KR970042469A - Method for producing terephthalic acid (1) - Google Patents

Method for producing terephthalic acid (1) Download PDF

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KR970042469A
KR970042469A KR1019950056785A KR19950056785A KR970042469A KR 970042469 A KR970042469 A KR 970042469A KR 1019950056785 A KR1019950056785 A KR 1019950056785A KR 19950056785 A KR19950056785 A KR 19950056785A KR 970042469 A KR970042469 A KR 970042469A
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terephthalic acid
polyethylene terephthalate
alkali metal
earth metal
producing
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KR1019950056785A
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Korean (ko)
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KR100224466B1 (en
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노항덕
배동목
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김준응
주식회사 선경인더스트리
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
    • 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
    • C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
    • C07C63/14—Monocyclic dicarboxylic acids
    • C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
    • C07C63/26—1,4 - Benzenedicarboxylic acid

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

본 발명은 테레트탈산의 제조방법에 관한 것으로서, 더욱 상세하게는 폐 폴리에틸렌 테레프탈레이트를 알칼리 수용액으로 가수분해하여 테레트탈산 알칼리금속/토금속염의 슬러리를 만들고, 산으로 중화하여 생성된 테레프탈산을 입자비대화시켜 높은 회수율로서 고순도의 테레프탈산을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing terephthalic acid, and more particularly, to hydrolyze waste polyethylene terephthalate with an aqueous alkali solution to form a slurry of alkali metal / earth metal salts of terephthalate, and to neutralize terephthalic acid produced by neutralization with an acid. It relates to a method of producing terephthalic acid of high purity with a high recovery rate by enlarging.

Description

테레프탈산의 제조방법(1)Method for producing terephthalic acid (1)

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

Claims (13)

폴리에틸렌 테레프탈레이트를 가수분해하고 결정화하여 테레프탈산을 제조하는 방법에 있어서, 가) 물 용매 및 침윤제 존재하에 폐폴리에틸렌 테레프탈레이트가 수산화알칼리금속/토금속에 의해 가수분해되어 테레프탈산 알칼리금속/토금속염을 형성하는 공정 ;나) 테레프탈산 알칼리금속/토금속염을 물에 용해시켜 얻은 수용액을 고액(固液)분리하여 고체는 상기 가) 가수분해 공정으로 피드백(feed back)되고, 액체는 다음의 흡착공정으로 옮겨가는 공정 ;다) 테레프탈산 알칼리금속/토금속염 수용액을 흡착시키고, 산으로 중화하여 테레프탈산을 얻는 공정 ;라) 테레프탈산을 비대화시키는 결정화공정 ;마) 비대화된 테레프탈산을 감압하에 냉각하고, 여과 및 건조하는 공정으로 이루어진 것을 특징으로 하는 테레프탈산의 제조방법.In the method of producing terephthalic acid by hydrolyzing and crystallizing polyethylene terephthalate, a) the waste polyethylene terephthalate is hydrolyzed by alkali metal hydroxide / earth metal in the presence of water solvent and infiltration agent to form alkali metal / earth metal salt of terephthalate Process; b) solid solution is separated by solid-liquid separation of aqueous solution obtained by dissolving alkali metal / earth metal salt of terephthalic acid in water, and a) is fed back to the hydrolysis process, and the liquid is transferred to the next adsorption process. Process; c) adsorbing an aqueous solution of an alkali metal / earth metal salt of terephthalic acid and neutralizing it with an acid to obtain terephthalic acid; d) a crystallization process for enlarging terephthalic acid; e) cooling the enlarged terephthalic acid under reduced pressure, and filtering and drying. Method for producing terephthalic acid, characterized in that made. 제 1 항에 있어서, 상기 가)가수분해 공정에서 폐 폴리에틸렌 테레프탈레이트로는 폐 폴리에스터 섬유, 폐 폴리에틸렌 테페프탈레이트 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 waste polyethylene terephthalate of claim 1, wherein in the hydrolysis process, waste polyethylene terephthalate comprises waste polyester fibers, waste polyethylene terephthalate bottles, waste polyethylene terephthalate containers, waste polyethylene terephthalate chips generated during polymerization of polyethylene terephthalate, Or waste polyester yarn (에서) generated during the polyester fiber manufacturing process characterized in that the production method of terephthalic acid. 제 1 항 또는 제 2 항에 있어서, 상기 폐폴리에틸렌 테레프탈레이트는 전체 가수분해 반응물 중에 1～25 중량% 첨가하는 것을 특징으로 하는 테레프탈산의 제조 및 회수방법.The method for producing and recovering 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 hydrolyzate. 제 1 항에 있어서, 상기 수산화알칼리금속/토금속은 전체 가수분해 반응물 중에 5～30 중량% 함유시키는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 1, wherein the alkali metal hydroxide / earth metal is contained in an amount of 5 to 30% by weight in the total hydrolysis reaction product. 제 1 항에 있어서, 상기 침윤제는 전체 가수분해 반응물 중에 1～30 중량% 첨가하는 것을 특징으로 하는 테레프탈산의 제조방법.The method 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)가수분해 공정은 30～200 ℃ 반응온도 및 1～20 kg/㎠ 반응압력하에서 진행되는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing 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 알칼리금속/토금속염에 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 alkali metal / earth metal salt of terephthalic acid. 제 1 항에 있어서, 상기 라)결정화공정은 1～5개의 결정화조가 직렬로 연결되어 있고 각 단계별 결정화조의 온도가 30～50 ℃씩 감소되도록 설치되어 있는 결정화조내에서 진행하는 것을 특징으로 하는 테레프탈산의 제조방법.2. The crystallization process 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. Method for producing terephthalic acid. 제 8 항에 있어서, 상기 결정화조는 120～300 ℃ 온도 및 2～86 kg/㎠ 압력이 유지되도록 하는 것을 특징으로 하는 테레프탈산의 제조방법.The method of claim 8, wherein the crystallization tank maintains 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 0.1～1.0 kg/㎠ 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 10 항에 있어서, 상기 마)냉각공정에서 배출되는 알코올과 물은 상기 가)가수분해 공정으로 피드백(feed back)되는 것을 특징으로 하는 테레프탈산의 제조방법.The method for producing terephthalic acid according to claim 1 or 10, wherein the alcohol and water discharged from the cooling process are fed back to the hydrolysis process. 제 1항에 있어서, 상기 마)여과공정에서 배출되는 여과액은 바이포라 막을 이용한 전기투석장치(electro-dialyzer)에 투입되어 산(acid)과 수산화알칼리금속/토금속으로 분리되며, 산(acid)은 상기의 다)중화공정으로 피드백(feed back)되고, 수산화알칼리금속/토금속은 상기의 가)가수분해 공정으로 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 biphora membrane is separated into acid and alkali metal hydroxide / earth metal, acid (acid) Is fed back to the above poly) neutralization process, and the alkali metal hydroxide / earth metal is fed back to the above-mentioned hydrolysis process of terephthalic acid. 폐 폴리에틸렌 테레프탈레이트를 원료물질로하여 테레프탈산을 제조하는 장치에 있어서, 상기 폐폴리에틸렌 테레프탈레이트가 테레프탈산 알칼리금속/토금속염으로 가수분해되는 가수분해장치(1), 테레프탈산 알칼리금속/토금속염을 용해하는 용해장치(2), 원심분리기(3), 흡착탑(4), 테레프탈산 알칼리금속/토금속염을 산(acid)으로 중화하여 테레프탈산을 생성하는 중화장치(5), 테레프탈산 입자를 비대화하는 결정화장치(6), 냉각장치(7), 비대화된 테레프탈산을 여과하는 여과장치(8), 여과된 테레프탈산을 건조하는 건조장치(9)가 연속적으로 설치되어 있는 것을 특징으로 하는 테레프탈산 제조 장치.In a device for producing terephthalic acid using waste polyethylene terephthalate as a raw material, a hydrolysis device (1) in which the waste polyethylene terephthalate is hydrolyzed to an alkali metal / earth metal salt of terephthalate, and a solution for dissolving terephthalate alkali metal / earth metal salt Apparatus (2), centrifuge (3), adsorption tower (4), neutralizer (5) for producing terephthalic acid by neutralizing alkali metal / earth metal salts of terephthalic acid, crystallization apparatus (6) for enlarging terephthalic acid particles And a cooling device (7), a filtration device (8) for filtering the enlarged terephthalic acid, and a drying device (9) for drying the filtered terephthalic acid.
KR1019950056785A 1995-12-26 1995-12-26 Process for producing terephthalic acid(1) KR100224466B1 (en)

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Cited By (3)

* 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
KR20240033639A (en) 2022-09-05 2024-03-12 에스케이케미칼 주식회사 Preparation method of terephthalic acid and terephthalic acid prepared therefrom
KR20240033640A (en) 2022-09-05 2024-03-12 에스케이케미칼 주식회사 Preparation method of terephthalic acid and terephthalic acid prepared therefrom

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102278269B1 (en) 2019-02-12 2021-07-20 한국화학연구원 BIOMASS-DERIVED SiO₂ CATALYST FOR TPA HYDROLYSIS OF PET, MANUFACTURING THEREOF, AND TPA HYDROLYSIS OF PET USING THE CATALIST

Cited By (3)

* 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
KR20240033639A (en) 2022-09-05 2024-03-12 에스케이케미칼 주식회사 Preparation method of terephthalic acid and terephthalic acid prepared therefrom
KR20240033640A (en) 2022-09-05 2024-03-12 에스케이케미칼 주식회사 Preparation method of terephthalic acid and terephthalic acid prepared therefrom

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