US3896006A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Mesityl oxide removal from high-purity phenol
Assignee: BP Chemicals Ltd
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Filing: 1974-05-08
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Granted: 1975-07-22
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Expires: 1994-05-08
Abstract
Abstract A process for the purification of phenol obtained from the acid cleavage of cumene hydroperoxide and consisting essentially of phenol and less than 1,000 parts per million of water-soluble colour forming impurities boiling from 152* to 182* by subjecting the phenol to a fractional distillation such that the impurities are retained within the column under distillation conditions for a period so as to concentrate them and at least partially to decompose them to mesityl oxide, removing a base product comprising phenol free from the water-soluble colour forming impurities boiling from 152* to 182* and an overhead fraction containing mesityl oxide and thereafter separating the phenol free from the higher boiling decomposition products. The purification is effected in a distillation column distilling crude phenol or other column with overhead take-off provided with an enlarged stripping section or by deep-topping of purified phenol or by removing a phenolic sidestream from a phenol dehydration column.
Inventors
- 👤 Maurice Dudley Cooke
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 02:31
CPC Classifications
C; C07; C07C; C07C37/00; C07C37/68; C07C37/70; C07C37/74
Claims Analysis
Total Claims: 17
Claim 1
Independent Claim
114 words
A PROCESS FOR THE PURIFICATION OF CRUDE PHENOL OBTAINED FROM THE ACID CLEAVAGE OF CUMENE HYDROPEROXIDE WHICH COMPRISES SUBJECTING A FEED OF CRUDE PHENOL CONSISTING ESSENTIALLY OF PHENOL AND LESS THAN 1,000 PARTS PER MILLION OF WATER-SOLUBLE COLOR-FORMING IMPURITIES BOILING FROM 152* TO 152*C. TO A FRACTIONAL DISTILLATION SUCH THAT WATER-SOLUBLE COLOR-FORMING IMPURITIES ARE RETAINED WITHIN A SECTION OF THE COLUMN UNDER DISTILLATION CONDITIONS SO AS TO CONCENTRATE SAID IMPURITIES AND AT LEAST PARTIALLY TO DECOMPOSE SAID IMPURITIES TO MESITYL OXIDE, REMOVING A BASE PRODUCT COMPRISING PHENOL FREE FROM WATER-SOLUBLE COLOR-FORMING IMPURITIES BOILING FROM 152* TO 182*C. AND AN OVERHEAD FRACTION CONTAINING MESITYL OXIDE, AND THEREAFTER DISTILLING THE PHENOL FROM THE HIGHERBOILING DECOMPOSITION PRODUCTS.
Claim 2
Dependent Claim
114 words
A PROCESS FOR THE PURIFICATION OF CRUDE PHENOL OBTAINED FROM THE ACID CLEAVAGE OF CUMENE HYDROPEROXIDE WHICH COMPRISES SUBJECTING A FEED OF CRUDE PHENOL CONSISTING ESSENTIALLY OF PHENOL AND LESS THAN 1,000 PARTS PER MILLION OF WATER-SOLUBLE COLOR-FORMING IMPURITIES BOILING FROM 152* TO 152*C. TO A FRACTIONAL DISTILLATION SUCH THAT WATER-SOLUBLE COLOR-FORMING IMPURITIES ARE RETAINED WITHIN A SECTION OF THE COLUMN UNDER DISTILLATION CONDITIONS SO AS TO CONCENTRATE SAID IMPURITIES AND AT LEAST PARTIALLY TO DECOMPOSE SAID IMPURITIES TO MESITYL OXIDE, REMOVING A BASE PRODUCT COMPRISING PHENOL FREE FROM WATER-SOLUBLE COLOR-FORMING IMPURITIES BOILING FROM 152* TO 182*C. AND AN OVERHEAD FRACTION CONTAINING MESITYL OXIDE, AND THEREAFTER DISTILLING THE PHENOL FROM THE HIGHERBOILING DECOMPOSITION PRODUCTS.
Claim 3
Dependent Claim
50 words
A process according to claim 1, wherein said distillation to concentrate and decompose said impurities is effected in an anhydrous part of an enlarged stripping section of a distillation column having an overhead take-off, said enlarged stripping section providing for an increased residence time of said impurities in said column.
Claim 4
Dependent Claim
61 words
A process according to claim 2 wherein: (a) the feed to said distillation column contains acetone, water, mesityl oxide, cumene and methyl styrene, and high boiling cleavage products; (b) water, acetone, and some hydrocarbon and mesityl oxide is removed in the overhead fraction; and (c) phenol, said impurities, and higher boiling cleavage products are in an anhydrous part of said column.
Claim 5
Dependent Claim
129 words
A process for the purification of crude phenol obtained from the acid cleavage of cumene hydroperoxide which comprises subjecting a feed consisting essentially of phenol and less than 1,000 parts per million of water-soluble color-forming impurities boilingg from 152* to 182*C., said crude phenol being free fRom acetone, water, mesityl oxide, cumene and methyl styrene, to a fractional distillation such that the water-soluble impurities are retained within a section of the column under distillation conditions so as to concentrate said impurities and at least partially to decompose them to mesityl oxide, removing a base product comprising phenol free from said impurities and higher boiling products and an overhead fraction containing some phenol, mesityl oxide, and water-soluble color-forming impurities, and thereafter distilling the base phenol from the higher boiling products.
Claim 6
Dependent Claim
129 words
A process for the purification of crude phenol obtained from the acid cleavage of cumene hydroperoxide which comprises subjecting a feed consisting essentially of phenol and less than 1,000 parts per million of water-soluble color-forming impurities boilingg from 152* to 182*C., said crude phenol being free fRom acetone, water, mesityl oxide, cumene and methyl styrene, to a fractional distillation such that the water-soluble impurities are retained within a section of the column under distillation conditions so as to concentrate said impurities and at least partially to decompose them to mesityl oxide, removing a base product comprising phenol free from said impurities and higher boiling products and an overhead fraction containing some phenol, mesityl oxide, and water-soluble color-forming impurities, and thereafter distilling the base phenol from the higher boiling products.
Claim 7
Dependent Claim
24 words
A process according to claim 4 wherein said distillation is effected just after the crude phenol distillation separating phenol from higher boiling distillation products.
Claim 8
Dependent Claim
25 words
A process according to claim 4 wherein said distillation is carried out just before final recovery of phenol as a distillate from higher boiling products.
Claim 9
Dependent Claim
70 words
A process according to claim 4 wherein said overhead fraction comprising some phenol, mesityl oxide, and said impurities is recycled to a point in the overall distillation sequence for the recovery of phenol from the acid cleavage of cumene hydroperoxide at which impurities tend to be concentrated under conditions of temperature above the temperature at which at least partial decomposition of said impurities to mesityl oxide occurs under anhydrouus conditions.
Claim 10
Dependent Claim
45 words
A process according to claim 7 wherein the overhead fraction is re-cycled to the stripping section of a continuously operated column separating phenol from acetone, water, cumene, mesityl oxide and methyl styrene and having an anhydrous zone in the stripping section below the feed point.
Claim 11
Dependent Claim
24 words
A process according to claim 8 wherein citric acid is introduced into the column separating phenol from acetone, cumene, mesityl oxide and methyl styrene.
Claim 12
Dependent Claim
24 words
A process according to claim 8 wherein sodium phenate is introduced into the column separating phenol from acetone, cumene, mesityl oxide and methyl styrene.
Claim 13
Dependent Claim
22 words
A process according to claim 4 wherein said fractional distillation is carried out immediately after distillation separating crude acetone from crude phenol.
Claim 14
Dependent Claim
139 words
A process for the purification of a crude phenol obtained from the acid cleavage of cumene hydroperoxide which comprises subjecting a feed of crude phenol consisting essentially of phenol and less than 1,000 parts per million of water-soluble color-forming impurities boiling from 152* to 182*C. to a fractional distillation such that the water-soluble color-forming impurities are maintained within a water-free section of a phenol dehydration column so as to concentrate the impurities and at least partially to decompose said impurities to mesityl oxide, removing a phenolic sidestream containing residual impurities at a point in said column where the water content is below about 10% by weight, removing a base product comprising phenol free from water-soluble color-formingg impurities boiling from 152* to 182*C. and an overhead fraction containing mesityl oxide, and thereafter separating the phenol from the higher-boiling decomposition products.
Claim 15
Dependent Claim
139 words
A process for the purification of a crude phenol obtained from the acid cleavage of cumene hydroperoxide which comprises subjecting a feed of crude phenol consisting essentially of phenol and less than 1,000 parts per million of water-soluble color-forming impurities boiling from 152* to 182*C. to a fractional distillation such that the water-soluble color-forming impurities are maintained within a water-free section of a phenol dehydration column so as to concentrate the impurities and at least partially to decompose said impurities to mesityl oxide, removing a phenolic sidestream containing residual impurities at a point in said column where the water content is below about 10% by weight, removing a base product comprising phenol free from water-soluble color-formingg impurities boiling from 152* to 182*C. and an overhead fraction containing mesityl oxide, and thereafter separating the phenol from the higher-boiling decomposition products.
Claim 16
Dependent Claim
48 words
A process according to claim 12 wherein the phenolic sidestream is re-cycled to the stripping section of continuously operated column separating phenol from acetone, water, cumene, mesityl oxide and methyl styrene for further decomposition of the impurities in the anhydrous zone of the stripping section of the column.
Claim 17
Dependent Claim
31 words
A process according to claim 12 wherein the base product comprising phenol free from water-soluble colour-forming impurities boiling from 152* to 182*C is removed as a sidestream from the distillation column.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-07-21 | 1979-01-20 | 1979-07-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-07-21 | 1983-01-20 | 1983-07-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-07-21 | 1987-01-20 | 1987-07-22 | $7700.00 | Window Closed / Lapsed |