. Then the secondary vapors with a temperature of 206 ° C and a pressure of 25 bar are fed to the turboexpansion 59, in which the secondary vapors are brought to a pressure of 1.2 bar and a temperature of 84 ° C. The energy released is used to compress the steam methanol fraction before it is fed to the esterification. The resulting pressure drop phase is fed to the pressure release stage of the esterification product, and the bottom product of the esterification secondary washing stage is recycled to the top of column 52.
    Get the target product of the same quality and in the same quantity as in example 1.
    Example 3 (by a known method, Fig. 1 and 4). Example 1 is repeated, with the difference that the entire methanol vapor fraction (42,000 kg / h) obtained by evaporation of the filtrate is condensed with cooling water. The resulting liquid phase is divided into two streams, one of which (9000 kg / h of composition: 96.9% by weight of methanol, 0.46% by weight and 2.64% by weight of GMP) is brought to a pressure of 3 bar and after evaporation, the residue of the crude target product is processed for processing, and another (33000 kg / h of the same composition) is brought to a pressure of 28 bar, heated to boiling point, evaporated at 182 ° C and the resulting steam is heated to 250 ° C at help high-temperature oil, then served on the esterification.
    Get the target product of the same quality and in the same quantity as in example 1.
    Data confirming the positive effect of examples 1 and 2 compared 10
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    a stream consisting of the recrystallization filtrate of the target product and the MEPTA fraction withdrawn from the separation stage by distillation of the MEPTCR to a pressure of 2 bar and evaporated at 86 ° C. The resulting vapor in the amount of 33,000 kg / h is the methanol vapor fraction of the composition, wt%: methanol 96.9; H70 0.46 and NPP 2.64, by compression in a ratio of 15: 1 are adjusted to a pressure of 30 bar and from a temperature of 300 ° C are fed to the esterification stage carried out at 280 ° C and a pressure of 25 bar.
    Get the target product of the same quality and in the same quantity as in Example 1.
    Example 5 (Fig. 1 and 3). Examples 1 and 4sc are repeated. The difference is that the secondary esterification vapors are washed with 1430 kg / g of an aqueous phase obtained at the stage of condensation of exhaust gases, which have a temperature of 100 ° C. Purified secondary vapors with a temperature of 195 ° C and a pressure of 27 bar are fed to a heater 58, in which they are dried using high-temperature oil. Then the secondary vapors with a temperature of 271 ° C and a pressure of 27 bar are fed to a turbine expander 59, in which the secondary pairs are adjusted to a pressure of 0 bar and 30 ° C. The energy released is used to compress the vapor methanol fraction before it is fed to the esterification. The resulting pressure relief phase is fed to the pressure relief stage of the esterification product, and the bottom product of the esterification secondary washing stage is recycled to the top of column 52.
    Get the target product of the same quality and in the same quantity as in example 1.
    Example 6 (by a known method, Fig. 1 and 4). Examples 4 and 4 are repeated, with the difference that the entire vapor methanol fraction (42,000 kg / h) obtained by evaporation of the filtrate is condensed with cooling water. The resulting liquid phase is divided into two streams, one of which with Comparative Example 3, fresh (9000 kg / h of composition: 96.9 wt.%
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    the stream consisting of the recrystallization filtrate of the target product and the MEPTA fraction withdrawn from the separation stage by distillation of the MEPTCR is brought to a pressure of 2 bar and evaporated at 86 ° C. The resulting methanol vapor fraction in the amount of 33,000 kg / h of the composition, wt.%: Methanol 96.9; H70 0.46 and NPP 2.64, by compression in a ratio of 15: 1 are adjusted to a pressure of 30 bar and with a temperature of 300 ° C are fed to the esterification stage carried out at 280 ° C and a pressure of 25 bar.
    Get the target product of the same quality and in the same quantity as in example 1.
    Example 5 (Fig. 1 and 3). Examples 1 and 4sc are repeated, with the difference that the secondary esterification vapors are washed with 1430 kg / g of an aqueous phase obtained at the stage of condensation of exhaust gases, which have a temperature of 100 ° C. Purified secondary pairs with a temperature of 195 ° C and a pressure of 27 bar are fed to a heater 58, in which they are dried using high-temperature oil. Then the secondary vapors with a temperature of 271 ° C and a pressure of 27 bar are fed to a turbine expander 59, in which the secondary vapors are brought to a pressure of 0 bar and 30 ° C. The energy released is used to compress the vapor methanol fraction before it is fed to the esterification. The resulting pressure relief phase is fed to the pressure relief stage of the esterification product, and the bottom product of the esterification secondary washing stage is recycled to the top of column 52.
    Get the target product of the same quality and in the same quantity as in example 1.
    Example 6 (by a known method, Fig. 1 and 4). Examples 4 are repeated, with the difference that the entire methanol vapor fraction (42,000 kg / h), obtained by evaporation of the filtrate, is condensed with cooling water. The resulting liquid phase is divided into two streams, one of which (9000 kg / h composition: 96.9 wt.%
    Deny in tab. 1 and 2.
    Example 4 (Fig. 1 and 2). Example 1 is repeated with the difference that
    methanol, 0.46% by weight of HCO and 2.64% by weight of NPP) is brought to a pressure of 2 bar and after evaporation is fed to the processing of the residue by distillation of the crude target product, and the other (33000 kg / h of the same composition) is brought to pressure of 30 bar, heated to boiling point, evaporated at 185 ° C and the resulting steam is heated to AIA ° C using high-temperature oil, after which it is fed to the esterification. Get the target product of the same quality and in the same quantity as in example I.
    Data confirming the positive effect of examples 4 and 5 compared with comparative example 6 are summarized in table. 3 and 4.
    Example 7 (Fig. I and 2). Example 1 is repeated, with the difference that the stream consisting of the recrystallization filter of the target product and the MEPTA fraction withdrawn from the MEPTA distillation stage is brought to a pressure of 20 bar and evaporated at 168 ° C. The resulting methanol vapor fraction in an amount of 33,000 kg / h, wt.%: Methanol 96.9 NgO 0.46 and HGO1 2.64, is adjusted to a pressure of 25 bar by compressing in a ratio of 1.25: 1 to a temperature of served on the stage of esterification, carried out at 220 ° C and a pressure of 25 bar.
    Get the target product of the same quality and in the same quantity as in example 1.
    Example 8 (Fig. 1 and 3). Examples 1 and 7 are repeated, with the difference that the secondary esterification vapors are washed with 1430 kg / h of the oxidation of the aqueous phase obtained at the stage of condensation of exhaust gases having a temperature of 100 ° C. Purified secondary fumes with a temperature of 187 ° C and a pressure of 22 bar are fed to a heater 58, in which they are dried using high-temperature oil. Then the secondary vapors with a temperature of 196 ° C and a pressure of 22 bar are fed to a turbo-condensate 59, in which the secondary vapors are brought to a pressure of 8 bar and 143 ° C. The energy released is used to compress the vapor methanol fraction before it is fed to the esterification. The resulting pressure relief phase is fed to the pressure relief stage of the esterification product, and the bottom product of the esterification secondary washing stage is recycled to the top of column 52.
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    45938 12
    Get ridiculous product of the same quality and in the same quantity as in example 1.
    Example 9 (by a known method, Fig. 1 and 4). Examples 1 and 7 are repeated, with the difference that the entire methanol vapor fraction (42000 kg / h), obtained by evaporation of the filtrate, is condensed with cooling water. The resulting liquid phase is divided into two streams, one of which (9000 kg / h composition: 96.9 mA ..% methanol, 0.46., Wt.% H, 0 and 2.64 wt.% GSP) is brought to a pressure of 20 bar and after evaporation is fed to the processing of the residue by distillation of the crude target product, and another (33,000 kg / h of the same composition) is brought to a pressure of 25 bar followed by evaporation. The resulting steam is heated to 180 ° C using high-temperature oil, after which it is fed to the esterification. The target product has the same quality as in the product of example 1.
    Data confirming the positive effect of examples 7 and 8 compared with comparative example 9 are summarized in table. 5 and 6.
    From the above data it can be seen that the proposed method allows significantly (by 30-50% reduction of energy consumption for the process and at the same time obtain the target product of high quality (with the content of the main substance more than 99%).
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    权利要求:
    Claims (2)
    [1]
    1. Method of producing dimethyl terephthalate by liquid-phase oxidation of a mixture of n-xylene and a fraction containing p-toluic acid methyl ester with oxygen of air at a temperature of 140-170 ° C and a pressure of 4-8 bar in the presence of dissolved heavy metal compounds as a catalyst , followed by esterification of the resulting oxidation product, brought to elevated pressure, with liquid and then evaporated methanol at elevated temperatures and pressure, with the resulting fraction of the crude ester transferred to the methanol-containing secondary steam from stage and. esterification and separation by distillation of the crude ester into a fraction of methyl ester of n-toluic acid recycled
    13
    to oxidation, to the fraction of crude dimethyl terephthalate, which is further processed by recrystallization from methanol, and to the residue, characterized in that, in order to reduce energy consumption, esterification is carried out with methanol-containing steam, reduced to the degree of compression (1.25 - 15 ): 1 pressure of 25-30 bar and evaporated at 180-300 ° C, which is obtained from the recrystallization filtrate of crude dimethyl terephthalate by evaporation, or rectification
    Low pressure steam, High pressure steam. High-temperature oil, with cooling water.
    Indicators
    The value of the indicator, kW, for example
    Primary energy low pressure steam from process
    high pressure steam high temperature oil Electricity Total savings Sum of onrrhoeet.
    545938
    14
    methanol-containing secondary steam under a pressure of 2–20 bar, and the heat released during compression of methanol-containing steam, is used to overheat the methanol-containing vapor to the esterification temperature.
    [2]
    2. A method according to claim 2, in which the secondary vapors withdrawn from the esterification stage are washed with an aqueous phase followed by depressurization to 0.1-8 bar in a turbine expander and recycling them to the process.
    Table I
    table 2
    Pump 4418
    Is dividing
    capacity 4814453 - Pump 64-368
    Condenser 62-13026 Pump 67.-2
    Evaporator 702811 - Pump 7359
    Heater 741607-Evaporator 76-8757- (The heater 79-3670
    Drive komiresso Low pressure steam. High pressure steam, High temperature oil. Drain with cooling water. Produced on a turboexpander. "
    Indicators
    The value of the indicator, kW, for example 64Is
    Primary energy low pressure steam from high pressure steam process high temperature oil Electricity Total savings Energy cost
    T a b l i and a 3
    18
    18
    14495
    14495
    Table 4
    Low pressure steam. High pressure steam. High temperature oil. Discharged with cooling water. "Produced on a turbo expander."
    Primary energy is low-distant steam from the process.
    high-pressure steam high-temperature oil Electricity Total saving Energy cost
    T l fl l and c l 5
    Table 6
    1973
    992 8810
    324 140 10266
    18270
    992 8780
    2202
    420
    12394
    17990
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    US5646331A|1997-07-08|Process for working up residues from the raw ester distillation in the preparation of dimethyl terephthalate|
    JPS61130336A|1986-06-18|Polyester polymerization apparatus
    SU866997A1|1990-04-23|Method of producing polybutylene terephthalate
    同族专利:
    公开号 | 公开日
    JPS60204747A|1985-10-16|
    RO91101B|1987-04-01|
    DE3407925C1|1985-09-05|
    PL145300B1|1988-08-31|
    MX161720A|1990-12-18|
    YU44491B|1990-08-31|
    EP0156133B1|1987-01-14|
    BG45698A3|1989-07-14|
    US4642369A|1987-02-10|
    BR8500934A|1985-10-22|
    AR245686A1|1994-02-28|
    YU31385A|1987-10-31|
    TR22471A|1987-07-22|
    DE3560052D1|1987-02-19|
    RO91101A|1987-03-30|
    JPH0566378B2|1993-09-21|
    IN163349B|1988-09-10|
    CS251094B2|1987-06-11|
    EP0156133A1|1985-10-02|
    PL252194A1|1985-09-24|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2664547C2|2013-04-08|2018-08-20|Стора Энсо Ойй|Methods of deoxygenating bio-based material and production of bio-based terephtalic acid and olefin monomers|US2894978A|1956-07-02|1959-07-14|Chemische Werke Witten Gmbh|Process of producing esters of phthalic acids by oxidation of xylene and toluic acid ester mixtures|
    DE1071688B|1958-06-14|1959-12-24|Basf Ag|Process for improving the rate of oxidation of the mixtures resulting from air oxidation of xylene or of mixtures of xylene and methyl p-toluene acid esters|
    NL110864C|1958-11-07|
    US3076019A|1959-12-21|1963-01-29|Standard Oil Co|Process for production of dimethyl terephthalate|
    DE2427875C3|1974-06-10|1980-03-20|Dynamit Nobel Ag, 5210 Troisdorf|Process for the production of dimethyl terephthalate and of intermediates in dimethyl terephthalate manufacture|
    US4096340A|1975-06-03|1978-06-20|Teijin Hercules Chemical Co., Ltd.|Process for the preparation of dimethyl terephthalate|DE4026732A1|1990-08-24|1992-02-27|Huels Chemische Werke Ag|METHOD FOR CLEANING AN OXIDATION EXHAUST GAS WITH ENERGY RECOVERY|
    DE19618152C1|1996-05-07|1997-08-14|Huels Chemische Werke Ag|Energy-saving separation of crude di:methyl terephthalate fraction under mild conditions|
    DE19750491A1|1997-11-14|1999-05-20|Huels Chemische Werke Ag|High boiler circuit in the DMT process|
    WO2009079213A2|2007-12-03|2009-06-25|Gevo, Inc.|Renewable compositions|
    US8193402B2|2007-12-03|2012-06-05|Gevo, Inc.|Renewable compositions|
    BRPI1008287A2|2009-02-24|2016-03-15|Gevo Inc|renewable butadiene and isoprene preparation methods|
    CA2776177A1|2009-10-06|2011-04-14|Gevo, Inc.|Integrated process to selectively convert renewable isobutanol to p-xylene|
    CA2786607A1|2010-01-08|2011-07-14|Gevo, Inc.|Integrated methods of preparing renewable chemicals|
    JP2013517796A|2010-01-29|2013-05-20|ジェノマティカ・インコーポレイテッド|Method and microorganism for biosynthesis of p-toluic acid and terephthalic acid|
    US8373012B2|2010-05-07|2013-02-12|Gevo, Inc.|Renewable jet fuel blendstock from isobutanol|
    TW201247596A|2011-04-19|2012-12-01|Gevo Inc|Variations on prins-like chemistry to produce 2,5-dimethylhexadiene from isobutanol|
    DE102012105876A1|2012-07-02|2014-01-02|Oxea Gmbh|Process for the preparation of terephthalic acid and its derivatives|
    CN105985240A|2015-02-04|2016-10-05|华东理工大学|Novel process for reinforcement of esterification process in production of plasticizer|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE3407925A|DE3407925C1|1984-03-03|1984-03-03|Process for the preparation of dimethyl terephthalate from p-xylene and methanol|
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