Patent US4243799A successfully refreshed from Google Patents.
← Back to Patent Explorer
US4243799A Expired / Lapsed US ⏱️ 0.0 years remaining

Polymerization of tetrahydrofuran

Assignee: BASF SE
•
Filing: 1979-05-18
•
Granted: 1981-01-06
•
Expires: 1999-05-18
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract A process for the preparation of polybutylene glycol carboxylic acid diesters of the formula R--CO--O--CH.sub.2 CH.sub.2 CH.sub.2 CH.sub.2 --O).sub.n CO--R.sup.1 by polymerizing pretreated tetrahydrofuran in the presence of one or more carboxylic acids and/or carboxylic acid anhydrides and of a polymerization catalyst, especially antimony pentachloride or a bleaching earth containing less than 3% by weight of water, wherein the tetrahydrofuran is treated with a strong mineral acid, an organic sulfonic acid, silica gel and/or a bleaching earth prior to the polymerization.

Inventors

  • 👤 Herbert Mueller
  • 👤 Otto H. Huchler
  • 👤 Herwig Hoffmann

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-06 13:10
CPC Classifications
C; C08; C08G; C08G65/00; C08G65/02; C08G65/26; C08G65/2642; C08G65/2645; C08G65/2654; C08G65/2657; C08G18/00; C08G18/06; C08G18/28; C08G18/40; C08G18/48; C08G18/4854; C08G65/04; C08G65/06; C08G65/16; C08G65/20; C08G65/266

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 166 words
In a process for the preparation of polybutylene glycol carboxylic acid diesters of the formula R--CO--O--CH.sub.2 CH.sub.2 CH.sub.2 CH.sub.2 --O).sub.n CO--R.sup.1 where R and R 1 are identical or different and each is alkyl, a carboxyl-containing aliphatic radical which may or may not be ethylenically unsaturated, or a carboxyl-containing aromatic radical and n is an integer from 2 to 200, by polymerizing tetrahydrofuran, wherein the tetrahydrofuran, after removal of the catalyst used in the preparation of the tetrahydrofuran, is treated, before polymerization, with a strong mineral acid, an organic sulfonic acid, silica gel and/or a bleaching earth, the treating agent is removed from the tetrahydrofuran, and the tetrahydrofuran is then polymerized in the presence of one or more carboxylic acid anhydrides and a polymerization catalyst, the improvement which comprises: using the polymerization catalyst a bleaching earth containing less than 3% by weight of water, said catalyst being arranged in a fixed bed, and passing a mixture of pretreated tetrahydrofuran and carboxylic anhydride through said fixed bed.
Claim 2
Dependent Claim 166 words
In a process for the preparation of polybutylene glycol carboxylic acid diesters of the formula R--CO--O--CH.sub.2 CH.sub.2 CH.sub.2 CH.sub.2 --O).sub.n CO--R.sup.1 where R and R 1 are identical or different and each is alkyl, a carboxyl-containing aliphatic radical which may or may not be ethylenically unsaturated, or a carboxyl-containing aromatic radical and n is an integer from 2 to 200, by polymerizing tetrahydrofuran, wherein the tetrahydrofuran, after removal of the catalyst used in the preparation of the tetrahydrofuran, is treated, before polymerization, with a strong mineral acid, an organic sulfonic acid, silica gel and/or a bleaching earth, the treating agent is removed from the tetrahydrofuran, and the tetrahydrofuran is then polymerized in the presence of one or more carboxylic acid anhydrides and a polymerization catalyst, the improvement which comprises: using the polymerization catalyst a bleaching earth containing less than 3% by weight of water, said catalyst being arranged in a fixed bed, and passing a mixture of pretreated tetrahydrofuran and carboxylic anhydride through said fixed bed.
Claim 3
Dependent Claim 36 words
A process as set forth in claim 1, wherein the strong mineral acid, organic sulfonic acid, silica gel and/or bleaching earth is used in an amount of from 0.1 to 3% by weight, based on tetrahydrofuran.
Claim 4
Dependent Claim 18 words
A process as set forth in claim 1, wherein the treatment time is from 0.5 to 3 hours.
Claim 5
Dependent Claim 18 words
A process as set forth in claim 1, wherein the treatment temperature is from 10° to 66° C.
Claim 6
Dependent Claim 18 words
A process as set forth in claim 1, wherein acetic anhydride is used as the carboxylic acid anhydride.
Claim 7
Dependent Claim 47 words
A process as set forth in claim 1 wherein the bleaching earth catalyst is in the form of spheres, rings, cylinders or tablets, said spheres, rings, cylinders or tablets having been produced from commercial hydrated bleaching earths by compression molding, and dried at temperatures above 100° C.
Claim 8
Dependent Claim 27 words
A process as set forth in claim 6 wherein the bleaching earth is in the form of spheres having a diameter of from 2 to 15 mm.
Claim 9
Dependent Claim 20 words
A process as set forth in claim 7 wherein the spheres have a diameter of from 3 to 5 mm.
Claim 10
Dependent Claim 36 words
A process as set forth in claim 6 wherein the bleaching earth is in the form of cylinders having a length of from 2 to 15 mm and a diameter of from 2 to 6 mm.
Claim 11
Dependent Claim 27 words
A process as set forth in claim 1 wherein from 1 to 20% by weight of bleaching earth is used as a catalyst based on the tetrahydrofuran.
Claim 12
Dependent Claim 25 words
A process as set forth in claim 1 wherein the bleaching earth used as a catalyst contains from 0.001 to 1.5% by weight of water.

References Cited (Backward Citations)

US2499725A Cited
US2790813A Cited
US2856370A Cited
US3433829A Cited
US3935252A Cited
US3980672A Cited
GB1512528A Cited
DE2461922A1 Cited
US4163915A Cited
US4127513A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-01-06 1984-07-07 1985-01-06 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-01-06 1988-07-07 1989-01-06 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-01-06 1992-07-07 1993-01-06 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag