US4075236A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Continuous manufacture of peroxyesters
Assignee: Arkema Inc
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Filing: 1976-09-30
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Granted: 1978-02-21
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Expires: 1996-09-30
Abstract
Abstract A continuous solvent-free process for the manufacturing of peroxyesters from an acid chloride, a hydroperoxide and an alkali metal hydroxide generates a pure product of good quality, high yields and throughput per unit volume of the reactor. The process comprises at least two reactors and a physical separation unit for separating the high purity product.
Inventors
- 👤 Uday Dakornath Wagle
- 👤 Venkatram Ramdas
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 13:46
CPC Classifications
C; C07; C07C; C07C407/00; C07C2601/00; C07C2601/12; C07C2601/16
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
359 words
A process for the continuous manufacture of a peroxyester having the formula ##STR2## wherein: (a) x, y, and n are 1 or 2; (b) when x is 2, y is 1 and n is 2; (c) when y is 2, x is 1 and n is 2; (d) when x, y and n are 1, R is selected from the group consisting of a primary, secondary, or tertiary alkyl of 1 to 17 carbons, aryl of 6 to 14 carbons, and cycloalkyl of 3 to 12 carbons, and R' is selected from the group consisting of a tertiary alkyl of 4 to 12 carbons, a tertiary aralkyl of 9 to 18 carbons, and tertiary cycloalkyl of 6 to 12 carbons; (e) when x is 2, R is a diradical selected from alkylene of 1 to 16 carbons, arylene of 6 to 14 carbons, cycloalkylene of 3 to 12 carbons, and aralkylene of 7 to 18 carbons; and (f) when y is 2, R' is a di-tertiary diradical selected from alkylene of 6 to 16 carbons, aralkylene of 12 to 18 carbons, and cycloalkylene of 7 to 12 carbons; which comprises: (I) continuously reacting an acid chloride having the formula ##STR3## a hydroperoxide having the formula R'(OOH) n , and an aqueous alkali metal hydroxide in two reaction zones of intense mixing connected in series in a temperature range of about -10° to +50° C and a pH of 10 to 14, wherein the first reaction zone is maintained in the upper part of the temperature range and the second reaction zone is maintained in the lower part of the temperature range; (II) continuously recovering the peroxyester product by (i) continuously feeding the reaction mixture directly from the second reaction zone through a liquid-liquid separation unit; (ii) continuously subjecting the product stream from the liquid-liquid separation unit to a series of washings and separations in a mixer-settler system; and (iii) continuously gas stripping the product from the mixer-settler system in a stripping column; and (iv) continuously adding the acid chloride, hydroperoxide and aqueous alkali metal hydroxide to the first reaction zone to replace that used up in the reaction effluent.
Claim 2
Dependent Claim
359 words
A process for the continuous manufacture of a peroxyester having the formula ##STR2## wherein: (a) x, y, and n are 1 or 2; (b) when x is 2, y is 1 and n is 2; (c) when y is 2, x is 1 and n is 2; (d) when x, y and n are 1, R is selected from the group consisting of a primary, secondary, or tertiary alkyl of 1 to 17 carbons, aryl of 6 to 14 carbons, and cycloalkyl of 3 to 12 carbons, and R' is selected from the group consisting of a tertiary alkyl of 4 to 12 carbons, a tertiary aralkyl of 9 to 18 carbons, and tertiary cycloalkyl of 6 to 12 carbons; (e) when x is 2, R is a diradical selected from alkylene of 1 to 16 carbons, arylene of 6 to 14 carbons, cycloalkylene of 3 to 12 carbons, and aralkylene of 7 to 18 carbons; and (f) when y is 2, R' is a di-tertiary diradical selected from alkylene of 6 to 16 carbons, aralkylene of 12 to 18 carbons, and cycloalkylene of 7 to 12 carbons; which comprises: (I) continuously reacting an acid chloride having the formula ##STR3## a hydroperoxide having the formula R'(OOH) n , and an aqueous alkali metal hydroxide in two reaction zones of intense mixing connected in series in a temperature range of about -10° to +50° C and a pH of 10 to 14, wherein the first reaction zone is maintained in the upper part of the temperature range and the second reaction zone is maintained in the lower part of the temperature range; (II) continuously recovering the peroxyester product by (i) continuously feeding the reaction mixture directly from the second reaction zone through a liquid-liquid separation unit; (ii) continuously subjecting the product stream from the liquid-liquid separation unit to a series of washings and separations in a mixer-settler system; and (iii) continuously gas stripping the product from the mixer-settler system in a stripping column; and (iv) continuously adding the acid chloride, hydroperoxide and aqueous alkali metal hydroxide to the first reaction zone to replace that used up in the reaction effluent.
Claim 3
Dependent Claim
27 words
The process of claim 1 wherein the throughput per unit volume of the reactor is 80 to 120 grams per gallon per hour of active oxygen content.
Claim 4
Dependent Claim
9 words
The process of claim 1 wherein R is t-butyl.
Claim 5
Dependent Claim
9 words
The process of claim 1 wherein R is phenyl.
Claim 6
Dependent Claim
9 words
The process of claim 1 wherein R is 3-heptyl.
Claim 7
Dependent Claim
9 words
The process of claim 1 wherein R is t-nonyl.
Claim 8
Dependent Claim
9 words
The process of claim 1 wherein R' is t-butyl.
Claim 9
Dependent Claim
15 words
The process of claim 3 wherein a solvent is added to the first reaction zone.
Claim 10
Dependent Claim
56 words
The process of claim 1 wherein the reaction zones have a liquid depth to reactor diameter ratio of 1 to 2, and the intense mixing is provided by an impeller with a tip speed of at least 1000 feet per minute and a power input in the range of 50 to 200 horsepower per 1000 gallons.
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) | 1981-02-20 | 1981-08-22 | 1982-02-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-02-20 | 1985-08-22 | 1986-02-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-02-20 | 1989-08-22 | 1990-02-21 | $7700.00 | Window Closed / Lapsed |