Claims
- 1. In a method of preparing a gamma-butyrolactone by reacting, in liquid acetic acid contained in a reaction zone, a minor fraction of said acetic acid with an aliphatic olefin that has an empirical formula C.sub.n H.sub.2n in which n is from 3 to 92 and a stoichiometric amount of an ion of manganese in higher-valent form, to form in said reaction zone a mixture comprising said gamma-butyrolactone, an ion of manganese in lower-valent form and a major fraction of said acetic acid, the improvement in the recovery of said gamma-butyrolactone comprising the steps of:
- passing to a recovery zone said mixture comprising said gamma-butyrolactone, an ion of manganese in lower-valent form and a major fraction of said acetic acid;
- treating said mixture with sufficient lactone solvent to effect separation into two streams, the first stream comprising said gamma-butyrolactone substantially free of said ion of manganese in lower-valent form, the second stream comprising said ion of manganese in lower-valent form and said major fraction of acetic acid substantially free of said gamma-butyrolactone;
- recovering said gamma-butrolactone from said first stream;
- converting, in said second stream, said ion of manganese in lower-valent form to higher-valent form;
- and recovering from said second stream a mixture, reusable in said reaction zone, consisting essentially of said major fraction of acetic acid and said ion of manganese in higher-valent form.
- 2. The process of claim 1 wherein said treating to effect separation into two streams comprises solvent-extracting said mixture with said lactone solvent.
- 3. In a method of preparing a gamma-butyrolactone by reacting, in liquid acetic acid contained in a reaction zone, a minor fraction of said acetic acid with an aliphatic olefin that has an empirical formula C.sub.n H.sub.2n in which n is from 3 to 92 and a stoichiometric amount of an ion of manganese in higher-valent form, to form in said reaction zone a mixture comprising said gamma-butyrolactone, an ion of manganese in lower-valent form and a major fraction of said acetic acid, the improvement in the recovery of said gamma-butyrolacetone comprising the steps of:
- passing to a recovery zone said mixture comprising said gamma-butyrolactone, an ion of manganese in lower-valent form and a major fraction of said acetic acid;
- treating said mixture with both a lactone solvent and a lactone non-solvent in quantities sufficient to effect separation into two streams, the first stream comprising said gamma-butyrolactone substantially free of said ion of manganese in low-valent form, the second stream comprising said ion of manganese in lower-valent form and said major fraction of acetic acid substantially free of said gamma-butyrolactone;
- recovering said gamma-butyrolactone from said first stream;
- converting, in said second stream, said ion of manganese in lower-valent form to higher-valent form;
- and recovering from said second stream a mixture, reusable in said reaction zone, consisting essentially of said major fraction of acetic acid and said ion of manganese in higher-valent form.
- 4. The process of claim 3 wherein said treatment comprises diluting said mixture with lactone non-solvent followed by solvent extraction of the diluted mixture.
- 5. The process of claim 4 in which the lactone non-solvent is water and the lactone solvent is a hydrocarbon.
- 6. The process of claim 3 in which said treating comprises adding to said mixture both a lactone solvent and water in quantities sufficient to effect stratification into an upper layer comprising said gamma-butyrolactone substantially free of said ion of manganese in lower-valent form, and a lower layer comprising said ion of manganese in said lower-valent form and said major fraction of acetic acid, and withdrawing the upper layer as a first stream and the lower layer as a second stream.
- 7. The process of claim 6 in which said lactone solvent is a hydrocarbon.
- 8. The process of claim 7 in which the hydrocarbon is the same olefin composition as that used to form the gamma-butyrolactone.
- 9. The process of claim 3 in which said converting, in said second stream, of said ion of manganese in lower-valent form to higher-valent form is done by reacting the lower-valent ion with ozone.
- 10. The process of claim 3 in which said converting, in said second stream, of said ion of manganese in lower-valent form to higher-valent form is done by electrolytically oxidizing the lower-valent ion.
- 11. The process of claim 3 in which said converting, in said second stream, of said ion of manganese in lower-valent form to higher-valent form is done by reacting the lower-valent ion with peracetic acid.
CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of copending application Ser. No. 772,994, filed Nov. 4, 1968, now abandoned, which is a continuation-in-part of application Ser. No. 714,447 abandoned, filed Mar. 30, 1968, now abandoned in favor of a continuation-in-part application thereof Ser. No. 30,582, filed Apr. 21, 1970, now abandoned in favor of continuation-in-part application thereof Ser. No. 336,857, filed Feb. 28, 1973. The entire disclosure of application Ser. No. 714,447, filed Mar. 30, 1968, is incorporated herein by reference. The synthesis of gamma-butyrolactones is described in detail in this latter disclosure.
US Referenced Citations (1)
Number |
Name |
Date |
Kind |
2986568 |
Johnston |
May 1961 |
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Non-Patent Literature Citations (1)
Entry |
R. E. Van der Ploeg et al. Journal of Catalysis, vol. 10 pp. 52-59 (1968). |
Continuation in Parts (4)
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Number |
Date |
Country |
Parent |
772994 |
Nov 1968 |
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Parent |
714447 |
Mar 1968 |
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Parent |
30582 |
Apr 1970 |
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Parent |
336857 |
Feb 1973 |
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