WO2012114434A1 - Procédé de traitement d'une liqueur mère d'acide téréphtalique purifié - Google Patents

Procédé de traitement d'une liqueur mère d'acide téréphtalique purifié Download PDF

Info

Publication number
WO2012114434A1
WO2012114434A1 PCT/JP2011/053701 JP2011053701W WO2012114434A1 WO 2012114434 A1 WO2012114434 A1 WO 2012114434A1 JP 2011053701 W JP2011053701 W JP 2011053701W WO 2012114434 A1 WO2012114434 A1 WO 2012114434A1
Authority
WO
WIPO (PCT)
Prior art keywords
terephthalic acid
mother liquor
crystals
primary
pressure
Prior art date
Application number
PCT/JP2011/053701
Other languages
English (en)
Japanese (ja)
Inventor
徳明 原
弘幸 豊嶋
初太郎 山▲崎▼
Original Assignee
株式会社日立プラントテクノロジー
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社日立プラントテクノロジー filed Critical 株式会社日立プラントテクノロジー
Priority to BR112013020492A priority Critical patent/BR112013020492A2/pt
Priority to PCT/JP2011/053701 priority patent/WO2012114434A1/fr
Priority to CN201180067951.5A priority patent/CN103443064B/zh
Publication of WO2012114434A1 publication Critical patent/WO2012114434A1/fr

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
    • C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
    • C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
    • C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation

Definitions

  • a crude terephthalic acid crystal produced by liquid phase oxidation of para-xylene is dissolved in high-temperature, high-pressure water, hydrorefined, and then cooled to produce a purified terephthalic acid crystal slurry.
  • PTA high-purity purified terephthalic acid
  • Para-xylene is used as a raw material to produce crude terephthalic acid (CTA) by liquid phase oxidation with an oxygen-containing gas in an acetic acid solvent in the presence of an oxidation catalyst, and then the crude terephthalic acid is dissolved in a high-temperature, high-pressure aqueous solvent.
  • CTA crude terephthalic acid
  • hydrorefining is performed with a hydrogen-containing gas to obtain a purified aqueous solution, and further through a crystallization step in which pressure-reducing cooling is performed to gradually reduce the pressure, a purified terephthalic acid crystal slurry is generated.
  • the purified terephthalic acid crystal slurry is subjected to solid-liquid separation to recover crystals, and the purified terephthalic acid (PTA) crystal powder that has undergone the drying process is used to produce polyester for fibers, films, and bottles. Manufactured as an acid.
  • PTA purified terephthalic acid
  • terephthalic acid crystals primary crystals
  • impurities such as 4-carboxybenzaldehyde (4-CBA) contained in crude terephthalic acid are converted to paratoluic acid by hydrogenation.
  • a separated mother liquor primary mother liquor
  • terephthalic acid that becomes saturated at the separation temperature is also dissolved in the primary mother liquor.
  • the primary mother liquor is further cooled to precipitate dissolved terephthalic acid and dissolved impurities, recovering low-purity terephthalic acid crystals (secondary crystals) and coexisting in the oxidation reaction of para-xylene.
  • Japanese Patent Publication No. 56-35175 Japanese Patent Laid-Open No. 5-58948.
  • the mother liquor (secondary mother liquor) from which the low-purity terephthalic acid crystal (secondary crystal) has been separated is directly used as it is or as a water solvent for dissolving the crude terephthalic acid crystal by subjecting it to fractional distillation.
  • a method of effectively using the secondary mother liquor such as using it has also been proposed.
  • the secondary mother liquor contains a lot of p-toluic acid, which is an impurity of purified terephthalic acid (PTA) crystals, so that it can be used directly as an aqueous solvent for dissolving crude terephthalic acid (CTA) crystals.
  • PTA purified terephthalic acid
  • CTA crude terephthalic acid
  • the suspension produced by the cooling method of the primary mother liquor is applied.
  • Suspensions are difficult to handle because the suspended particles (secondary crystals) are fine and sticky, and separation of the suspended particles (secondary crystals) causes clogging of the filter and a decrease in the recovery rate. It is said.
  • the secondary mother liquor remains in the dissolved impurities, in order to circulate and use it as dissolved water for hydrorefining, treatment by evaporation or distillation is required, but it is circulated and used without any treatment. However, there is a problem that it is limited by its use and its usage.
  • the present invention separates and recovers low-purity terephthalic acid crystals (secondary crystals) from the mother liquor separated with the primary crystals (primary mother liquor) with simple processing steps and good filtration performance. For the purpose.
  • the present invention improves the yield of terephthalic acid by recycling and using low-purity terephthalic acid crystals (secondary crystals) separated and recovered with good filtration performance as part of the raw material for producing terephthalic acid. Furthermore, it aims at reducing the amount of dissolved impurities in the primary mother liquor to reduce the generation of water to be reused and the wastewater treatment load.
  • purified terephthalic acid crystal slurry is solid-liquid separated under pressure (0.2 to 0.9 MPa), and the separated mother liquor (primary mother liquor) is obtained at a temperature of about 120 to 170 ° C. under pressure. Therefore, the present inventors added terephthalic acid crystals to the primary mother liquor, mixed, then supplied to the cooling tank adjusted to a pressure lower than atmospheric pressure, cooled by pressure reduction, and precipitated the crystals Thus, a processing method capable of obtaining a cooled suspension with improved filtration characteristics was achieved.
  • the present invention is to dissolve crude terephthalic acid produced by liquid-phase oxidation of para-xylene in water under high temperature and high pressure, hydrotreat it, cool it, and purify terephthalic acid.
  • the cooling suspension is characterized by comprising a secondary separation step of separating and recovering low-purity terephthalic acid crystals (secondary crystals) by filtration and separation under a pressure of atmospheric pressure or higher.
  • the purified terephthalic acid crystal slurry is separated from a mother liquor (primary mother liquor) at a temperature of about 120 to 170 ° C. and a pressure higher than the vapor pressure of the slurry (about 0.2 to 0.9 MPa),
  • a cooling suspension generation process terephthalic acid crystals are added to the separated mother liquor (primary mother liquor) and then supplied to a cooling tank adjusted to a reduced pressure of about 1.3 to 53 kPa (about 10 to 400 mmHg) to release the pressure.
  • a cooling suspension is produced by cooling.
  • terephthalic acid crystals are prepared in a slurry with water and added to the separated mother liquor (primary mother liquor) in a proportion of 0.05 to 1% by weight.
  • the terephthalic acid crystal added to the separated mother liquor is a crystal powder obtained by drying purified terephthalic acid crystals.
  • low-purity terephthalic acid crystals (secondary crystals) separated and recovered from the cooling suspension are used as part of the raw material for the liquid phase oxidation reaction of para-xylene. It is characterized by.
  • the mother liquor (secondary mother liquor) separated from the cooling suspension is used as a part of water for dissolving crude terephthalic acid.
  • the suspended primary mother liquor to which terephthalic acid crystals have been added in advance and mixed is subjected to pressure cooling, so that precipitates dissolved in the primary mother liquor, particularly crystalline impurities such as terephthalic acid and p-toluic acid are added.
  • the terephthalic acid crystal particles formed are deposited or adsorbed on the surface of the crystal as a nucleus, and the added terephthalic acid crystal particles are produced as grown. It is done.
  • the cooled suspension is recovered as low-purity terephthalic acid crystals (secondary crystals) to which impurities are more adhered by filtration separation.
  • the filterability is improved and the adhesion of the secondary crystals is also improved, so that a practical suspension is obtained.
  • the recovered secondary crystals are supplied as a part of the raw material for producing terephthalic acid by liquid phase oxidation of para-xylene, and the crystallized terephthalic acid as well as reaction intermediates such as p-toluic acid, which is an impurity, are oxidized to terephthalic acid.
  • the terephthalic acid crystals that contribute to the improvement of the yield and are added and mixed are also circulated and recovered, and there is no production loss.
  • the separated secondary mother liquor has a significantly reduced content of p-toluic acid as dissolved impurities and a small amount of dissolved metal compared to the secondary mother liquor separated by the conventional method without the addition of terephthalic acid crystals. It is also possible to increase the amount of reuse that is recycled in the aqueous solvent for chemical purification. In addition, the reduction of dissolved impurities in the secondary mother liquor reduces environmental burdens such as chemical oxygen demand (COD) when treating wastewater as industrial wastewater.
  • COD chemical oxygen demand
  • any terephthalic acid can be added to and mixed with terephthalic acid crystals
  • dried terephthalic acid is preferred, and the use of purified terephthalic acid (PTA) crystals, that is, high-purity terephthalic acid products contain p-toluic acid. Effective in reducing the amount. This is thought to be due to the fact that the terephthalic acid crystals are dried, which enlarges the crystal surface (increases pores and surface roughness) or activates it, increasing the adsorption power and the amount of terephthalic acid crystals. More dissolved impurities with good affinity are adsorbed on the surface of the added terephthalic acid crystal, and the residual impurities in the secondary mother liquor are reduced.
  • PTA purified terephthalic acid
  • the filterability of the product crystal separation is improved.
  • the practical effect on the primary treatment method such as improvement of the recovery rate of secondary crystals and reduction of the impurity content in the secondary mother liquor is great. That is, the improvement in filterability improves the filtration rate and the stability of filtration, makes the filter smaller, and enables stable continuous or semi-continuous operation.
  • the recovery rate of the secondary crystals is improved by stable operation, and the cost and labor of the equipment and maintenance of the filter are reduced.
  • the improvement in the recovery rate of the secondary crystals greatly contributes to the improvement in the yield of crude terephthalic acid and purified terephthalic acid because the recovered secondary crystals are reused as part of the oxidation reaction raw material.
  • the reduction of dissolved impurities (paratoluic acid) in the secondary mother liquor leads to an improvement in the recovery rate of the secondary crystals, and the secondary mother liquor can be recycled in the water that dissolves crude terephthalic acid. Reduction. As a result, the amount of wastewater treated is reduced and the environmental load is reduced.
  • FIG. 1 shows all steps of a high-purity terephthalic acid production method using para-xylene as a raw material, positioning of a primary mother liquor during separation of purified terephthalic acid crystals, secondary crystals after the treatment of the primary mother liquor according to the present invention, and The positioning of the next mother liquor and the flow of processing outline are shown.
  • CTA crude terephthalic acid
  • crystallization is performed by oxidation reaction using paraxylene as a raw material, and then crude terephthalic acid (CTA) crystals are produced by a solid-liquid separator.
  • CTA crystals are prepared in a CTA slurry adjustment tank, dissolved, hydrorefined and cooled to obtain purified terephthalic acid crystal slurry, and then solid-liquid separator 1 Separated into PTA crystals and primary mother liquor.
  • the primary mother liquor is produced as a cooled suspension in the pressure-reducing cooling tank 13 and separated into secondary crystals and secondary mother liquor by the filter 15.
  • the separated secondary crystals are reused as part of the crude terephthalic acid production raw material para-xylene, and the separated secondary mother liquor is a part of the aqueous solvent that dissolves the crude terephthalic acid crystals in the purified terephthalic acid production process. Will be reused. Secondary mother liquor that has not been reused is treated in a wastewater treatment process.
  • the flow which uses a refined terephthalic acid (PTA) crystal as a terephthalic acid (TA) crystal added to a primary mother liquor is shown with the dotted line.
  • FIG. 2 shows an overall process for producing high-purity terephthalic acid according to an embodiment of the present invention.
  • the purified terephthalic acid crystal slurry is subjected to solid-liquid separation with a solid-liquid separator 1 under pressure, and purified terephthalic acid crystals ( Primary crystals) are collected and supplied to a schematic flow for producing high-purity terephthalic acid via the crystal washing tank 2.
  • the outline flow of the processing method of the embodiment of the present invention using the mother liquor (primary mother liquor) from which purified terephthalic acid crystals (primary crystals) are separated is as follows: primary mother liquor tank 10 ⁇ slurry preparation tank 12 ⁇ pressure-reduction cooling tank 13 ⁇ filter 15. ⁇ The secondary mother liquor tank 16 flows. Note that the description of the stirring blade of the container (tank) is provided with a stirrer because the content is slurry or suspension.
  • FIG. 3 is an explanatory diagram for performing a treatment test of the separated primary mother liquor according to the embodiment of the present invention.
  • the purified terephthalic acid slurry produced in the purified terephthalic acid production process is solid-liquid separated to obtain purified terephthalic acid crystals and a separated mother liquor (primary mother liquor), and then the flow of processing of the primary mother liquor in the production process (purified terephthalic acid
  • a flow (primary mother liquor treatment test area) in which the primary mother liquor is collected from the high temperature / high pressure primary mother liquor tank and the method of the present invention is carried out is shown separately from the production area).
  • the filtration test was conducted by sampling a steady flow from the pressure-reducing cooling tank to the waste liquid treatment process.
  • a solid-liquid separation system for purified terephthalic acid crystal slurry performed under pressure (about 0.2 to 0.9 MPa) is further used for primary crystals obtained by centrifugation or filtration separation as described in JP-B-47-49049.
  • a system for performing high-purity purified terephthalic acid crystals after washing by re-slurrying with water is as follows: solid-liquid separator 1 ⁇ crystal washing tank 2 ⁇ flash cooling tank 3 ⁇ slurry supply tank 4 ⁇
  • the flow of the solid-liquid separator 5 ⁇ the dryer 6, and the method according to the embodiment of the present invention is performed using the primary mother liquor obtained from the system as a starting material.
  • the primary mother liquor obtained by filtration separation through a filter medium contains a trace amount of suspended suspended solids (terephthalic acid crystal particles) in the mother liquor that is leaked (about 0.01% by weight or less). Therefore, when the primary mother liquor by filtration separation is selected as a starting material, the effect of the method of the embodiment of the present invention in which terephthalic acid crystals are added and mixed is expected more.
  • the filterability of the secondary crystals and the remaining amount of dissolved impurities in the secondary mother liquor, which is the subject of the present invention, with respect to the primary mother liquor from the filtration separation of the purified terephthalic acid crystal slurry are improved. Needs for practical use were higher.
  • the primary mother liquor primary mother liquor tank 10 obtained at about 120 to 170 ° C. under pressure (about 0.2 to 0.9 MPa)
  • about 0.1 to 0.5% by weight of terephthalic acid is dissolved and paratoluic acid is about 0.03 as an impurity. It is dissolved at a rate of ⁇ 0.15% by weight.
  • terephthalic acid crystals are added to and mixed with the primary mother liquor.
  • the terephthalic acid crystals to be added may be added directly and mixed as they are. It is preferable that the slurry is made into a slurry (40% by weight) (slurry preparation tank 12) and then fed and mixed in a primary mother liquor under pressure (about 0.2 to 0.9 MPa). The amount is supplied to be about 0.05 to 1% by weight with respect to the primary mother liquor, but it is preferable to add about 0.1 to 0.5% by weight to improve the filterability relative to the amount of terephthalic acid crystals added.
  • Suspended primary mother liquor mixed with terephthalic acid crystals is directly supplied to the depressurization cooling tank 13 that is decompressed to about 1.3 to 53 kPa (about 10 to 400 mmHg) below atmospheric pressure using a vacuum pump or an ejector.
  • a suspension is formed which is decompressed and evaporated to about 10-80 ° C.
  • the cooling suspension may be generated by reducing the pressure of the plurality of cooling tanks to about 1.3 to 53 kPa (about 10 to 400 mmHg) below atmospheric pressure by stepwise releasing the pressure.
  • the effect of this embodiment can be obtained if the final cooling tank can be cooled by releasing pressure under a reduced pressure of about 1.3 to 53 kPa (about 10 to 400 mmHg) below atmospheric pressure to produce a cooled suspension.
  • the final temperature in the pressure-reduction cooling bath 13 is preferably a lower cooling temperature under a reduced pressure of less than atmospheric pressure from the viewpoint of crystallization and recovery of dissolved substances and reduction of dissolved impurities in the secondary mother liquor after separation.
  • a cooled suspension at about 30 to 65 ° C. under a reduced pressure of about 4 to 26 kPa (about 30 to 200 mmHg).
  • the evaporated vapor is condensed and recirculated to the pressure-reducing cooling tank 13, but is reconstituted as treated water having a reduced paratoluic acid content as evaporative condensed water proposed by the present inventors in WO2009 / 141968. It can also be used.
  • the suspension in the pressure-relief cooling tank 13 is separated into secondary crystals and secondary mother liquor by a filter.
  • a filter In order to filter and separate a suspension containing fine particles that remain sticky, It is preferable to carry out clarification filtration under atmospheric pressure or pressure exceeding the pressure of the final cooling tank (below atmospheric pressure), press filter, hundback filter (manufactured by IHI), cricket filter (manufactured by Tsukishima Kikai Co., Ltd.) A pressure filter such as is used.
  • the separated secondary crystal is prepared as a raw material for the oxidation reaction of para-xylene, slurried with solvent acetic acid, and then used as a part of the raw material for producing terephthalic acid (secondary crystal flow in FIG. 1).
  • the secondary mother liquor will be reused as part of the dissolved water for dissolving and hydrotreating crude terephthalic acid, but the amount reused is dissolved impurities (paratriylic acid) remaining in the secondary mother liquor. It will be adjusted according to the amount.
  • the secondary mother liquor that has not been used is directly treated as wastewater by a method such as activated sludge that has been carried out conventionally, the amount and load of wastewater treatment to be treated can be further reduced (secondary mother liquor flow in FIG. 1). .
  • an aqueous solvent with a further reduced amount of impurities (a content of p-toluic acid) can be recovered by a treatment such as fractional distillation proposed in JP-A-5-58948.
  • Example 1 After producing crude terephthalic acid (CTA) by liquid-phase air oxidation of p-xylene, the obtained crude terephthalic acid is dissolved in water and hydrorefined at high temperature and pressure to produce high-purity terephthalic acid (PTA) During production, the purified terephthalic acid (PTA) crystal slurry at high temperature and high pressure (about 145 ° C, about 0.4 MPa) obtained from the crystallization process is solid-liquid separated to obtain purified terephthalic acid (PTA) crystals, washed and dried The process produces purified terephthalic acid (PTA).
  • CTA crude terephthalic acid
  • PTA purified terephthalic acid
  • the separation mother liquor (primary mother liquor) obtained from the solid-liquid separation step is transferred to a waste liquid treatment step under atmospheric pressure through a high temperature / high pressure storage tank (high temperature / high pressure primary mother liquor) and processed. ing.
  • a portion of the primary mother liquor in the high-temperature / high-pressure primary mother liquor tank of the purified terephthalic acid production area (FIG. 3) is separated by piping branching under high-temperature / high pressure (about 145 ° C, about 0.4 MPa). Taken (primary mother liquor treatment test area in Fig.
  • terephthalic acid crystals dried purified terephthalic acid crystals (PTA powder)
  • PTA powder dried purified terephthalic acid crystals
  • the terephthalic acid slurry is continuously supplied at a ratio of 0.75 wt% (PTA crystal addition rate 0.15%) with respect to the primary mother liquor, mixed with the primary mother liquor, and then supplied to the cooling tank to cool by pressure reduction.
  • the cooling suspension at about 60 ° C. generated in the cooling tank is discharged back to the waste water treatment step for the primary mother liquor.
  • Example 2 In the method of Example 1, 20 wt% terephthalic acid crystal water slurry is supplied at a ratio of 0.35 wt% (PTA crystal addition rate 0.07%) to the primary mother liquor, and is cooled by releasing pressure to produce a cooled suspension. did. As in Example 1, the cooled suspension was collected and subjected to a filtration test. As a result, each filtration time was 113 sec and the content of p-toluic acid was 0.033 wt%.
  • Example 3 In the method of Example 1, a 20 wt% terephthalic acid crystal water slurry was supplied at a ratio of 1.5 wt% (PTA crystal addition rate: 0.3%) to the primary mother liquor, and cooled under pressure to produce a cooled suspension. . As in Example 1, the cooled suspension was collected and subjected to a filtration test. As a result, each filtration time was 38 sec, and the content of p-toluic acid was 0.017 wt%.
  • Example 4 In the method of Example 1, a 20 wt% terephthalic acid crystal water slurry was supplied at a rate of 2.25 wt% (PTA crystal addition rate 0.45%) to the primary mother liquor, cooled under pressure, and cooled and suspended. A liquid was produced. As in Example 1, the cooled suspension was collected and subjected to a filtration test. As a result, each filtration time was 41 sec, and the content of p-toluic acid was 0.011 wt%.
  • Example 5 In the method of Example 1, a 20 wt% terephthalic acid crystal water slurry was prepared using a wet cake (PTA crystals before drying) separated from the purified terephthalic acid crystal slurry, and 0.75 wt% (PTA) relative to the primary mother liquor. The crystal was added at a rate of 0.15%) and cooled under pressure to produce a cooled suspension. As in Example 1, the cooled suspension was collected and subjected to a filtration test. As a result, each filtration time was 40 sec and the content of p-toluic acid was 0.032 wt%.
  • Example 6 In the method of Example 1, the pressure-release cooling tank pressure was adjusted to about 7.3 kPa (about 55 mmHg temperature about 40 ° C.), and the pressure-release cooling was performed to produce a cooled suspension. As in Example 1, the cooled suspension was collected and subjected to a filtration test. As a result, the filtration time was 59 sec and the paratoluic acid content was 0.008 wt%.
  • Example 7 In the method of Example 1, the pressure-release cooling tank pressure was adjusted to about 47 kPa (about 355 mmHg temperature about 80 ° C.), and 20 wt% terephthalic acid crystal water slurry was added to 1.5 wt% (PTA crystal addition rate 0.3%) with respect to the primary mother liquor. %) was applied to perform pressure relief cooling to produce a cooled suspension. As in Example 1, the cooled suspension drainage was collected and subjected to a filtration test. As a result, the filtration time was 28 sec and the paratoluic acid content was 0.031 wt%.

Abstract

Dans la présente invention, une suspension épaisse d'acide téréphtalique purifié générée au cours de la production d'acide téréphtalique de pureté élevée par une oxydation en phase liquide et une purification par hydrogénation en utilisant du p-xylène comme matériau de départ, est séparée en une liqueur mère primaire et des cristaux primaires de l'acide téréphtalique purifié. L'acide téréphtalique ainsi que l'acide p-toluique et d'autres matières dissoutes sont refroidis et précipités dans la liqueur mère primaire séparée, et séparés par filtration pour séparer et récupérer des cristaux d'acide téréphtalique de faible pureté, en tant que partie d'une matière première pour la réaction d'oxydation en phase liquide du p-xylène. Les cristaux d'acide téréphtaliques sont nouvellement ajoutés à et mélangés dans la liqueur mère primaire séparée, et ensuite le mélange est chargé dans une cuve de refroidissement ajustée pour être à une pression réduite inférieure à la pression atmosphérique, et refroidi par décompression, améliorant de cette manière la filtrabilité de la matière précipitée. La quantité de matière dissoute résiduelle dans une liqueur mère secondaire également séparée par filtration est réduite.
PCT/JP2011/053701 2011-02-21 2011-02-21 Procédé de traitement d'une liqueur mère d'acide téréphtalique purifié WO2012114434A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
BR112013020492A BR112013020492A2 (pt) 2011-02-21 2011-02-21 método para tratar um licor mãe separado de um ácido tereftálico purificado
PCT/JP2011/053701 WO2012114434A1 (fr) 2011-02-21 2011-02-21 Procédé de traitement d'une liqueur mère d'acide téréphtalique purifié
CN201180067951.5A CN103443064B (zh) 2011-02-21 2011-02-21 精制对苯二甲酸母液的处理方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2011/053701 WO2012114434A1 (fr) 2011-02-21 2011-02-21 Procédé de traitement d'une liqueur mère d'acide téréphtalique purifié

Publications (1)

Publication Number Publication Date
WO2012114434A1 true WO2012114434A1 (fr) 2012-08-30

Family

ID=46720255

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2011/053701 WO2012114434A1 (fr) 2011-02-21 2011-02-21 Procédé de traitement d'une liqueur mère d'acide téréphtalique purifié

Country Status (3)

Country Link
CN (1) CN103443064B (fr)
BR (1) BR112013020492A2 (fr)
WO (1) WO2012114434A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111960941A (zh) * 2020-07-31 2020-11-20 贵州永润天泽化工有限公司 一种3,5-二甲基苯甲酸的提纯方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01121239A (ja) * 1987-11-04 1989-05-12 Idemitsu Petrochem Co Ltd 芳香族カルボン酸の製造方法
JP2004231642A (ja) * 2003-01-10 2004-08-19 Mitsubishi Chemicals Corp 芳香族カルボン酸含有スラリーの遠心分離方法
JP2006008671A (ja) * 2004-05-28 2006-01-12 Mitsubishi Chemicals Corp 高純度テレフタル酸の製造方法
JP2009203163A (ja) * 2006-06-13 2009-09-10 Mitsubishi Chemicals Corp テレフタル酸の乾燥方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2003292742A1 (en) * 2003-01-10 2004-08-10 Mitsubishi Chemical Corporation Method of centrifugal separation of slurry containing aromatic carboxylic acid
CN1960960B (zh) * 2004-05-28 2010-09-15 三菱化学株式会社 高纯度对苯二甲酸的制造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01121239A (ja) * 1987-11-04 1989-05-12 Idemitsu Petrochem Co Ltd 芳香族カルボン酸の製造方法
JP2004231642A (ja) * 2003-01-10 2004-08-19 Mitsubishi Chemicals Corp 芳香族カルボン酸含有スラリーの遠心分離方法
JP2006008671A (ja) * 2004-05-28 2006-01-12 Mitsubishi Chemicals Corp 高純度テレフタル酸の製造方法
JP2009203163A (ja) * 2006-06-13 2009-09-10 Mitsubishi Chemicals Corp テレフタル酸の乾燥方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111960941A (zh) * 2020-07-31 2020-11-20 贵州永润天泽化工有限公司 一种3,5-二甲基苯甲酸的提纯方法

Also Published As

Publication number Publication date
CN103443064A (zh) 2013-12-11
BR112013020492A2 (pt) 2016-10-25
CN103443064B (zh) 2015-09-23

Similar Documents

Publication Publication Date Title
JPH1025266A (ja) 高純度イソフタル酸の製造方法
WO2005075403A1 (fr) Procede pour produire de l'acide carboxylique aromatique
WO2004043893A1 (fr) Procede de production d'acide terephtalique
JP2014221791A (ja) テレフタル酸の回収のための改善された方法
KR101943115B1 (ko) 필터 공급 슬러리중 물의 백분율을 제어함으로써 테레프탈산 퍼지 여과 속도를 개선하는 방법
WO2012114434A1 (fr) Procédé de traitement d'une liqueur mère d'acide téréphtalique purifié
JP5973437B2 (ja) フィルターフィードスラリーにおける水のパーセントを制御することによるテレフタル酸パージろ過速度の向上
JP5802115B2 (ja) 粗製テレフタル酸の精製方法
JP5869571B2 (ja) フィルターフィードスラリーにおける水の％を制御することによるテレフタル酸パージろ過速度の向上
JP2013537548A5 (fr)
JP2006045201A (ja) 高純度テレフタル酸の製造方法
JP2004231644A (ja) 高純度テレフタル酸の製造方法
KR20150138844A (ko) 순수 플랜트 모액 용매 추출 시스템 및 방법
JP2004175797A (ja) テレフタル酸の製造方法
JP2019131526A (ja) 酢酸含有水溶液からの酢酸の回収方法
CN1708472A (zh) 对苯二甲酸的制备方法
TW201544460A (zh) 純工廠廢水的純化及回收
JP2006008673A (ja) 高純度テレフタル酸の製造方法
KR100708919B1 (ko) 테레프탈산의 회수 방법
WO2005115957A1 (fr) Procédé servant à produire de l'acide téréphtalique de pureté élevée
JP2004269521A (ja) 芳香族カルボン酸の製造方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 11859037

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

REG Reference to national code

Ref country code: BR

Ref legal event code: B01A

Ref document number: 112013020492

Country of ref document: BR

122 Ep: pct application non-entry in european phase

Ref document number: 11859037

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: JP

ENP Entry into the national phase

Ref document number: 112013020492

Country of ref document: BR

Kind code of ref document: A2

Effective date: 20130812