KR100708919B1 - A method of recovering terephthalic acid - Google Patents
A method of recovering terephthalic acid Download PDFInfo
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Abstract
본 발명은 테레프탈산의 회수 방법에 관한 것으로서, 보다 상세하게는 조테레프탈산을 수소화 반응 시키고 결정화 공정을 통하여 테레프탈산을 석출시킨 후, 1차 고액분리공정에서 석출된 테레프탈산을 회수하고, 남은 모액을 50~90℃로 냉각시키고 고액분리기를 사용하여 석출물을 분리하는 것을 특징으로 하는 테레프탈산 회수 방법에 대한 것이다. 본 발명의 테레프탈산 회수 방법에 따르면, 모액에 포함되어 폐수처리되는 테레프탈산을 효율적으로 회수함으로써 테레프탈산 제조 수율을 향상시키고 폐수처리 부하를 감소시킬 수 있다. The present invention relates to a method for recovering terephthalic acid, and more particularly, after hydrogenation of crude terephthalic acid and precipitation of terephthalic acid through a crystallization process, recovering terephthalic acid precipitated in the first solid-liquid separation process, the remaining mother liquor is 50 ~ 90 It is about a terephthalic acid recovery method characterized by cooling to ℃ and separating the precipitate using a solid-liquid separator. According to the terephthalic acid recovery method of the present invention, it is possible to efficiently recover the terephthalic acid contained in the mother liquor to be treated with waste water, thereby improving the yield of terephthalic acid and reducing the wastewater treatment load.
Description
도 1은 본 발명에 따른 테레프탈산 회수 공정의 모식도이다.1 is a schematic diagram of a terephthalic acid recovery process according to the present invention.
1: 산화 반응기 2: 결정조1: oxidation reactor 2: crystal bath
3: 고액분리기 4: 건조기3: solid-liquid separator 4: dryer
5: 환원반응기 6: 결정조5: reduction reactor 6: crystal bath
7: 1차 고액분리기 8: 건조기7: first solid-liquid separator 8: dryer
9: 냉각기 10: 2차 고액분리기9: chiller 10: secondary solid-liquid separator
L1 : 조테레프탈산 L2: 테레프탈산 슬러리L1: Zoterephthalic Acid L2: Terephthalic Acid Slurry
L3, L4, L8 : 모액 L5: 초산 또는 물L3, L4, L8: mother liquor L5: acetic acid or water
L6, L7 : 슬러리L6, L7: Slurry
본 발명은 테레프탈산의 회수 방법에 관한 것으로서, 보다 상세하게는 조테레프탈산을 수소화 반응 시키고 결정화 공정을 통하여 테레프탈산을 석출시킨 후, 1차 고액분리공정에서 석출된 테레프탈산을 회수하고, 남은 모액을 50~90℃로 냉각시키고 고액분리기를 사용하여 석출물을 분리하는 것을 특징으로 하는 테레프탈산 회수 방법에 대한 것이다.The present invention relates to a method for recovering terephthalic acid, and more particularly, after hydrogenation of crude terephthalic acid and precipitation of terephthalic acid through a crystallization process, recovering terephthalic acid precipitated in the first solid-liquid separation process, the remaining mother liquor is 50 ~ 90 It is about a terephthalic acid recovery method characterized by cooling to ℃ and separating the precipitate using a solid-liquid separator.
테레프탈산은 방향족 카르복실산의 일종으로서 섬유, 수지 등에 널리 사용되는 폴리에스테르의 원료로서 사용되고 있다. 테레프탈산의 제조방법으로는 산화반응기에서 코발트, 망간 등의 중금속 화합물 및 브롬 화합물을 촉매로 하고 초산 등의 저급 지방족 카르복실산을 함유하는 반응 용매 중에서, 파라자일렌을 분자상 산소 함유 가스와 접촉시켜 액상 산화하는 방법이 상용화되어 있다. Terephthalic acid is a kind of aromatic carboxylic acid and is used as a raw material of polyester widely used in fibers, resins and the like. As a method for producing terephthalic acid, paraxylene is contacted with a molecular oxygen-containing gas in a reaction solvent containing heavy aliphatic carboxylic acids such as cobalt and manganese and bromine compounds in an oxidation reactor as a catalyst. Liquid phase oxidation is commercially available.
그러나, 파라자일렌의 산화에 의해 얻어지는 조테레프탈산(Crude Teraphthalic Acid)중에는, 4-카르복시벤즈알데히드 등의 불순물이 다량으로 함유되어 있는데, 불순물인 4-카르복시벤즈알데하이드는 테레프탈산과 달리 관능기가 하나로 중합시 중합반응을 종료시키는 물질이므로 정제공정을 거쳐 제거해 주어야 고순도의 테레프탈산을 얻을 수 있다. However, Crude Teraphthalic Acid obtained by oxidation of paraxylene contains a large amount of impurities such as 4-carboxybenzaldehyde, and 4-carboxybenzaldehyde, which is an impurity, is polymerized when one functional group is polymerized unlike terephthalic acid. As it is a substance that terminates the reaction, it must be removed through a purification process to obtain high purity terephthalic acid.
이를 위하여, 조테레프탈산을 고온, 고압조건에서 물에 녹여 수소화 반응을 통해 4-카르복시벤즈알데하이드를 파라톨루익산으로 전환한다. To this end, Zoterephthalic acid is dissolved in water at high temperature and high pressure to convert 4-carboxybenzaldehyde to paratoluic acid through hydrogenation.
수소화 반응 후 감압, 감온의 결정화 공정을 거치게 되는데, 이때 파라톨루익산보다 물에 대한 용해도가 낮은 테레프탈산은 결정화되어 석출되게 되고, 파라톨루익산은 물에 용해된 상태로 존재하게 된다. 고액 분리 공정을 거쳐 파라톨루익산은 물과 함께 배출되며, 고체 형태로 분리된 테레프탈산은 불순물이 제거된 고순도 테레프탈산이 되며, 건조 후 제품으로 완성된다. 분리된 액체는 냉각시켜 일반적으로 폐수처리장으로 보내진다. After the hydrogenation reaction, a pressure reduction and a temperature reduction crystallization process are performed, wherein terephthalic acid having a lower solubility in water than paratoluic acid is crystallized and precipitated, and paratoluic acid is present in a dissolved state in water. Paratoluic acid is discharged with water through a solid-liquid separation process, and terephthalic acid separated in solid form becomes high-purity terephthalic acid from which impurities are removed. The separated liquid is cooled down and generally sent to a wastewater treatment plant.
그러나, 고액 분리 공정의 온도가 150℃ 정도로 고온이어서 파라톨루익산 및 기타 불순물 이외에 상당량의 테레프탈산을 포함하게 되기 때문에, 이를 효율적으로 회수하여 테레프탈산 제조 수율을 향상시킴으로써 경제적 손실을 방지하고, 폐수처리장으로 유입되는 유기물을 줄여 폐수처리 부하를 감소시킬 수 있는 공정의 개발이 요구되고 있다. However, since the solid-liquid separation process has a high temperature of about 150 ° C., it contains a significant amount of terephthalic acid in addition to paratoluic acid and other impurities, thereby efficiently recovering it and improving the yield of terephthalic acid, thereby preventing economic loss and entering the wastewater treatment plant. There is a need for development of a process that can reduce wastewater treatment load by reducing organic matter.
본 발명의 목적은 테레프탈산 제조 수율을 향상시키고 폐수처리 부하를 감소시키기 위하여, 조테레프탈산을 수소화 반응시키고 결정화 공정을 통하여 테레프탈산을 석출시킨 후, 1차 고액분리공정에서 석출된 테레프탈산을 회수하고, 남은 모액을 50~90℃로 냉각시키고 2차 고액분리기를 사용하여 석출물을 분리하는 것을 특징으로 하는 테레프탈산 회수 방법을 제공하는 것이다. An object of the present invention is to improve the production yield of terephthalic acid and reduce the waste water treatment load, after the hydrogenation of the crude terephthalic acid and precipitated terephthalic acid through the crystallization process, to recover the terephthalic acid precipitated in the first solid-liquid separation process, the remaining mother liquor It is to provide a terephthalic acid recovery method characterized in that to cool to 50 ~ 90 ℃ and to separate the precipitate using a secondary solid-liquid separator.
본 발명의 목적은 조테레프탈산을 수소화 반응시키고 결정화 공정을 통하여 테레프탈산을 석출시킨 후, 1차 고액분리공정에서 석출된 테레프탈산을 회수하고, 남은 모액을 50~90℃로 냉각시키고 2차 고액분리기를 사용하여 석출물을 분리하는 것을 특징으로 하는 테레프탈산 회수 방법을 제공함으로써 달성된다. An object of the present invention is to hydrogenate the crude terephthalic acid and precipitate the terephthalic acid through the crystallization process, recover the terephthalic acid precipitated in the first solid-liquid separation process, the remaining mother liquor is cooled to 50 ~ 90 ℃ and using a second solid-liquid separator It is achieved by providing a terephthalic acid recovery method characterized in that the precipitate is separated.
일반적으로, 산화공정에서 생성된 조테레프탈산(L1)은 정제공정의 환원반응기, 결정조, 고액분리기 및 건조기를 거쳐서 불순물이 제거되어 고순도 테레프탈산이 얻어진다. 환원공정에서는 테레프탈산의 중간체인 4-카르복시벤즈알데하이드를 파라톨루익산으로 전환하며, 결정조를 거쳐 압력과 온도를 낮추어 테레프탈산(L2)을 결정으로 석출한다. 결정조는 대개 3-5개로 구성되며, 순차적으로 압력 및 온 도를 낮추어 석출되는 테레프탈산의 입자를 조정해 준다. 마지막 단계의 결정조의 온도는 160도, 압력은 5기압 정도이다. 이 조건에서 테레프탈산은 대부분 고체 형태로 존재하며, 일부가 액체상에 녹아있게 되고, 파라톨루익산 등의 불순물은 물에 대한 용해도가 커서 거의 대부분이 액체상인 모액에 녹아 존재하게 된다. In general, the crude terephthalic acid (L1) produced in the oxidation process is removed through the reduction reactor, crystal bath, solid-liquid separator and dryer of the purification process to obtain a high purity terephthalic acid. In the reduction process, 4-carboxybenzaldehyde, an intermediate of terephthalic acid, is converted to paratoluic acid, and the terephthalic acid (L2) is precipitated as a crystal by lowering the pressure and temperature through a crystal bath. The crystal bath is usually composed of 3-5 pieces, in order to adjust the particles of terephthalic acid precipitated by sequentially lowering the pressure and temperature. The temperature of the crystallization tank of the last stage is 160 degrees and the pressure is about 5 atmospheres. Under these conditions, terephthalic acid is mostly present in solid form, and part of it is dissolved in the liquid phase, and impurities such as paratoluic acid are solubility in water that most of them are dissolved in the mother liquor, which is in the liquid phase.
결정조를 거친 후 테레프탈산(L2)은 슬러리 형태가 되어 1차 고액분리기로 유입된다. 1차 고액분리기는 일반적으로 원심분리기, 진공분리기 등을 사용하며, 분리된 고체 형태의 테레프탈산은 건조기를 거쳐 고순도 테레프탈산 제품이 된다. After passing through the crystal bath, terephthalic acid (L2) is in the form of a slurry is introduced into the first solid-liquid separator. The primary solid-liquid separator generally uses a centrifuge, a vacuum separator, and the like, and the terephthalic acid in the form of a separated solid is converted into a high purity terephthalic acid product through a dryer.
테레프탈산이 분리되고 남은 모액(L3)에는 불순물인 파라톨루익산 이외에도 테레프탈산이 함께 용해되어 존재하므로 이의 회수가 경제성 측면이나 폐기물 처리관점에서 중요하다. 모액중에 포함되어 있는 테레프탈산의 농도는 결정조 압력 및 온도 조건, 1차 고액분리기 분리 성능에 따라 달라지는데, 대개 3,000-10,000 중량ppm 정도이며, 파라톨루익산의 농도는 500-4000중량ppm이고, 기타 불순물의 농도가 300-1500중량ppm정도이다. In addition to paratoluic acid, which is an impurity, terephthalic acid is dissolved in the mother liquor (L3) remaining after terephthalic acid is separated, its recovery is important in terms of economics and waste disposal. The concentration of terephthalic acid in the mother liquor depends on the crystal bath pressure and temperature conditions, and the separation performance of the first solid-liquid separator, usually about 3,000-10,000 ppm by weight, the concentration of paratoluic acid is 500-4000 ppm by weight, and other impurities. The concentration of is about 300-1500 ppm by weight.
모액(L3)은 온도가 160도, 압력 5기압 정도로서, 본 발명에서는 모액을 적정 온도로 냉각시키면서 압력을 낮추어서 테레프탈산, 파라톨루익산 및 기타 불순물들을 용해도에 따라 석출시킨다. 상기 냉각을 위해서는 냉각수를 사용하는 열교환기를 사용할 수 있다. The mother liquor L3 has a temperature of 160 degrees and a pressure of about 5 atmospheres. In the present invention, the mother liquor is cooled down to an appropriate temperature to lower the pressure to precipitate terephthalic acid, paratoluic acid and other impurities according to solubility. For the cooling may be used a heat exchanger using a cooling water.
모액의 온도를 낮춤에 따라 용해도가 낮고 농도가 높은 테레프탈산이 먼저 석출되고, 용해도는 높으나 농도가 높은 파라톨루익산이 석출되고, 계속 온도를 낮추어 줄 경우 기타 불순물도 석출되기 시작한다.As the temperature of the mother liquor is lowered, terephthalic acid with lower solubility and higher concentration is precipitated first, paratoluic acid with higher solubility but higher concentration is precipitated and other impurities start to precipitate when the temperature is lowered.
테레프탈산의 회수를 증가시키기 위해서는 냉각기를 통해 모액(L3)의 온도를 최대한 낮추어 주어야 하나 과도하게 냉각할 경우 상대적으로 용해도가 높은 파라톨루익산 및 기타 불순물들의 석출이 많아지게 되며, 이를 회수할 경우 공정에 불순물을 증가시켜 품질을 저하시킬 수 있다. In order to increase the recovery of terephthalic acid, it is necessary to lower the temperature of the mother liquor (L3) as much as possible through a cooler. However, excessive cooling causes the precipitation of relatively high solubility of paratoluic acid and other impurities. Increasing the impurities may degrade the quality.
따라서, 본 발명에서 적절한 냉각온도는 50-90℃이고 바람직하게는 60~80℃이다. 상기 온도에서는 용해되어 있는 테레프탈산의 80%이상이 석출되게 되며, 파라톨루익산은 석출이 시작되고 기타 불순물들은 거의 석출이 되지 않으므로, 테레프탈산의 회수 효율은 높이면서 불순물을 줄일 수 있다. Therefore, suitable cooling temperature in the present invention is 50-90 ℃ and preferably 60-80 ℃. At this temperature, more than 80% of the dissolved terephthalic acid is precipitated, and since paratoluic acid starts to precipitate and other impurities hardly precipitate, it is possible to reduce impurities while increasing the recovery efficiency of terephthalic acid.
냉각기를 거친 모액(L4)에 포함되어 있는 석출된 테레프탈산과 파라톨루익산을 회수하기 위해 2차 고액분리기를 사용할 수 있다. 2차 고액분리기는 카트리지(cartridge) 필터, 미세여과필터(microfilter), 원심분리기, 침전조 등을 사용할 수 있다. 2차 고액분리기에서 회수된 고체는 90%이상이 테레프탈산이며, 10%미만이 파라톨루익산이며, 미량의 기타 불순물을 포함하게 된다. A secondary solid-liquid separator may be used to recover the precipitated terephthalic acid and paratoluic acid contained in the mother liquor (L4) passed through the cooler. The secondary solid-liquid separator may use a cartridge filter, a microfilter, a centrifuge, a settling tank, and the like. More than 90% of the solids recovered in the secondary solid-liquid separator are terephthalic acid, less than 10% of paratoluic acid, and contain traces of other impurities.
본 발명에서 2차 고액분리공정에서 분리한 테레프탈산을 고순도 테레프탈산으로 회수하기 위해서는 파라톨루익산과 기타불순물을 제거해 주어야 하는데 이를 위해 두 가지 방법을 사용할 수 있다. 첫 번째 방법은 회수된 고체를 산화반응기로 보내서 파라톨루익산을 테레프탈산으로 산화시키고, 기타 불순물을 제거해 주는 것이고, 두 번째 방법은 정제공정으로 보내서 테레프탈산은 회수하고, 파라톨루익산과 기타 불순물들을 제거하는 것이다. In the present invention, in order to recover the terephthalic acid separated in the second solid-liquid separation process as high purity terephthalic acid, paratoluic acid and other impurities must be removed, and two methods can be used. The first method is to send the recovered solid to the oxidation reactor to oxidize paratoluic acid to terephthalic acid and to remove other impurities. The second method is to send the purification process to recover terephthalic acid and to remove paratoluic acid and other impurities. will be.
첫번째 방법에 따라서 산화반응기로 유입시키기 위해서는 산화반응에 사용되 는 용매가 초산이므로 회수된 고체에 초산(L5)을 넣어주어 고체 농도가 3-20%정도가 되게 조정하여 슬러리(7) 형태로 산화반응기로 유입시킨다. 테레프탈산과 함께 유입된 파라톨루익산 및 기타 불순물들은 산화되어 역시 테레프탈산으로 회수되며, 불순물중의 일부는 산화공정의 불순물로 작용할 수 있으며, 이를 제거해 주기 위해 산화공정 모액의 일부를 빼내 줄 수 있다. 두 번째 방법에 따라서 정제공정으로 보내 회수하기 위해서는 정제공정의 용매인 물(L5) 을 유입시켜 역시 고체 농도가 3-20%정도가 되게 조정하여 슬러리(L6) 형태로 정제공정의 환원반응기로 유입시킨다. 테레프탈산은 정제공정을 거쳐 회수되며, 파라톨루익산이나 기타 불순물은 1차 고액분리기를 거쳐 모액으로 처리되어 제거된다.In order to flow into the oxidation reactor according to the first method, since the solvent used for the oxidation reaction is acetic acid, acetic acid (L5) is added to the recovered solid to adjust the solid concentration to about 3-20% and oxidize in the form of slurry (7). Flow into the reactor. Paratoluic acid and other impurities introduced with terephthalic acid are oxidized and recovered as terephthalic acid, and some of the impurities may act as impurities in the oxidation process, and some of the oxidation mother liquor may be removed to remove them. According to the second method, water (L5), which is a solvent of the purification process, is introduced into the refining process for recovery, and the solid concentration is adjusted to 3-20%. Let's do it. Terephthalic acid is recovered through a purification process and paratoluic acid or other impurities are removed by treatment with the mother liquor via a first solid-liquid separator.
이하, 실시예를 참조하여 본 발명을 상세히 설명한다. 그러나, 본 발명의 범위가 이들 실시예의 기재만으로 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail with reference to Examples. However, the scope of the present invention is not limited only to the description of these examples.
실시예 1Example 1
1차 고액분리기로 분리된 150℃ 정도의 모액을 냉각기를 이용하여 60℃까지 냉각시키고 석출된 고체를 100 마이크로미터의 미세필터를 장착한 2차 고액분리기로 분리하였다. 모액 및 석출된 고체에 포함된 각 성분의 함량은 하기 표 1에 기재하였으며, 모액으로부터 분리된 고체상의 함량은 테레프탈산 87%, 파라톨루익산 12%, 기타 불순물 1%이었다. 상기 결과로부터, 본 발명의 테레프탈산 회수방법에 의하여 효과적으로 모액 중의 테레프탈산이 회수됨을 확인할 수 있었다. The mother liquor at 150 ° C. separated by the first solid-liquid separator was cooled to 60 ° C. using a cooler, and the precipitated solid was separated by a second solid-liquid separator equipped with a 100 micrometer fine filter. The content of each component included in the mother liquor and the precipitated solid is shown in Table 1 below, and the content of the solid phase separated from the mother liquor was 87% terephthalic acid, 12% paratoluic acid, and 1% other impurities. From the above results, it was confirmed that the terephthalic acid in the mother liquid was effectively recovered by the terephthalic acid recovery method of the present invention.
이어서, 초산을 가하여 이들 고체 성분이 10%, 초산 90%가 되도록 슬러리 형 태로 만들어서 산화반응기로 유입시킨 후, 테레프탈산을 회수하고, 파라톨루익산은 산화반응을 통해 테레프탈산으로 전환하여 회수한다.Subsequently, acetic acid is added to form a slurry so that these solid components are 10% and 90% acetic acid, and introduced into an oxidation reactor. Then, terephthalic acid is recovered, and paratoluic acid is converted to terephthalic acid through an oxidation reaction and recovered.
표 1Table 1
실시예 2Example 2
1차 고액분리기로 분리된 모액은 150도로 이를 냉각기를 이용하여 80℃까지 냉각시켜 석출된 고체를 80마이크로미터의 미세필터를 장착한 2차 고액분리기로 분리하였다. 모액 및 석출된 고체에 포함된 각 성분의 함량은 하기 표 2에 기재하였으며, 모액으로부터 분리된 고체상의 함량은 테레프탈산 97%, 파라톨루익산 3%, 기타 불순물 0.1%이었다. 상기 결과로부터, 냉각 온도 80℃에서도 본 발명의 테레프탈산 회수방법에 의하여 효과적으로 모액 중의 테레프탈산이 회수됨을 확인할 수 있었다. The mother liquor separated by the first solid-liquid separator was cooled to 80 ° C. using a cooler to separate the precipitated solid by a second solid-liquid separator equipped with a 80 micrometer fine filter. The content of each component contained in the mother liquor and the precipitated solid is shown in Table 2 below, and the content of the solid phase separated from the mother liquor was 97% terephthalic acid, 3% paratoluic acid and 0.1% other impurities. From the above results, it was confirmed that the terephthalic acid in the mother liquid was effectively recovered by the terephthalic acid recovery method of the present invention even at a cooling temperature of 80 ° C.
이어서, 이들 고체 성분이 10%, 물 90%가 되도록 슬러리 형태로 만들어 환원반응기로 유입시켜, 테레프탈산을 회수하고, 파라톨루익산 및 기타 불순물은 정제공정을 거쳐 제거한다. Subsequently, these solid components are made into a slurry so that 10% and 90% of water are introduced into a reduction reactor to recover terephthalic acid, and paratoluic acid and other impurities are removed through a purification process.
표 2 TABLE 2
본 발명에 따르면, 테레프탈산 제조시 정제공정의 고액분리단계에서 모액에 포함되어 폐수처리되는 테레프탈산을 효율적으로 회수함으로써 테레프탈산 제조 수율을 향상시켜 경제적 손실을 방지하고, 폐수처리장으로 유입되는 유기물을 줄여 폐수처리 부하를 감소시킬 수 있다. According to the present invention, when terephthalic acid is produced in the solid-liquid separation step of the refining process, by efficiently recovering terephthalic acid to be treated in the wastewater to improve the production rate of terephthalic acid to prevent economic losses, to reduce the organic matter flowing into the wastewater treatment plant wastewater treatment The load can be reduced.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04145044A (en) * | 1990-10-03 | 1992-05-19 | Mitsubishi Gas Chem Co Inc | Production of high-purity terephthalic acid |
| WO1993024440A1 (en) | 1992-05-29 | 1993-12-09 | Imperial Chemical Industries Plc | Process for the production of purified terephthalic acid |
| JPH0648982A (en) * | 1992-07-27 | 1994-02-22 | Mitsubishi Gas Chem Co Inc | Production of high-purity terephthalic acid |
| US5563293A (en) * | 1991-03-07 | 1996-10-08 | Imperial Chemical Industries Plc | Process for the production of terephthalic acid |
| JPH0987230A (en) * | 1995-09-22 | 1997-03-31 | Mitsubishi Gas Chem Co Inc | Production of high-purity terephthalic acid |
| JPH10287614A (en) | 1997-02-17 | 1998-10-27 | Mitsui Chem Inc | Production of highly pure terephthalic acid |
| JP2001031621A (en) | 1999-05-18 | 2001-02-06 | Mitsui Chemicals Inc | Production of high-purity terephthalic acid |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04145044A (en) * | 1990-10-03 | 1992-05-19 | Mitsubishi Gas Chem Co Inc | Production of high-purity terephthalic acid |
| US5563293A (en) * | 1991-03-07 | 1996-10-08 | Imperial Chemical Industries Plc | Process for the production of terephthalic acid |
| WO1993024440A1 (en) | 1992-05-29 | 1993-12-09 | Imperial Chemical Industries Plc | Process for the production of purified terephthalic acid |
| JPH0648982A (en) * | 1992-07-27 | 1994-02-22 | Mitsubishi Gas Chem Co Inc | Production of high-purity terephthalic acid |
| JPH0987230A (en) * | 1995-09-22 | 1997-03-31 | Mitsubishi Gas Chem Co Inc | Production of high-purity terephthalic acid |
| JPH10287614A (en) | 1997-02-17 | 1998-10-27 | Mitsui Chem Inc | Production of highly pure terephthalic acid |
| JP2001031621A (en) | 1999-05-18 | 2001-02-06 | Mitsui Chemicals Inc | Production of high-purity terephthalic acid |
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