JPWO2022083396A5 - - Google Patents

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JPWO2022083396A5
JPWO2022083396A5 JP2022576527A JP2022576527A JPWO2022083396A5 JP WO2022083396 A5 JPWO2022083396 A5 JP WO2022083396A5 JP 2022576527 A JP2022576527 A JP 2022576527A JP 2022576527 A JP2022576527 A JP 2022576527A JP WO2022083396 A5 JPWO2022083396 A5 JP WO2022083396A5
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column
ethyl acetate
acetic acid
tower
extraction rectification
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JP2023531171A (en
JP7486847B2 (en
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Priority claimed from CN202011127390.0A external-priority patent/CN112209830B/en
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酢酸ビニル合成プロセスと、酢酸ビニル精製プロセスと、酢酸ビニルと酢酸エチルの分離プロセスとを含み、前記酢酸ビニル合成プロセスは、主に順次接続されたエチレン回収塔(117)、酢酸蒸発器(103)、酸素混合器(106)、酢酸ビニル合成反応器(107)、第1ガス分離塔(108)、第2ガス分離塔(112)及び循環ガス圧縮機(101)から成り、前記第1ガス分離塔(108)及び前記第2ガス分離塔(112)は脱気缶(113)に接続されてから回収ガス圧縮機(114)、水洗塔(115)、吸収塔(116)、脱着塔(122)に順次接続され、前記酢酸ビニル精製プロセスは、主に順次接続された酢酸塔(201)、粗VAC塔(202)、精製VAC塔(203)、前記粗VAC塔(202)の塔頂の1つの分岐に順次接続されたアルデヒドエステル濃縮塔(204)及びアセトアルデヒド塔(205)、前記酢酸塔(201)と前記粗VAC塔(202)の塔頂の1つの分岐に順次接続された水相受槽(207)と脱水塔(206)から成り、前記酢酸ビニルと酢酸エチルの分離プロセスは、主に順次接続された抽出精留塔(401)、抽出精留塔凝縮器(402)、抽出精留塔サブクーラー(403)、抽出精留塔相分離器(404)、及び前記抽出精留塔(401)釜が順次接続する酢酸エチル塔(405)、酢酸エチル塔凝縮器(406)、酢酸エチル塔サブクーラー(407)、酢酸エチル塔相分離器(408)から成るエチレンアセタートの製造方法であって、前記酢酸ビニルと酢酸エチルの分離プロセスは、抽出精留法を用い
前記酢酸塔(201)の側線から抜き出された酢酸、酢酸ビニル、水及び酢酸エチルを含むストリームは、前記抽出精留塔(401)の中部に入り、酢酸を抽出剤として前記抽出精留塔(401)の上部から仕込み、前記抽出精留塔(401)の塔頂蒸気内の主成分は、酢酸ビニルと水、きれいに除去していない微量の酢酸エチルであり、前記抽出精留塔凝縮器(402)で凝縮して得られた凝縮液が前記抽出精留塔サブクーラー(403)に入り、さらに冷却された後前記抽出精留塔相分離器(404)に送り込まれて相分離を行い、相分離後の油相部分が還流され、残り部分が抜き出されて前システムの前記酢酸塔(201)に送られて処理され、水相が前記脱水塔(206)に送られて水相中の有機物を回収することを特徴とする、方法。
It includes a vinyl acetate synthesis process, a vinyl acetate purification process, and a separation process of vinyl acetate and ethyl acetate, and the vinyl acetate synthesis process mainly consists of an ethylene recovery column (117) and an acetic acid evaporator (103) connected in sequence. , an oxygen mixer (106), a vinyl acetate synthesis reactor (107), a first gas separation column (108), a second gas separation column (112) and a circulating gas compressor (101), and the first gas separation The column (108) and the second gas separation column (112) are connected to a degassing can (113), and then connected to a recovery gas compressor (114), a water washing column (115), an absorption column (116), and a desorption column (122). ), and the vinyl acetate purification process mainly consists of an acetic acid tower (201), a crude VAC tower (202), a purified VAC tower (203), and the top of the crude VAC tower (202), which are connected in sequence. an aldehyde ester concentration column (204) and an acetaldehyde column (205) sequentially connected to one branch; an aqueous phase sequentially connected to one branch at the top of the acetic acid column (201) and the crude VAC column (202); It consists of a receiving tank (207) and a dehydration tower (206), and the separation process of vinyl acetate and ethyl acetate is mainly performed by an extraction rectification tower (401), an extraction rectification tower condenser (402), and an extraction rectification tower (402), which are connected in sequence. A distillation column subcooler (403), an extraction rectification column phase separator (404), and an ethyl acetate column (405) to which the extraction rectification column (401) vessel is connected in sequence, an ethyl acetate column condenser (406), and an acetic acid column. A method for producing ethylene acetate comprising an ethyl tower subcooler (407) and an ethyl acetate tower phase separator (408), the separation process of vinyl acetate and ethyl acetate using an extractive rectification method ,
A stream containing acetic acid, vinyl acetate, water and ethyl acetate extracted from the side line of the acetic acid tower (201) enters the middle of the extraction rectification tower (401), and is passed through the extraction rectification tower using acetic acid as an extractant. (401), and the main components in the top vapor of the extraction rectification column (401) are vinyl acetate, water, and a trace amount of ethyl acetate that has not been completely removed. The condensate obtained by condensation in (402) enters the extraction rectification column subcooler (403), and after being further cooled, it is sent to the extraction rectification column phase separator (404) for phase separation. After phase separation, the oil phase portion is refluxed, the remaining portion is extracted and sent to the acetic acid tower (201) of the previous system for treatment, and the aqueous phase is sent to the dehydration tower (206) to form an aqueous phase. A method characterized by recovering organic matter therein .
前記酢酸ビニルと酢酸エチルの分離プロセスは、抽出精留法を用い、主要設備は前記抽出精留塔(401)と、前記酢酸エチル塔(405)と前記抽出精留塔凝縮器(402)と、前記抽出精留塔サブクーラー(403)と、前記抽出精留塔相分離器(404)と、前記酢酸エチル塔凝縮器(406)と、前記酢酸エチル塔サブクーラー(407)と、前記酢酸エチル塔相分離器(408)とを備え、前記抽出精留塔(401)の塔頂部は、前記抽出精留塔凝縮器(402)、前記抽出精留塔サブクーラー(403)、前記抽出精留塔相分離器(404)に順次接続され、前記抽出精留塔相分離器(404)の油相出口に2つの分岐が設けられ、各々前記抽出精留塔(401)及び前システムの前記酢酸塔(201)に戻され、水相出口が前記水相受槽(207)に接続され、前記抽出精留塔(401)の塔釜は、前記酢酸エチル塔(405)に接続され、前記酢酸エチル塔(405)の塔頂部が前記酢酸エチル塔凝縮器(406)、前記酢酸エチル塔サブクーラー(407)及び前記酢酸エチル塔相分離器(408)に順次接続され、前記酢酸エチル塔相分離器(408)の水相出口が前記酢酸エチル塔(405)に接続され、油相出口の原材料がシステムから送り出され、前記酢酸エチル塔(405)の塔釜出口に2つの分岐が設けられ、各々抽出精留塔及び前システムの前記酢酸塔(201)に接続されることを特徴とする、請求項1に記載の方法。 The separation process of vinyl acetate and ethyl acetate uses an extraction rectification method, and the main equipment includes the extraction rectification column (401), the ethyl acetate column (405), and the extraction rectification column condenser (402). , the extraction rectification column subcooler (403), the extraction rectification column phase separator (404), the ethyl acetate column condenser (406), the ethyl acetate column subcooler (407), the acetic acid an ethyl column phase separator (408); Two branches are provided at the oil phase outlet of the extraction rectification column phase separator (404), which are sequentially connected to the distillation column phase separator (404), and are respectively connected to the extraction rectification column (401) and the oil phase outlet of the extraction rectification column phase separator (404). The acetic acid is returned to the acetic acid column (201), and the aqueous phase outlet is connected to the aqueous phase receiving tank (207), and the column kettle of the extraction rectification column (401) is connected to the ethyl acetate column (405). The top of the ethyl column (405) is connected in sequence to the ethyl acetate column condenser (406), the ethyl acetate column subcooler (407) and the ethyl acetate column phase separator (408), and the ethyl acetate column phase separation The aqueous phase outlet of the vessel (408) is connected to the ethyl acetate column (405), the raw material at the oil phase outlet is sent out from the system, and two branches are provided at the column outlet of the ethyl acetate column (405), 2. The method according to claim 1, characterized in that it is connected to an extraction rectification column and the acetic acid column (201) of the pre-system, respectively . 前記抽出精留塔(401)の塔釜には、酢酸エチル、少量の水と酢酸の混合物が含まれ、前記酢酸エチル塔(405)に入れられ精留され、前記酢酸エチル塔(405)の塔頂蒸気の主成分が酢酸エチルと水、微量の酢酸ビニルであり、前記酢酸エチル塔凝縮器(406)で凝縮して得られた凝縮液が前記酢酸エチル塔サブクーラー(407)に入れられ、されに冷却された後で前記酢酸エチル塔相分離器(408)に送り込まれて相分離を行い、相分離後の水相は還流され、油相が酢酸エチル不純物ストリームとしてシステムから排出され、前記酢酸エチル塔(405)の塔釜の主成分は、酢酸で、一部が前記抽出精留塔(401)に戻されて抽出剤となり、残りは前システムの前記酢酸塔(201)に戻されて仕込むことを特徴とする、請求項に記載の方法。 The column kettle of the extraction rectification column (401) contains ethyl acetate, a mixture of a small amount of water and acetic acid, which is put into the ethyl acetate column (405) and rectified, and is then collected in the ethyl acetate column (405). The main components of the tower top vapor are ethyl acetate, water, and a trace amount of vinyl acetate, and the condensate obtained by condensing in the ethyl acetate tower condenser (406) is put into the ethyl acetate tower subcooler (407). , after being cooled, it is sent to the ethyl acetate column phase separator (408) to perform phase separation, the aqueous phase after phase separation is refluxed, and the oil phase is discharged from the system as an ethyl acetate impurity stream; The main component of the column of the ethyl acetate column (405) is acetic acid, a portion of which is returned to the extraction rectification column (401) to become an extractant, and the remainder is returned to the acetic acid column (201) of the previous system. 3. The method according to claim 2 , characterized in that the method is prepared by: 抽出精留法による前記酢酸ビニルと酢酸エチルの分離プロセスでは、酢酸を抽出剤として用い、抽出剤は前記抽出精留塔(401)の上部から加えられることを特徴とする、請求項1に記載の方法。 According to claim 1, in the separation process of vinyl acetate and ethyl acetate by the extractive rectification method, acetic acid is used as an extractant, and the extractant is added from the upper part of the extractive rectification column (401). the method of. 抽出剤の酢酸の質量流量と前記酢酸塔(201)の側線から抜き出された仕込みの質量流量の比率は、0.2~2:1であることを特徴とする、請求項4に記載の方法。 5. The method according to claim 4, wherein the ratio of the mass flow rate of the extractant acetic acid to the mass flow rate of the charge extracted from the side line of the acetic acid column (201) is 0.2 to 2:1. Method. 抽出剤の酢酸の質量流量と前記酢酸塔(201)の側線から抜き出された仕込みの質量流量の比率は、1.2:1であることを特徴とする、請求項に記載の方法。 6. Process according to claim 5 , characterized in that the ratio of the mass flow rate of the extractant acetic acid to the mass flow rate of the charge withdrawn from the side line of the acetic acid column (201) is 1.2:1.
JP2022576527A 2020-10-20 2021-09-23 Method for producing ethylene acetate Active JP7486847B2 (en)

Applications Claiming Priority (3)

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CN202011127390.0A CN112209830B (en) 2020-10-20 2020-10-20 Method for producing vinyl acetate
CN202011127390.0 2020-10-20
PCT/CN2021/119874 WO2022083396A1 (en) 2020-10-20 2021-09-23 Method for producing vinyl acetate

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JP2023531171A JP2023531171A (en) 2023-07-21
JPWO2022083396A5 true JPWO2022083396A5 (en) 2023-10-03
JP7486847B2 JP7486847B2 (en) 2024-05-20

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Publication number Priority date Publication date Assignee Title
CN112299989B (en) * 2020-10-20 2021-08-31 天津大学 Vinyl acetate production process and device
CN112209830B (en) 2020-10-20 2021-08-27 天津大学 Method for producing vinyl acetate
CN113861026B (en) * 2021-10-29 2022-09-06 天津大学 Refining method of vinyl acetate and acetic acid synthesized by acetylene method
CN115745794B (en) * 2022-11-16 2023-06-20 天津大学 Ethylene process and apparatus for producing vinyl acetate
CN116924877A (en) * 2023-07-26 2023-10-24 天津大学 Process and device for refining recycle gas in vinyl acetate synthesis process

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US3905875A (en) * 1968-05-10 1975-09-16 Bayer Ag Process for the purification of crude liquid vinyl acetate
US3616271A (en) * 1968-10-25 1971-10-26 Du Pont Separation of chloroform and/or ethyl acetate from vinyl acetate by extractive distillation
GB1305367A (en) * 1970-07-01 1973-01-31
US4897161A (en) * 1989-03-20 1990-01-30 Lloyd Berg Separation of vinyl acetate from ethyl acetate by extractive distillation
DE102004053184B4 (en) * 2004-11-04 2013-12-12 Celanese Chemicals Europe Gmbh Process for saturating ethylene-containing gases with acetic acid
DE102006038689B4 (en) * 2006-08-17 2015-01-22 Celanese Chemicals Europe Gmbh Process for working up vinyl acetate
EP2890670B1 (en) * 2012-08-30 2016-09-21 Celanese International Corporation Process for vinyl acetate production having sidecar reactor for predehydrating column
CN102936198B (en) * 2012-10-12 2016-05-25 天津大学 Produce the method for vinyl acetate
CN112209830B (en) * 2020-10-20 2021-08-27 天津大学 Method for producing vinyl acetate

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