US3873468A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of removing substance harmful to oxidation reaction in the production of benzenecarboxylic acids by oxidation
Assignee: Kuraray Yuka Co Ltd
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Filing: 1971-11-30
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Granted: 1975-03-25
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Expires: 1991-11-30
Abstract
Abstract In the production of benzene carboxylic acids by the oxidation of alkyl benzenes with molecular oxygen in the presence of a heavy metal oxidation catalyst, the catalyst is recovered as a residue contaminated by iron and tar-like by-products which act as inhibitors for the oxidation reaction and cannot be re-used as such. The catalyst is recovered in such a purity as re-usable by extracting the residue by water, regulating the pH of the aqueous phase to a value more than 5 but not exceeding 8 to thereby separate the tar-like products as an oily float and iron as precipitates and removing such oily float and precipitates from the aqueous phase.
Inventors
- 👤 Sadao Kobinata
- 👤 Takeo Satake
- 👤 Naonobu Hiramoto
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 10:46
CPC Classifications
B; B01; B01J; B01J31/00; B01J31/40; B01J31/4015; B01J31/4023; B01J31/403; B01J27/00; B01J27/28; B01J27/32; B01J31/26; C; C07; C07C; C07C51/00; C07C51/42; B01J2231/00; B01J2231/70; B01J2531/00; B01J2531/70; B01J2531/72; B01J2531/80; B01J2531/84; B01J2531/845; B01J27/20; B01J27/232; B01J31/02; B01J31/04; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/584
Claims Analysis
Total Claims: 7
Claim 1
Independent Claim
191 words
A METHOD OF REMOVING IRON AND TAR-LIKE BY-PRODUCTS FROM THE RESIDUE CONTAINING A HEAVY METAL OXIDATION CATALYST, SAID RESIDUE BEING DERIVED BY SEPARATING THE FORMED BENZENE CARBOXYLIC ACID AND THEN RECOVERING A SOLVENT FROM THE REACTION MIXTURE RESULTING FROM THE LIQUID PHASE OXIDATION OF AN ALKYL BENZENE WITH A MOLECULAR OXYGEN-CONTAINING GAS USING A HEAVY METAL OXIDATION CATALYST IN THE PRESENCE OF A SATURATED LOWER ALIPHATIC MONOCARBOXYLIC ACID HAVING 2 TO 4 CARBON ATOMS AS A SOLVENT, WHEREIN THE REACTION MIXTURE IS CONTAMINATED BY IRON AND TAR-LIKE OXIDATION BY-PRODUCTS WHICH ACT AS INHIBITORS FOR THE OXIDATION REACTION, SAID METHOD COMPRISING THE STEPS OF: SUBJECTING SAID RESIDUE TO EXTRACTION WITH WATER; SEPARATING THE CATALYST-CONTAINING AQUEOUS PHASE FROM THE SO-TREATED WATER-INSOLUBLE RESIDUE, ADDING AN ALKALI SALT OF A SATURATED LOWER ALIPHATIC MONOCARBOXYLIC ACID PLUS A SATURATED LOWER ALIPHATIC MONOCARBOXYLIC ACID TO THE AQUEOUS PHASE TO REGULATE THE PH OF THE AQUEOUS PHASE TO A VALUE MORE THAN 5 BUT NOT EXCEEDING 8 TO THEREBY SEPARATE THE TAR-LIKE BY-PRODUCTS AS AN OILY FLOAT AND IRON AS A PRECIPITATE OF BASIC IRON CARBOXYLATE; AND REMOVING SAID OILY FLOAT AND SAID PRECIPITATE FROM THE AQUEOUS PHASE.
Claim 2
Independent Claim
191 words
A METHOD OF REMOVING IRON AND TAR-LIKE BY-PRODUCTS FROM THE RESIDUE CONTAINING A HEAVY METAL OXIDATION CATALYST, SAID RESIDUE BEING DERIVED BY SEPARATING THE FORMED BENZENE CARBOXYLIC ACID AND THEN RECOVERING A SOLVENT FROM THE REACTION MIXTURE RESULTING FROM THE LIQUID PHASE OXIDATION OF AN ALKYL BENZENE WITH A MOLECULAR OXYGEN-CONTAINING GAS USING A HEAVY METAL OXIDATION CATALYST IN THE PRESENCE OF A SATURATED LOWER ALIPHATIC MONOCARBOXYLIC ACID HAVING 2 TO 4 CARBON ATOMS AS A SOLVENT, WHEREIN THE REACTION MIXTURE IS CONTAMINATED BY IRON AND TAR-LIKE OXIDATION BY-PRODUCTS WHICH ACT AS INHIBITORS FOR THE OXIDATION REACTION, SAID METHOD COMPRISING THE STEPS OF: SUBJECTING SAID RESIDUE TO EXTRACTION WITH WATER; SEPARATING THE CATALYST-CONTAINING AQUEOUS PHASE FROM THE SO-TREATED WATER-INSOLUBLE RESIDUE, ADDING AN ALKALI SALT OF A SATURATED LOWER ALIPHATIC MONOCARBOXYLIC ACID PLUS A SATURATED LOWER ALIPHATIC MONOCARBOXYLIC ACID TO THE AQUEOUS PHASE TO REGULATE THE PH OF THE AQUEOUS PHASE TO A VALUE MORE THAN 5 BUT NOT EXCEEDING 8 TO THEREBY SEPARATE THE TAR-LIKE BY-PRODUCTS AS AN OILY FLOAT AND IRON AS A PRECIPITATE OF BASIC IRON CARBOXYLATE; AND REMOVING SAID OILY FLOAT AND SAID PRECIPITATE FROM THE AQUEOUS PHASE.
Claim 3
Independent Claim
39 words
THE METHOD OF CLAIM, WHEREIN AFTER SEPARATING THE OILY FLOAT AND THE PRECIPITATE FROM THE AQUEOUS PHASE, AN ALKALI CARBONATE IS ADDED TO THE AQUEOUS PHASE TO SEPARATE AND RECOVER THE CATALYST HEAVY METAL AS A PRECIPITATE OF CARBONATE.
Claim 4
Dependent Claim
54 words
The method of claim 1, wherein the separated aqueous phase is subjected to pre-treatment to maintain its pH within the range of 4 to 5 to thereby precipitate iron as a basic iron carboxylate and then the pH of the aqueous phase is adjusted to a value more than 5 but not exceeding 8.
Claim 5
Dependent Claim
41 words
The method of claim 3, wherein after removing the oily float and the precipitate from the aqueous phase, an alkali carbonate is added to the aqueous phase to thereby separate and recover the catalyst heavy metal as a precipitate of carbonate.
Claim 6
Dependent Claim
56 words
The method of claim 1, wherein the pH of the aqueous phase is adjusted to a value more than 5 but not exceeding 8 to thereby separate the tar-like oxidation by-products and iron from the aqueous phase, and then the pH of the aqueous phase is re-adjusted to 4-5, to thereby promote the precipitation of iron.
Claim 7
Dependent Claim
39 words
The method of claim 5, wherein after removing iron and tar-like by-products from the aqueous phase, an alkali carbonate is added to the aqueous phase to thereby separate and recover the catalyst heavy metal as a precipitate of carbonate.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-03-24 | 1978-09-23 | 1979-03-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-03-24 | 1982-09-23 | 1983-03-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-03-24 | 1986-09-23 | 1987-03-25 | $7700.00 | Window Closed / Lapsed |