KR970042471A - Method for producing terephthalic acid (3) - Google Patents

Method for producing terephthalic acid (3) Download PDF

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Publication number
KR970042471A
KR970042471A KR1019950056787A KR19950056787A KR970042471A KR 970042471 A KR970042471 A KR 970042471A KR 1019950056787 A KR1019950056787 A KR 1019950056787A KR 19950056787 A KR19950056787 A KR 19950056787A KR 970042471 A KR970042471 A KR 970042471A
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South Korea
Prior art keywords
terephthalic acid
polyethylene terephthalate
producing terephthalic
terephthalate
waste
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KR1019950056787A
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Korean (ko)
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노항덕
배동목
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김준응
주식회사 선경인더스트리
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Priority to KR1019950056787A priority Critical patent/KR970042471A/en
Publication of KR970042471A publication Critical patent/KR970042471A/en

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Abstract

본 발명은 테레프탈산의 제조방법에 관한 것으로서 더욱 상세하게는 폴리에스터 섬유 감량가공 공정에서 배출되는 알칼리 감량 페액을 사용하여 폐 폴리에틸렌 테레프탈레이트(Polythylene terephthalate)를 가수분해하여 테레프탈산 나트륨염의 슬러리를 만들고, 이를 물에 용해하고 흡착시켜 불순물을 제거한 다음, 산으로 중화하여 고순도의 테레프탈산을 제조. 회수하는 방법에 관한 것이다.The present invention relates to a method for preparing terephthalic acid, and more particularly, to waste polyethylene terephthalate (Polythylene terephthalate) by using an alkaline weight loss liquid discharged from a polyester fiber weight reduction process to make a slurry of sodium terephthalate salt, and water Dissolved in and adsorbed to remove impurities, and then neutralized with acid to prepare terephthalic acid of high purity. It relates to a method of recovery.

Description

테레프탈산의 제조방법(3)Method for producing terephthalic acid (3)

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

Claims (16)

폴리에틸렌 테레프탈레이트를 가수분해하고 결정화하여 테레프탈산을 제조하는 방법에 있어서, 가) 폐 폴리에틸렌 테레프탈레이트를 알칼리 감량 페액과 침윤제에 의해 가수분해시켜 테레프탈산 나트륨염을 형성하는 공정 ; 나) 테레프탈산 나트륨염을 물에 용해시켜 얻은 수용액을 고액(固液)분리하여 고체는 상기의 가)가수분해 공정으로 피드백(feed back)되고, 액체는 다음의 흡착공정으로 옮겨가는 공정 ; 다)테레프탈산 나트륨염 수용액을 흡차시키고, 산으로 중화하여 테레프탈산을 얻는 공정 ; 라) 테레프탈산을 비대화시키는 결정화 공정 ; 마) 비대화된 테레프탈산을 감압하에 냉각하고, 여과 및 건조하는 공정으로 이루어진 것을 특징으로 하는 테레프탈산의 제조방법A method for producing terephthalic acid by hydrolyzing and crystallizing polyethylene terephthalate, comprising the steps of: a) forming a terephthalate sodium salt by hydrolyzing the waste polyethylene terephthalate with an alkaline weight loss solution and a wetting agent; B) solid-liquid separation of the aqueous solution obtained by dissolving the terephthalate sodium salt in water, and the solid is fed back to the above hydrolysis process, and the liquid is transferred to the next adsorption process; C) a step of sucking the aqueous terephthalate sodium salt solution and neutralizing with acid to obtain terephthalic acid; D) a crystallization step of enlarging terephthalic acid; E) a method of producing terephthalic acid, characterized in that the enlarged terephthalic acid is cooled under reduced pressure, filtered and dried. 제 1 항에 있어서, 상기 가)가수분해공정시 폴리에틸렌 테레프탈레이트로는 폐 폴리에스터 섬유, 페 폴리에틸렌 테레프탈레이트 병, 폐 폴리에틸렌 테레프탈레이트 용기, 폴리에틸렌 테레프탈레이트 중합과정에서 발생하는 폐 폴리에틸렌 테레프탈레이트 칩, 또는 폴리에스터 섬유 제조과정에서 발생하는 폐 폴리에스터사(絲)를 사용하는 것을 특징으로 하는 테레프탈산의 제조방법.The method of claim 1, wherein a) polyethylene terephthalate in the hydrolysis process, waste polyester fiber, waste polyethylene terephthalate bottle, waste polyethylene terephthalate container, waste polyethylene terephthalate chip generated during the polymerization of polyethylene terephthalate, or A method for producing terephthalic acid, characterized by using waste polyester yarns produced during polyester fiber production. 제 1 항 또는 제 2 항에 있어서, 상기 폐폴리에틸렌 테레프탈레이트는 전체 가수분해 반응물 중에 1~25 중량% 첨가하는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 1 or 2, wherein the waste polyethylene terephthalate is added in an amount of 1 to 25% by weight in the total hydrolysis reactants. 제 1 항에 있어서, 상기 가)가수분해공정에서 알칼리 감량 폐액으로는 폴리에스터 섬유의 감량 가공 공정에서 배출되는 폐액을 사용하는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 1, wherein the a) waste liquid discharged from the weight loss processing step of the polyester fiber is used as the alkali loss solution in the hydrolysis step. 제 4 항에 있어서, 상기 알칼리 감량 폐액은 전체 가수분해 반응물 중에 수산화나트륨이 5~30 중량% 함유되도록 첨가하는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 4, wherein the alkaline weight loss solution is added so that 5-30% by weight of sodium hydroxide is contained in the total hydrolyzate. 제 5 항에 있어서, 상기 알칼리 감량 폐액은 수산화나트륨이 1~20% 함유되어 있는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 5, wherein the alkaline weight loss liquid contains 1 to 20% of sodium hydroxide. 제 5 항에 있어서, 상기 알칼리 감량 폐액 첨가시 수산화나트륨을 함께 첨가하여 사용하는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 5, wherein sodium hydroxide is added together when the alkaline weighting waste solution is added. 제 1 항에 있어서, 상기 침윤제는 전체 가수분해 반응물 중에 1~30 중량 % 첨가하는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 1, wherein the wetting agent is added in an amount of 1 to 30% by weight in the total hydrolysis reactants. 제 1 항에 있어서, 상기 가)가수분해공정은 30~200 ℃ 반응온도 및 1~20 kg/㎠ 반응압력하에서 진행되는 것을 특징으로 하는 테레프탈산의 제조방법.The method for preparing terephthalic acid according to claim 1, wherein the a) hydrolysis process is performed at a reaction temperature of 30 to 200 ° C and a reaction pressure of 1 to 20 kg / cm 2. 제 1 항에 있어서, 상기 나)용해공정에서 물은 테레프탈산 나트륨염 용액에 대하여 0.5~3.0 중량배 사용하는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 1, wherein water is used in a dissolution step in an amount of 0.5 to 3.0 times by weight based on the terephthalate sodium salt solution. 제 1 항에 있어서, 상기 라)결정화 공정은 1~5개의 결정화조가 직렬로 연결되어 있고 각 단계별 결정화조의 온도가 30~50 ℃씩 감소되도록 설치되어 있는 결정화 조내에서 진행하는 것을 특징으로 하는 테레프탈산의 제조방법.2. The terephthalic acid according to claim 1, wherein the crystallization process is performed in a crystallization tank in which 1 to 5 crystallization tanks are connected in series and installed so that the temperature of each stage crystallization tank is reduced by 30 to 50 ° C. Manufacturing method. 제 11항에 있어서, 상기 결정화조는 120~300 ℃ 온도 및 2~86kg/㎠ 압력이 유지 되도록 하는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 11, wherein the crystallization tank is maintained at a temperature of 120 to 300 ° C. and a pressure of 2 to 86 kg / cm 2. 제 1 항에 있어서, 상기 마)냉각공정은 60~90 ℃ 온도 및 0.1~1.0kg/㎠ 압력하에서 진행하는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 1, wherein the cooling step is performed at a temperature of 60 to 90 ° C. and a pressure of 0.1 to 1.0 kg / cm 2. 제 1 항 또는 제 13 항에 있어서, 상기 마)냉각공정은 배출되는 알코올과 물은 상기의 가)가수분해공정으로 피드백(feed back)되는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 1 or 13, wherein in the e) cooling step, the alcohol and water discharged are fed back to the a) hydrolysis step. 제 1 항에 있어서, 상기 마) 여과공정에서 배출되는 여과액은 바이포라 막을 이용한 전기투석장치(electro-dialyzer)에 투입되어 산(acid)과 수산화나트륨으로 분리되며, 산(acid)은 상기의 다)중화공정으로 피드백(feed back)되고, 수산화나트륨은 상기의 가)가수분해공정으로 피드백(feed back)되는 것을 특징으로 하는 테레프탈산의 제조방법.According to claim 1, wherein the filtrate discharged from the filtration process is put into an electro-dialyzer using a bipora membrane (separated into acid and sodium hydroxide), the acid (acid) is C) A method of producing terephthalic acid, characterized in that it is fed back to the neutralization process, and sodium hydroxide is fed back to the hydrolysis process described above. 페 폴리에틸렌 테레프탈레이트를 원료물질로하여 테레프탈산을 제조하는 장치에 있어서, 페 폴리에틸렌 테레프탈레이트가 알칼리 감량 폐액에 의해 가수분해되는 가수분해장치(1), 테레프탈산 나트륨염을 용해하는 용해장치(2), 원심분리기(3), 흡착탑(4), 테레프탈산 나트륨염을 산(acid)으로 중화하여 테레프탈산을 생성하는 중화장치(5), 테레프탈산 입자를 비대화하여 결정화장치(6), 냉각장치(7), 비대화된 테레프탈산을 여과하는 여과장치(8), 그리고 여과된 테레프탈산을 건조하는 건조장치(9)가 연속적으로 설치되어 있는 것을 특징으로 하는 테레프탈산 제조 장치.In the apparatus for producing terephthalic acid using pe polyethylene terephthalate as a raw material, a hydrolysis device (1) in which the pe polyethylene terephthalate is hydrolyzed by an alkali reduction waste solution, a dissolving device (2) for dissolving terephthalate sodium salt, and centrifugation Separator (3), adsorption tower (4), neutralizing device (5) for neutralizing sodium terephthalate with acid to produce terephthalic acid, crystallizing device (6), cooling device (7), enlarged A filtering device (8) for filtering terephthalic acid and a drying device (9) for drying the filtered terephthalic acid are continuously provided.
KR1019950056787A 1995-12-26 1995-12-26 Method for producing terephthalic acid (3) KR970042471A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100429385B1 (en) * 2001-04-09 2004-04-29 한국화학연구원 Process for preparing high purified terephthalic acid from PET
KR100493136B1 (en) * 2002-04-06 2005-06-01 주식회사 부림이앤씨 Method for treating waste water from loss-in-quantity process of polyester-based textures

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100429385B1 (en) * 2001-04-09 2004-04-29 한국화학연구원 Process for preparing high purified terephthalic acid from PET
KR100493136B1 (en) * 2002-04-06 2005-06-01 주식회사 부림이앤씨 Method for treating waste water from loss-in-quantity process of polyester-based textures

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