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US3839267A Expired / Lapsed US ⏱️ 0.0 years remaining

Heterogeneous melt hydrolysis of oxymethylene copolymers

Assignee: Celanese Corp
•
Filing: 1973-04-12
•
Granted: 1974-10-01
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Expires: 1993-04-12
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Abstract

Abstract An improved process for the stabilization of a normally solid oxymethylene copolymer whose molecules contain a majority of relatively unstable monomeric oxymethylene units interspersed with comparatively stable, monomeric higher oxyalkylene units, e.g., -O- CH2-CH2- units, at least part of the terminal portions of said molecule comprising said unstable monomeric units, wherein said copolymer is hydrolyzed in the presence of water, alcohol, trioxane or mixtures thereof is present as a vapor in which said improvement comprises hydrolyzing in the presence of a stabilizer system comprising an acid scavenger; an antioxidant; or an acid scavenger and an antioxidant.

Inventors

  • 👤 M Golder

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-06 09:50
CPC Classifications
C; C08; C08G; C08G2/00; C08G2/30; C08G2/36

Claims Analysis

Total Claims: 14
Claim 1
Independent Claim 275 words
IN AN EXTRUDER PROCESS FOR THE STABILIZATION OF A NORMALLY SOLID OXYMETHYLENE COPOLYMER HAVING A MELTING POINT ABOVE ABOUT 150*C., THE MOLECULES OF SAID COPOLYMER CONTAINING FROM 60 TO 99.6 MOLE PERCENT OF COMPARATIVELY UNSTABLE MONOMERIC OXYMETHYLENE UNITS INTERSPERSED WITH COMPARATIVELY STABLE MONOMERIC-OR- UNITS INWHEREIN R IS A DIVALENT RADICAL CONTAINING AT LEAST TWO CARBON ATOMS DIRECTLY LINKED TO EACH OTHER AND POSITIONED IN THE POLYMER CHAIN BETWEEN THE TWO VALENCES, WITH ANY SUBSTITUENTS ON SAID R RADICALS BEING INERT, AT LEAST PART OF THE TERMINAL PORTIONS OF SAID MOLECULES COMPRISING SAID UNSTABLE MONOMERIC UNITS, WHEREIN THE IMPROVEMENT COMPRISES REACTING IN AN EXTRUDER SAID COPOLYMER; FROM 2 TO ABOUT 25 WEIGHT PERCENT, BASED ON THE COPOLYMER OF A REACTANT SELECTED FROM THE CLASS CONSISTING OF WATER, AND ALCOHOL, AND MIXTURES THEREOF AND FROM ABOUT 0.05 TO ABOUT 10.0 WEIGHT PERCENT BASED ON POLYMER WEIGHT OF A STABILIZER SYSTEM SELECTED FROM THE GROUP CONSISTING OF AN ACID SCAVENGER, AN ANTIOXIDANT AND AN ACID SCAVENGER AND AN ANTIOXIDANT IN A HETEROGENOUS REACTION ZONE COMPRISING MOLTEN COPOLYMER AND VAPOROUS REACTANT BY MAINTAINING THE REACTION ZONE AT A TEMPERATURE ABOVE THE MELTING POINT OF COPOLYMER AND AT A PRESSURE SUFFICIENT TO MAINTAIN THE COPOLYMER IN A MOLTEN STATE AND THE REACTANT IN A VAPOR STATE, AND SAID SYSTEM IS REACTED UNDER THE ABOVE CONDITIONS OF TEMPERATURE AND PRESSURE FOR A PERIOD OF TIME IN THE RANGE OF FROM ABOUT 0.1 TO ABOUT 15 MINUTES TO REMOVE UNSTABLE MONOMERIC OXYMETHYLENE UNITS FROM THE TERMINAL PORTIONS OF THE COPOLYMER MOLECULES SO THAT AT LEAST 90 PERCENT OF THE RESULTING POLYMERIC CHAINS OF THE MOLECULES ARE TERMINATED BY THE STABLE MONOMERIC UNITS.
Claim 2
Dependent Claim 275 words
IN AN EXTRUDER PROCESS FOR THE STABILIZATION OF A NORMALLY SOLID OXYMETHYLENE COPOLYMER HAVING A MELTING POINT ABOVE ABOUT 150*C., THE MOLECULES OF SAID COPOLYMER CONTAINING FROM 60 TO 99.6 MOLE PERCENT OF COMPARATIVELY UNSTABLE MONOMERIC OXYMETHYLENE UNITS INTERSPERSED WITH COMPARATIVELY STABLE MONOMERIC-OR- UNITS INWHEREIN R IS A DIVALENT RADICAL CONTAINING AT LEAST TWO CARBON ATOMS DIRECTLY LINKED TO EACH OTHER AND POSITIONED IN THE POLYMER CHAIN BETWEEN THE TWO VALENCES, WITH ANY SUBSTITUENTS ON SAID R RADICALS BEING INERT, AT LEAST PART OF THE TERMINAL PORTIONS OF SAID MOLECULES COMPRISING SAID UNSTABLE MONOMERIC UNITS, WHEREIN THE IMPROVEMENT COMPRISES REACTING IN AN EXTRUDER SAID COPOLYMER; FROM 2 TO ABOUT 25 WEIGHT PERCENT, BASED ON THE COPOLYMER OF A REACTANT SELECTED FROM THE CLASS CONSISTING OF WATER, AND ALCOHOL, AND MIXTURES THEREOF AND FROM ABOUT 0.05 TO ABOUT 10.0 WEIGHT PERCENT BASED ON POLYMER WEIGHT OF A STABILIZER SYSTEM SELECTED FROM THE GROUP CONSISTING OF AN ACID SCAVENGER, AN ANTIOXIDANT AND AN ACID SCAVENGER AND AN ANTIOXIDANT IN A HETEROGENOUS REACTION ZONE COMPRISING MOLTEN COPOLYMER AND VAPOROUS REACTANT BY MAINTAINING THE REACTION ZONE AT A TEMPERATURE ABOVE THE MELTING POINT OF COPOLYMER AND AT A PRESSURE SUFFICIENT TO MAINTAIN THE COPOLYMER IN A MOLTEN STATE AND THE REACTANT IN A VAPOR STATE, AND SAID SYSTEM IS REACTED UNDER THE ABOVE CONDITIONS OF TEMPERATURE AND PRESSURE FOR A PERIOD OF TIME IN THE RANGE OF FROM ABOUT 0.1 TO ABOUT 15 MINUTES TO REMOVE UNSTABLE MONOMERIC OXYMETHYLENE UNITS FROM THE TERMINAL PORTIONS OF THE COPOLYMER MOLECULES SO THAT AT LEAST 90 PERCENT OF THE RESULTING POLYMERIC CHAINS OF THE MOLECULES ARE TERMINATED BY THE STABLE MONOMERIC UNITS.
Claim 3
Dependent Claim 18 words
The process of claim 1 wherein the temperature is in the range of from about 160* to 240*C.
Claim 4
Dependent Claim 13 words
The process of claim 1 wherein the pressure is below about 150 p.s.i.a.
Claim 5
Dependent Claim 12 words
The process of claim 1 wherein said stable units are oxymethylene units.
Claim 6
Dependent Claim 43 words
The process of claim 1 wherein any unreacted reactant is removed from the resulting stabilized copolymer by reducing the pressure in said reaction zone to a pressure in the range of from about 0.1 to about 50 p.s.i.a. to volatilize the unreacted reactant.
Claim 7
Dependent Claim 24 words
The process of claim 1 wherein the alcohol is selected from the class consisting of methyl alcohol, ethyl alcohol, n-propyl alcohol and isopropyl alcohol.
Claim 8
Dependent Claim 16 words
The process of claim 1 wherein the copolymer is reacted with the reactant under alkaline conditions.
Claim 9
Dependent Claim 16 words
The process of claim 1 wherein a reinforcing agent is present in the hydrolysis reaction zone.
Claim 10
Dependent Claim 11 words
The process of claim 8 wherein the reinforcing agent is fiberglass.
Claim 11
Dependent Claim 13 words
The process of claim 8 wherein the reinforcing agent is acicular calcium metasilicate.
Claim 12
Dependent Claim 14 words
The process of claim 8 wherein the reinforcing agent is fiberglass and calcium metasilicate.
Claim 13
Dependent Claim 13 words
The process of claim 8 wherein the reinforcing agent is fiberglass and asbestos.
Claim 14
Dependent Claim 16 words
The process of claim 1 wherein a substituted benzotriazole is present in the hydrolysis reaction zone.

References Cited (Backward Citations)

US3189615A Cited
US3169938A Cited
US3219623A Cited
US3318848A Cited
US3450665A Cited
US3484400A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1977-09-30 1978-04-01 1978-10-01 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1981-09-30 1982-04-01 1982-10-01 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1985-09-30 1986-04-01 1986-10-01 $7700.00 Window Closed / Lapsed

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