IPC분류정보
국가/구분 |
United States(US) Patent
등록
|
국제특허분류(IPC7판) |
|
출원번호 |
US-0181460
(2001-01-24)
|
우선권정보 |
DE-0002793 (2000-01-24) |
국제출원번호 |
PCT/EP01/00749
(2002-07-18)
|
§371/§102 date |
20020718
(20020718)
|
국제공개번호 |
WO01/55071
(2001-08-02)
|
발명자
/ 주소 |
- Auer, Heinz
- Bessling, Bernd
- Hammer, Hans
- Hasse, Hans
- Sauer, Friedrich
- Vicari, Maximilian
- Wagner, Gerhard
- Adrian, Till
|
출원인 / 주소 |
|
대리인 / 주소 |
|
인용정보 |
피인용 횟수 :
1 인용 특허 :
2 |
초록
▼
The invention relates to a process for obtaining anhydrous or substantially anhydrous formic acid in which, during the work-up, a compound of the general formula I where the radicals R1 and R2 are alkyl, cycloalkyl, aryl or aralkyl groups, or R1 and R2 jointly, together with the N atom, form a heter
The invention relates to a process for obtaining anhydrous or substantially anhydrous formic acid in which, during the work-up, a compound of the general formula I where the radicals R1 and R2 are alkyl, cycloalkyl, aryl or aralkyl groups, or R1 and R2 jointly, together with the N atom, form a heterocyclic 5- or 6-membered ring, and only one of the radicals is an aryl group, and where R3 is hydrogen or a C1-C4-alkyl group,is employed simultaneously as extractant for formic acid and as antifoam for a distillation process.
대표청구항
▼
1. A process for obtaining anhydrous or substantially anhydrous formic acid, in whichi) methyl formate is subjected to hydrolysis, ii) methanol and excess methyl formate are distilled off from the resultant hydrolysis mixture, iii) the bottom product from distillation (ii), comprising formic acid an
1. A process for obtaining anhydrous or substantially anhydrous formic acid, in whichi) methyl formate is subjected to hydrolysis, ii) methanol and excess methyl formate are distilled off from the resultant hydrolysis mixture, iii) the bottom product from distillation (ii), comprising formic acid and water, is extracted in a liquid?liquid extraction with an extractant which principally takes up the formic acid, and the extractant employed here is a carboxamide of the general formula I ?where the radicals R1 and R2 are alkyl, cycloalkyl, aryl or aralkyl groups, or R1 and R2 jointly, together with the N atom, form a heterocyclic 5- or 6-membered ring, and only one of the radicals is an aryl group, and where R3 is hydrogen or a C1-C4-alkyl group, iv) the resultant extract phase, comprising formic acid, extractant and some water, is subjected to distillation, v) the top product obtained in this distillation, which comprises water and some of the formic acid, is fed back into the lower part of the distillation device in step ii), vi) the bottom product from distillation step iv), which comprises predominantly extractant and formic acid, is separated by distillation into anhydrous or substantially anhydrous formic acid and the extractant, and vii) the extractant leaving step vi) is fed back into the process, which comprises removing a sub-stream of the extractant employed from the process and feeding it to the distillation device provided for carrying out step ii), with the corresponding feed point for the sub-stream of the extractant in the distillation device being above the feed point of the hydrolysis mixture and below the removal point of methanol. 2. The process claimed in claim 1, wherein the extractant employed is at least one compound selected from the group consisting of N,N-di-n-butylformamide, N,N-di-n-butylacetamide, N-methyl-N-2-heptylformamide, N-n-butyl-N-2-ethylhexylformamide, N-n-butyl-N-cyclohexylformamide and N-ethylformanilide.3. The process claimed in claim 1, wherein the sub-stream of the extractant employed is taken from the extractant leaving step vi).4. The process claimed in claim 1, wherein distillation steps ii) and iv) are carried out in a single distillation device.5. A method for preventing foam in a distillation of a hydrolysis mixture comprising methyl formate, water, formic acid and methanol in a distillation device in a process according to claim 1 which comprises feeding to the distillation device a separate stream consisting essentially of a carboxyamide of formula I where the radicals R1 and R2 are alkyl, cycloalkyl, aryl or aralkyl groups, or R1 and R2 jointly, together with the N atom, form a heterocyclic 5- or 6-membered ring, and only one of the radicals is an aryl group, and where R3 is hydrogen or a C1-C4-alkyl group. 6. The process claimed in claim 1, wherein the sub-stream of extractant is cooled before being fed to the distillation device provided for carrying out step ii).
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