KR930702555A - Process for preparing halogenated acrylic acid - Google Patents

Process for preparing halogenated acrylic acid

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Publication number
KR930702555A
KR930702555A KR1019930700768A KR930700768A KR930702555A KR 930702555 A KR930702555 A KR 930702555A KR 1019930700768 A KR1019930700768 A KR 1019930700768A KR 930700768 A KR930700768 A KR 930700768A KR 930702555 A KR930702555 A KR 930702555A
Authority
KR
South Korea
Prior art keywords
electrolyte
cell
compound
formula
undivided
Prior art date
Application number
KR1019930700768A
Other languages
Korean (ko)
Inventor
답퍼헬트 슈테펜
호이뮐러 루돌프
울름슈나이더 디이터
빌트 만프레트
Original Assignee
귀트라인, 슈미트
훽스트 아크티엔게젤샤프트
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by 귀트라인, 슈미트, 훽스트 아크티엔게젤샤프트 filed Critical 귀트라인, 슈미트
Publication of KR930702555A publication Critical patent/KR930702555A/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/20—Processes
    • C25B3/25—Reduction
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/065—Carbon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/02—Process control or regulation
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B3/00—Electrolytic production of organic compounds
    • C25B3/20—Processes
    • C25B3/23—Oxidation

Abstract

본 발명은 일반식(Ⅱ)의 화합물 또는 일반식(Ⅲ)의 화합물을 -10℃ 내지 전해질 액체의 비점 온도에서, pH6이하 및 전류밀도 10내지 500mA/㎠에서, 전해질중 1내지 5000ppm 농도의 철 염의 존재하에, -분할되지 않은 셀중 전해질 또는 분할된 셀중 음극액(음극은 탄소로 구성됨)의 총량을 각각의 경우에서 기준으로 하여-, 중수 또는 물 0내지 100중량% 및 하나 이상의 유기 용매 100내지 0중량%로 이루어진 전기분해액중 분할된 또는 분할되지 않은 셀중에서 전해분해시킴을 특징으로 하는 전기분해 환원에 의해 일반식(Ⅰ)의 화합물을 제조하는 방법에 관한 것이다.The present invention provides a compound of formula (II) or a compound of formula (III) at -10 ° C. to a boiling point temperature of the electrolyte liquid, at a pH of 6 or less and a current density of 10 to 500 mA / cm 2, in a concentration of 1 to 5000 ppm in the electrolyte. In the presence of salts-from 0 to 100% by weight of heavy water or water and from 100 to at least one organic solvent-based on the total amount of the electrolyte in the undivided cell or the catholyte in the divided cell (the cathode consists of carbon) in each case. The present invention relates to a method for preparing a compound of formula (I) by electrolytic reduction, characterized in that it is electrolyzed in divided or undivided cells in an electrolysis solution consisting of 0% by weight.

상기식에서, R1은 불소 원자 또는 메틸 또는 듀테로메틸 그룹이고, R2및 R3은 동일하거나 상이하며 불소, 염소, 수소 또는 중수소 원자이며 R4는그룹이고, R5는 -OH, OD, C1-C4-알콕시 또는 -OMe(여기서, Me는 알칼리 금속, 알칼리 토금속 또는 NH4이온이다)이며, R6은 염소원자이다.Wherein R 1 is a fluorine atom or a methyl or deuteromethyl group, R 2 and R 3 are the same or different and fluorine, chlorine, hydrogen or deuterium atoms and R 4 is And R 5 is —OH, OD, C 1 -C 4 -alkoxy or —OMe, where Me is an alkali metal, alkaline earth metal or NH 4 ion, and R 6 is a chlorine atom.

Description

할로겐화된 아크릴산의 제조방법Process for preparing halogenated acrylic acid

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

Claims (13)

일반식(Ⅱ)의 화합물 또는 일반식(Ⅲ)의 화합물을 -10℃ 내지 전해질액의 비점에서, pH 6이하 및 전류밀도 10내지 500mA/㎤에서, 전해질중 1내지 5000ppm 농도의 철염의 존재하에, -분할되지 않은 셀중 전해질 또는 분할된 셀중 음극액(음극은 탄소로 구성됨)의 총량을 각각의 경우에서 기본으로 하여- 중수 또는 물 0내지 100중량% 및 하나 이상의 유기 용매 100내지 0중량%로 이루어진 전해분해액중 분할된 또는 분할되지 않은 셀중에서 전기분해시킴을 특징으로 하는 전기분해 환원에 의해 일반식(Ⅰ)의 화합물을 제조하는 방법.The compound of formula (II) or compound of formula (III) was reacted in the presence of 1 to 5000 ppm of iron salt in the electrolyte at a pH of 6 to 10 and a current density of 10 to 500 mA / cm 3 at a boiling point of -10 ° C to the electrolyte solution. -Based on the total amount of electrolyte in the undivided cell or catholyte in the divided cell (the cathode consists of carbon) in each case-from 0 to 100% by weight of heavy water or water and from 100 to 0% by weight of one or more organic solvents. A process for preparing a compound of formula (I) by electrolytic reduction, characterized in that it is electrolyzed in cells which have been divided or undivided in the resulting electrolytic solution. 상기식에서, R1은 불소 원자 또는 메틸 또는 듀테로메틸 그룹이고, R2및 R3은 동일하거나 상이하며 불소, 염소, 수소 또는 중수소 원자이며 R4는그룹이고, R5는 -OH, OD, C1-C4-알콕시 또는 -OMe(여기서, Me는 알칼리 금속, 알칼리 토금속 또는 NH4이온이다)이며, R6은 염소원자이다.Wherein R 1 is a fluorine atom or a methyl or deuteromethyl group, R 2 and R 3 are the same or different and fluorine, chlorine, hydrogen or deuterium atoms and R 4 is And R 5 is —OH, OD, C 1 -C 4 -alkoxy or —OMe, where Me is an alkali metal, alkaline earth metal or NH 4 ion, and R 6 is a chlorine atom. 제1항에 있어서, R1이 불소 원자이고 R2및 R3가 염소, 수소 또는 중수소 원자인 방법.The method of claim 1 wherein R 1 is a fluorine atom and R 2 and R 3 are chlorine, hydrogen or deuterium atoms. 제1항에 있어서, 분할되지 않은 셀중 전해액 또는 분할된 셀중 음극액중의 서로 나란히 둘다 산화상태 +2 또는 +3으로 존재하는 방법.The method according to claim 1, wherein both of the electrolyte in the undivided cell or the catholyte in the divided cell are present in the oxidation state +2 or +3. 제1항에 있어서, 전기분해를 바람직하게는 20내지 400mA/㎤의 전류밀도, 특히 50내지 300mA/㎤의 전해밀도에서 수행하는 방법.The process according to claim 1, wherein the electrolysis is carried out preferably at a current density of 20 to 400 mA / cm 3, in particular at an electrolytic density of 50 to 300 mA / cm 3. 제1항에 있어서, 전기분해를 0내지 25V 이상의 수소 과전압(전류 밀도 300A/㎤를 기준으로 함)을 갖는 금속의 염의 존재하에 수행하는 방법.The process of claim 1 wherein the electrolysis is carried out in the presence of a salt of a metal having a hydrogen overvoltage (based on a current density of 300 A / cm 3) of 0 to 25 V or more. 제5항에 있어서, 분할되지 않는 셀중 전해질 또는 분할된 셀중 음극액에 사용되는 금속 염이 구리, 아연, 카드뮴, 주석, 납 또는 비스무트의 가용성 염인 방법.The method of claim 5, wherein the metal salt used in the electrolyte in the undivided cell or the catholyte in the divided cell is a soluble salt of copper, zinc, cadmium, tin, lead or bismuth. 제6항에 있어서, 분할되지 않는 셀중 전해질 또는 분할된 셀중 음극액에 사용되는 금속이 가용성 납염인 방법.The method of claim 6, wherein the metal used in the electrolyte in the undivided cell or the catholyte in the divided cell is soluble lead salt. 제5항에 있어서, 금속염의 농도가 0.1내지 5000ppm, 바람직하게는 10내지 3000ppm의 범위인 방법.The method according to claim 5, wherein the concentration of the metal salt is in the range of 0.1 to 5000 ppm, preferably 10 to 3000 ppm. 제1항에 있어서, 전기분해를 10내지 90℃, 바람직하게는 15내지 80℃에서 수행하는 방법.The process according to claim 1, wherein the electrolysis is carried out at 10 to 90 ° C., preferably at 15 to 80 ° C. 7. 제1항에 있어서, 전기분해를 불연속 음극 반응 및 연속 양극 반응을 사용하는 분할 셀에서 수행하는 방법.The process of claim 1 wherein the electrolysis is carried out in a split cell using discontinuous cathode reactions and continuous anode reactions. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019930700768A 1990-09-13 1991-09-12 Process for preparing halogenated acrylic acid KR930702555A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4029068A DE4029068A1 (en) 1990-09-13 1990-09-13 METHOD FOR PRODUCING HALOGENATED ACRYLIC ACIDS
DEP4029068.9 1990-09-13
PCT/EP1991/001738 WO1992005299A1 (en) 1990-09-13 1991-09-12 Process for producing halogenated acrylic acids

Publications (1)

Publication Number Publication Date
KR930702555A true KR930702555A (en) 1993-09-09

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ID=6414186

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1019930700768A KR930702555A (en) 1990-09-13 1991-09-12 Process for preparing halogenated acrylic acid

Country Status (6)

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EP (1) EP0548141A1 (en)
JP (1) JPH05506273A (en)
KR (1) KR930702555A (en)
CA (1) CA2092693A1 (en)
DE (1) DE4029068A1 (en)
WO (1) WO1992005299A1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110438523B (en) * 2019-09-05 2021-12-03 南京大学 Catalyst-free electrochemical deuteration method taking heavy water as deuterium source
EP4253603A1 (en) * 2022-03-28 2023-10-04 Evonik Operations GmbH Electrochemical oxidation of cycloalkanes to cycloalkanone compounds
EP4253602A1 (en) * 2022-03-28 2023-10-04 Evonik Operations GmbH Electrochemical oxidation of cycloalkenes and cycloalkanes to alpha, omega-dicarboxylic acids or ketocarboxylic acids and cycloalkanone compounds
EP4253605A1 (en) * 2022-03-28 2023-10-04 Evonik Operations GmbH Electrochemical oxidation of cycloalkenes to alpha, omega-dicarboxylic acids and ketocarboxylic acids
EP4253604A1 (en) * 2022-03-28 2023-10-04 Evonik Operations GmbH Electrochemical oxidation of fatty acids and fatty acid esters to monocarboxylic acids and alpha, omega-dicarboxylic acids

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL63449C (en) * 1942-03-12
US4482437A (en) * 1984-04-05 1984-11-13 Reilly Tar & Chemical Corp. Electrochemical reductions of cyanopyridine bases
DE3731914A1 (en) * 1987-09-23 1989-04-06 Hoechst Ag METHOD FOR THE PRODUCTION OF FLUORINATED ACRYLIC ACIDS AND THEIR DERIVATIVES

Also Published As

Publication number Publication date
JPH05506273A (en) 1993-09-16
EP0548141A1 (en) 1993-06-30
CA2092693A1 (en) 1992-03-14
DE4029068A1 (en) 1992-03-19
WO1992005299A1 (en) 1992-04-02

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