JP3058155B2 - Apparatus and method for producing high-purity terephthalic acid - Google Patents
Apparatus and method for producing high-purity terephthalic acidInfo
- Publication number
- JP3058155B2 JP3058155B2 JP10343837A JP34383798A JP3058155B2 JP 3058155 B2 JP3058155 B2 JP 3058155B2 JP 10343837 A JP10343837 A JP 10343837A JP 34383798 A JP34383798 A JP 34383798A JP 3058155 B2 JP3058155 B2 JP 3058155B2
- Authority
- JP
- Japan
- Prior art keywords
- terephthalic acid
- water
- solid
- liquid separation
- purity terephthalic
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired - Lifetime
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、粗テレフタル酸
（ＣＴＡ）から高純度テレフタル酸（ＰＴＡ）を得る高
純度テレフタル酸の製造装置および方法に関するもので
ある。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus and a method for producing high-purity terephthalic acid (PTA) from crude terephthalic acid (CTA).
【０００２】[0002]
【従来の技術】粗テレフタル酸（ＣＴＡ）を含むスラリ
ーを、高温・高圧かつ適正な触媒下で水素と反応させた
後、フラッシュ蒸発冷却法に依り段階的に高純度テレフ
タル酸（ＰＴＡ）を結晶化する高純度テレフタル酸の製
造方法は、例えば、特表平７−５０７２９２号公報に開
示されている。このような高純度テレフタル酸の製造方
法においては、ＰＴＡをフラッシュ蒸発冷却法により段
階的に結晶化する際に発生する蒸気を熱源として利用し
ＣＴＡスラリーを加熱昇温する方法が知られている。2. Description of the Related Art A slurry containing crude terephthalic acid (CTA) is reacted with hydrogen at a high temperature and a high pressure under an appropriate catalyst, and then high-purity terephthalic acid (PTA) is crystallized stepwise by a flash evaporation cooling method. A method for producing high-purity terephthalic acid is disclosed in, for example, Japanese Patent Publication No. 7-507292. In such a method for producing high-purity terephthalic acid, there is known a method of heating and increasing the temperature of a CTA slurry by using steam generated when PTA is crystallized stepwise by a flash evaporation cooling method as a heat source.
【０００３】[0003]
【発明が解決しようとする課題】従来の技術において
は、フラッシュ蒸発冷却法により発生する蒸気は系外へ
排出されるかあるいはＣＴＡスラリーの加熱昇温用に使
用されている。In the prior art, the steam generated by the flash evaporation cooling method is discharged out of the system or used for heating and raising the temperature of the CTA slurry.
【０００４】しかし、フラッシュ蒸発冷却法により発生
する蒸気は数種類の圧力レベルを持ち、そのすべての圧
力レベルの蒸気が再利用されているわけではない。すな
わち、ＣＴＡスラリーの加熱昇温に利用する場合、フラ
ッシュ蒸発冷却法により段階的に得られる数種類の圧力
レベルの蒸気にうち最終段から発生する蒸気は温度差等
の問題から効率的な再利用が困難である。従って、エネ
ルギー原単位の向上の為には、最終段から発生する蒸気
を効率的に再利用することが課題であった。一方、固液
分離セクションにて、再スラリー用に供給される水の加
熱昇温のための熱源にはスチームや熱媒等のユーティリ
ティーが使用されているのが実状である。[0004] However, steam generated by the flash evaporative cooling method has several types of pressure levels, and not all of the pressure levels are reused. In other words, when utilizing the heating and heating of the CTA slurry, the steam generated from the final stage among the steams of several types of pressure levels obtained stepwise by the flash evaporative cooling method can be efficiently reused due to a problem such as a temperature difference. Have difficulty. Therefore, in order to improve the energy consumption unit, it has been a problem to efficiently reuse the steam generated from the last stage. On the other hand, in the solid-liquid separation section, utilities such as steam and a heat medium are used as a heat source for heating and raising the temperature of water supplied for reslurry.
【０００５】本発明の目的は、エネルギー回収がより効
率的になされた高純度テレフタル酸の製造装置および方
法を提供するものである。[0005] It is an object of the present invention to provide an apparatus and method for producing high-purity terephthalic acid with more efficient energy recovery.
【０００６】本発明の他の目的は、フラッシュ蒸発冷却
法により段階的に得られる数種類の圧力レベルの蒸気の
うち最終段から発生する蒸気を再利用した高純度テレフ
タル酸の製造装置および方法を提供するものである。Another object of the present invention is to provide an apparatus and a method for producing high-purity terephthalic acid by reusing steam generated from the final stage out of steam at several pressure levels obtained stepwise by flash evaporation cooling. Is what you do.
【０００７】[0007]
【課題を解決するための手段】固液分離セクションにお
いては、フラッシュ蒸発冷却法により得たＰＴＡスラリ
ーを固液分離装置を用いて母液と分離した後、分離され
たＰＴＡと同程度の温度まで加熱昇温された水にて再ス
ラリー化し、再度固液分離装置にて母液と分離すること
によりＰＴＡの洗浄を数回行う。In the solid-liquid separation section, the PTA slurry obtained by the flash evaporation cooling method is separated from the mother liquor using a solid-liquid separation device, and then heated to a temperature similar to that of the separated PTA. The PTA is washed several times by re-slurrying with heated water and separating it again from the mother liquor in a solid-liquid separator.
【０００８】そこで、フラッシュ蒸発冷却法により段階
的に発生する数種類の圧力レベルの蒸気の中で最低レベ
ルのものを直接あるいは間接的に熱源として利用し、供
給される水の加熱昇温に必要な熱量のいくらかを補い、
効率的なエネルギーの再利用を行うことが可能となる。[0008] In view of this, the lowest level steam of several pressure levels generated stepwise by the flash evaporative cooling method is used directly or indirectly as a heat source to heat and raise the temperature of the supplied water. Supplement some of the calories,
It is possible to efficiently reuse energy.
【０００９】[0009]
【発明の実施の形態】以下、本発明を図１により説明す
る。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to FIG.
【００１０】粗テレフタル酸（ＣＴＡ）は、純水と混合
されＣＴＡスラリー（１）となる。ＣＴＡスラリーは水
溶性溶媒が蒸発しないように約９０ｋｇ／ｃｍ２Ｇに加
圧され、直列に接続された多段の熱交換器により構成さ
れた昇温セクション（２）に供給され、後段の晶析セク
ションの晶析槽より発生する水蒸気（８）を一部利用し
約２８５℃の所定温度まで昇温され、水添反応槽の前段
に設置されたＣＴＡ溶解槽にて一定時間滞留され完全溶
解される。このＣＴＡ溶液は、第VIII族金属触媒を充填
した水添反応槽（３）において水添反応により精製が行
われる。ＣＴＡ溶液中の４−ＣＢＡはｐ−トルイル酸に
比較してテレフタル酸の結晶に共晶しやすい性質を有す
る為、ほぼ全量が水素との反応により還元され水溶性の
ｐ−トルイル酸に転化する。[0010] Crude terephthalic acid (CTA) is mixed with pure water to form a CTA slurry (1). The CTA slurry is pressurized to about 90 kg / cm 2 G so that the water-soluble solvent does not evaporate, supplied to a heating section (2) constituted by a multi-stage heat exchanger connected in series, and The temperature is raised to a predetermined temperature of about 285 ° C. using a part of the steam (8) generated from the crystallization tank, and is retained for a certain time in a CTA dissolving tank installed in front of the hydrogenation reaction tank to be completely dissolved. This CTA solution is purified by a hydrogenation reaction in a hydrogenation reaction tank (3) filled with a Group VIII metal catalyst. Since 4-CBA in the CTA solution has a property of being more likely to co-crystallize with terephthalic acid crystals than p-toluic acid, almost all the amount is reduced by reaction with hydrogen and converted to water-soluble p-toluic acid. .
【００１１】水添反応後のテレフタル酸溶液は結晶化セ
クション（４）に送られる。結晶化セクション（４）は
直列に接続された複数段の晶析槽より構成されており、
フラッシュ蒸発を利用して順時降温し、高純度テレフタ
ル酸結晶を得る。このフラッシュ蒸発の際に各晶析槽で
は降温の為に減圧をおこなうため、高温の水蒸気が放出
される。この実施例では最終段の晶析槽にて放出される
水蒸気（７）が選択される。The terephthalic acid solution after the hydrogenation reaction is sent to the crystallization section (4). The crystallization section (4) comprises a plurality of crystallization tanks connected in series,
The temperature is lowered gradually using flash evaporation to obtain high-purity terephthalic acid crystals. During this flash evaporation, high pressure water vapor is released in each crystallization tank because the pressure is reduced in order to lower the temperature. In this embodiment, the water vapor (7) released in the last stage crystallization tank is selected.
【００１２】結晶化セクションにて得られたテレフタル
酸溶液は固液分離セクション（５）に送られ固液分離装
置を用いてテレフタル酸と母液（６）とに分離される。
この際、分離されるテレフタル酸は、テレフタル酸と同
程度の温度まで昇温された水（１０）を用いて少なくと
も一回以上再スラリー化され、固液分離装置により分離
され洗浄される。この時、再スラリー化するための水を
昇温する熱交換器（９）の熱源として先のフラッシュ蒸
発により得られた水蒸気（７）を用いる。The terephthalic acid solution obtained in the crystallization section is sent to a solid-liquid separation section (5) and separated into terephthalic acid and a mother liquor (6) using a solid-liquid separation device.
At this time, the terephthalic acid to be separated is reslurried at least once using water (10) heated to a temperature similar to that of terephthalic acid, and separated and washed by a solid-liquid separator. At this time, water vapor (7) obtained by flash evaporation is used as a heat source of a heat exchanger (9) for raising the temperature of water for reslurrying.
【００１３】ここで得られたＰＴＡは乾燥セクション
（１１）にて乾燥させ、高純度テレフタル酸（１２）を
得る。The PTA obtained here is dried in the drying section (11) to obtain high-purity terephthalic acid (12).
【００１４】[0014]
【発明の効果】以上述べたように、本発明によれば、フ
ラッシュ蒸発冷却法により発生した数種の蒸気の中でエ
ネルギー回収の困難であった最低レベルの蒸気を利用し
てＰＴＡの洗浄のための再スラリー化用の水を昇温させ
ることができるので、エネルギーの回収効率を向上させ
ることが可能となった。As described above, according to the present invention, the cleaning of PTA is carried out by utilizing the lowest level of steam which is difficult to recover energy among several types of steam generated by the flash evaporation cooling method. The temperature of the water for reslurry can be raised, so that the energy recovery efficiency can be improved.
【図１】本発明による高純度テレフタル酸の製造方法の
一実施例を示すブロック図である。FIG. 1 is a block diagram showing one embodiment of a method for producing high-purity terephthalic acid according to the present invention.
１…ＣＴＡスラリー、２…昇温セクション、３…水添反
応槽、４…結晶化セクション、５…固液分離セクショ
ン、６…分離母液、７…水蒸気（最終段）、８…水蒸
気、９…熱交換器、１０…高純度の水溶性溶媒、１１…
乾燥セクション、１２…ＰＴＡ。DESCRIPTION OF SYMBOLS 1 ... CTA slurry, 2 ... Temperature rising section, 3 ... Hydrogenation reaction tank, 4 ... Crystallization section, 5 ... Solid-liquid separation section, 6 ... Separation mother liquor, 7 ... Steam (final stage), 8 ... Steam, 9 ... Heat exchanger, 10 ... high-purity water-soluble solvent, 11 ...
Dry section, 12 ... PTA.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平８−208561（ＪＰ，Ａ) 特開 昭50−49248（ＪＰ，Ａ) 特開 平５−58948（ＪＰ，Ａ) 特開 平９−295957（ＪＰ，Ａ) 特表 平７−507292（ＪＰ，Ａ) 特表 平９−511253（ＪＰ，Ａ) 国際公開98／18750（ＷＯ，Ａ１) (58)調査した分野(Int.Cl.7，ＤＢ名) C07C 63/26 C07C 51/44 ＣＡＰＬＵＳ（ＳＴＮ) ＲＥＧＩＳＴＲＹ（ＳＴＮ) ＷＰＩＤＳ（ＳＴＮ)──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-8-208561 (JP, A) JP-A-50-49248 (JP, A) JP-A-5-58948 (JP, A) JP-A-9-98 295957 (JP, A) Table 7-507292 (JP, A) Table 9-511253 (JP, A) WO 98/18750 (WO, A1) (58) Fields surveyed (Int. Cl. 7) , DB name) C07C 63/26 C07C 51/44 CAPLUS (STN) REGISTRY (STN) WPIDS (STN)
Claims (2)
ラリーを、昇温する昇温セクションと、昇温により水溶
液化されたＣＴＡ水溶液を所定の反応条件下で水素と反
応させる水添反応槽と、この水添反応槽からのテレフタ
ル酸水溶液をフラッシュ蒸発冷却法により段階的に結晶
化する結晶化セクションと、この結晶化セクションから
のテレフタル酸水溶液を、高純度テレフタル酸と母液と
に分離する固液分離セクションと、この固液分離セクシ
ョンからの高純度テレフタル酸を乾燥させる乾燥セクシ
ョンとからなり、上記固液分離セクションは、複数の固
液分離装置を備え、前段より分離された高純度テレフタ
ル酸をそれと同程度に昇温された水を用いて再スラリー
化して後段に送り洗浄するように構成され、さらに、上
記フラッシュ蒸発冷却法により段階的に発生した数種類
の圧力レベルの蒸気の中で最低レベルのものにより、上
記再スラリー化用の水を昇温させる熱交換器を有するこ
とを特徴とする高純度テレフタル酸の製造装置。1. A CTA powder in which crude terephthalic acid is mixed with water.
Heating section for heating the rally and water soluble by heating
The liquefied CTA aqueous solution reacts with hydrogen under predetermined reaction conditions.
Hydrogenation reaction tank and terephthalate from this hydrogenation reaction tank
Stepwise crystals Ri by Le acid solution to a flash evaporation cooling method
Crystallization section to crystallize, and from this crystallization section
Terephthalic acid aqueous solution with high purity terephthalic acid and mother liquor
And a solid-liquid separation section
Drying of high-purity terephthalic acid from
The solid-liquid separation section is composed of multiple solid-liquid separation sections.
High-purity terephthalate equipped with a liquid separator and separated from the previous stage
Re-slurry the luic acid with water of similar temperature
It is configured to be sent to the subsequent stage for cleaning.
Several types generated stepwise by the flash evaporation cooling method
The lowest level of steam at the pressure level
An apparatus for producing high-purity terephthalic acid, comprising a heat exchanger that raises the temperature of water for reslurrying .
条件下で水素と反応させ、フラッシュ蒸発冷却法により
段階的に結晶化し、その後、固液分離セクションにおい
て、高純度テレフタル酸と母液とを分離し、さらに乾燥
セクションにて乾燥させて高純度テレフタル酸を製造す
る際に、上記固液分離セクションは、複数の固液分離装
置を備え、前段より分離された高純度テレフタル酸をそ
れと同程度に昇温された水を用いて再スラリー化して後
段に送り洗浄するように構成され、再スラリー化用の水
の昇温の熱源として、フラッシュ蒸発冷却法により段階
的に発生した数種類の圧力レベルの蒸気の中で最低レベ
ルのものを直接あるいは間接的に利用することを特徴と
する高純度テレフタル酸の製造方法。2. Crude terephthalic acid is dissolved in water, reacted with hydrogen under predetermined reaction conditions, crystallized stepwise by flash evaporation cooling, and then, in a solid-liquid separation section, high-purity terephthalic acid and mother liquor are mixed. When the high-purity terephthalic acid is produced by further drying in a drying section, the solid-liquid separation section includes a plurality of solid-liquid separation devices, and the high-purity terephthalic acid separated from the preceding stage is separated therefrom. It is configured to re-slurry using water that has been heated to the same extent and send it to the subsequent stage for cleaning, and as a heat source for raising the temperature of water for re-slurry, several types of stepwise generated by flash evaporation cooling method A method for producing high-purity terephthalic acid, characterized by directly or indirectly using the lowest level of steam at a pressure level.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10343837A JP3058155B2 (en) | 1998-12-03 | 1998-12-03 | Apparatus and method for producing high-purity terephthalic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10343837A JP3058155B2 (en) | 1998-12-03 | 1998-12-03 | Apparatus and method for producing high-purity terephthalic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000169428A JP2000169428A (en) | 2000-06-20 |
| JP3058155B2 true JP3058155B2 (en) | 2000-07-04 |
Family
ID=18364631
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10343837A Expired - Lifetime JP3058155B2 (en) | 1998-12-03 | 1998-12-03 | Apparatus and method for producing high-purity terephthalic acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3058155B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110864308A (en) * | 2019-11-29 | 2020-03-06 | 沈福昌 | Harmless recovery and incineration treatment method for residue of purified terephthalic acid |
| WO2021103338A1 (en) * | 2019-11-29 | 2021-06-03 | 沈福昌 | Purified terephthalic acid residue recylcing recovery incineration treatment method |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MX359077B (en) * | 2004-09-02 | 2018-09-13 | Grupo Petrotemex Sa De Cv | Optimized production of aromatic dicarboxylic acids. |
| KR100826450B1 (en) | 2004-12-31 | 2008-04-29 | 주식회사 효성 | Process for economically refining naphthalenedicarboxylic acid and apparatus for processing the same |
| JP4569893B2 (en) * | 2006-11-14 | 2010-10-27 | クリーンメカニカル株式会社 | Citrus beverage manufacturing method and apparatus |
| MX2010012094A (en) * | 2008-05-20 | 2010-12-07 | Hitachi Plant Technologies Ltd | Method for treating separated mother liquor from terephthalic acid refinement. |
-
1998
- 1998-12-03 JP JP10343837A patent/JP3058155B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110864308A (en) * | 2019-11-29 | 2020-03-06 | 沈福昌 | Harmless recovery and incineration treatment method for residue of purified terephthalic acid |
| WO2021103338A1 (en) * | 2019-11-29 | 2021-06-03 | 沈福昌 | Purified terephthalic acid residue recylcing recovery incineration treatment method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2000169428A (en) | 2000-06-20 |
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