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US3928474A Expired / Lapsed US ⏱️ 0.0 years remaining

Manufacture of glycols

Assignee: Wyeth Holdings LLC
•
Filing: 1974-06-21
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Granted: 1975-12-23
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Expires: 1994-06-21
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Abstract

Abstract There is provided a process for preparing ethylene glycol by adding about 1 mole of water, from about 0.350 to 0.490 mole of oxygen and an aqueous solution of a catalytic iodine-containing compound selected from the group consisting of iodine, hydrogen iodide, ethylene diiodide and iodoethanol to a first reaction zone, introducing about 1 mole of ethylene and about 0.010 to 0.150 mole of oxygen to a second reaction zone, the amount of oxygen in both zones being equal to about 0.5 mole, withdrawing ethylene from the second reaction from overheads and introducing the same into the said first reaction zone, withdrawing from the first reaction zone a mixture of relatively high boiling organic iodides, iodine and ethylene glycol, introducing the latter mixture into said second reaction zone while maintaining said reaction zones at temperatures ranging from between 75*C. and 175*C. and pressures ranging from between 50 psi and 1,000 psi in each of said reaction zones, withdrawing a mixture of low boiling iodides and ethylene glycol as bottoms from the second reaction zone, subjecting the latter to distillation at a temperature of from 50*C. to 190*C. and under subatmospheric pressure ranging from about 1 mm. Hg. to about 700 mm. Hg., withdrawing as an overhead low boiling iodine compounds which are recycled to the first reaction zone, and recovering as bottoms an ethylene glycol product of markedly improved purity substantially devoid of iodinecontaining catalyst.

Inventors

  • 👤 John Maurice Witheford

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 22:12
CPC Classifications
C; C07; C07C; C07C29/00; C07C29/03

Claims Analysis

Total Claims: 3
Claim 1
Independent Claim 135 words
IN A PROCESS FOR PREPARING ETHYLENE GLYCOL WHICH COMPRISES BRINGING INTO REACTIVE COMBINATION ETHYLENE, WATER AND OXYGEN IN SUBSTANTIALLY STOICHIOMETRIC AMOUNTS IN AT LEAST TWO REACTION ZONES MAINTAINED AT AN ELEVATED TEMPERATURE AND UNDER SUPERATMOSPHERIC PRESSURE IN THE PRESENCE OF AN AQUEOUS OUS IODINE-CONTAINING CATALYST FOR SAID REACTION, DISTILLING THE LATTER REACTION MIXTURE AND RECOVERING ETHYLENE GLYCOL FROM SAID REACTION MIXTURE, THE IMPROVEMENT WHICH COMPRISES THE STEPS OF: ADDING FROM ABOUT 0.350 TO 0.490 MOLE OF OXYGEN AND AN AQUEOUS SOLUTION OF A CATALYST IODINE-CONTAINING COMPOUND SELECTED FROM THE GROUP CONSISTING OF IODINE, HYDROGEN IODIDE, ETHYLENE DIIODIE, IODOETHANOL AND MIXTURES THEREOF DISSOLVED IN AT LEAST 1 MOLE OF WATER TO A FIRST REACTION ZONE INTRODUCING ABOUT 1 MOLE OF ETHYLENE AND ABOUT 0.010 TO 0.150 MOLE OF OXYGEN TO A SECOND REACTION ZONE, THE AMOUNT
Claim 2
Dependent Claim 135 words
IN A PROCESS FOR PREPARING ETHYLENE GLYCOL WHICH COMPRISES BRINGING INTO REACTIVE COMBINATION ETHYLENE, WATER AND OXYGEN IN SUBSTANTIALLY STOICHIOMETRIC AMOUNTS IN AT LEAST TWO REACTION ZONES MAINTAINED AT AN ELEVATED TEMPERATURE AND UNDER SUPERATMOSPHERIC PRESSURE IN THE PRESENCE OF AN AQUEOUS OUS IODINE-CONTAINING CATALYST FOR SAID REACTION, DISTILLING THE LATTER REACTION MIXTURE AND RECOVERING ETHYLENE GLYCOL FROM SAID REACTION MIXTURE, THE IMPROVEMENT WHICH COMPRISES THE STEPS OF: ADDING FROM ABOUT 0.350 TO 0.490 MOLE OF OXYGEN AND AN AQUEOUS SOLUTION OF A CATALYST IODINE-CONTAINING COMPOUND SELECTED FROM THE GROUP CONSISTING OF IODINE, HYDROGEN IODIDE, ETHYLENE DIIODIE, IODOETHANOL AND MIXTURES THEREOF DISSOLVED IN AT LEAST 1 MOLE OF WATER TO A FIRST REACTION ZONE INTRODUCING ABOUT 1 MOLE OF ETHYLENE AND ABOUT 0.010 TO 0.150 MOLE OF OXYGEN TO A SECOND REACTION ZONE, THE AMOUNT
Claim 3
Dependent Claim 31 words
The process of claim 1 wherein there is present in the first reaction zone 0.475 mole of oxygen and in the second reaction zone there is present 0.025 mole of oxygen.

References Cited (Backward Citations)

US1724761A Cited
US1982545A Cited
US2378104A Cited
US3629343A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-12-22 1979-06-23 1979-12-23 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-12-22 1983-06-23 1983-12-23 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-12-22 1987-06-23 1987-12-23 $7700.00 Window Closed / Lapsed

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