← Back to Patent Explorer
US3969325A Expired / Lapsed US ⏱️ 0.0 years remaining

Production of particulate BBB type polymer having an unusually high surface area

Assignee: Celanese Corp
•
Filing: 1973-12-14
•
Granted: 1976-07-13
•
Expires: 1993-12-14
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract An improved process is provided for the formation of BBB type polymer, i.e. poly(bisbenzimidazobenzophenanthroline) and related nitrogenous polymers, in finely divided form having an unusually high surface area. The condensation reaction of at least one organic tetra-amine and at least one tetracarboxylic acid (which optionally may be in the form of the corresponding half anhydride or dianhydride) is conducted at an elevated temperature with agitation in the presence of a major concentration of a liquid sulfone (e.g. diphenyl sulfone) which is inert under the reaction conditions. The resulting particulate product of BBB type polymer commonly exhibits a surface area of about 100 to 500, or more, square meters per gram, and may be used in the formation of pressure molded articles of high temperature resistance.

Inventors

  • 👤 Anthony B. Conciatori
  • 👤 Rufus S. Jones, Jr.

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-05 17:25
CPC Classifications
C; C08; C08G; C08G73/00; C08G73/06; C08G73/20

Claims Analysis

Total Claims: 18
Claim 1
Independent Claim 229 words
In a process for forming a BBB type polymer comprising condensing with intimate admixture a. at least one organic tetra-amine having the structural formula ##EQU6## wherein R is an aromatic or cycloaliphatic tetravalent radical and wherein each of the four amino groups is attached directly to a carbon atom present in a ring of said aromatic or cycloaliphatic radical in a position which is ortho or peri to another carbon atom to which another of said amino groups is also directly attached, and b. at least one tetracarboxylic acid or its corresponding half anhydride or dianhydride having the structural formula ##EQU7## wherein R' is a tetravalent aromatic or cycloaliphatic radical wherein each of the four carboxyl groups is attached directly to a carbon atom present in a ring of said aromatic or cycloaliphatic radical in a position which is ortho or peri to another carbon atom to which another of said carboxyl groups is also directly attached; the improvement of conducting said condensation with agitation at a temperature of about 300° to 450°C. in the presence of a major concentration of a liquid aryl sulfone which is inert under the reaction conditions, with said BBB type polymer upon formation assuming the configuration of a particulate solid having an unusually high surface area of 100 to 500 square meters per gram and an inherent viscosity of at least 0.2 dl./gram.
Claim 2
Dependent Claim 229 words
In a process for forming a BBB type polymer comprising condensing with intimate admixture a. at least one organic tetra-amine having the structural formula ##EQU6## wherein R is an aromatic or cycloaliphatic tetravalent radical and wherein each of the four amino groups is attached directly to a carbon atom present in a ring of said aromatic or cycloaliphatic radical in a position which is ortho or peri to another carbon atom to which another of said amino groups is also directly attached, and b. at least one tetracarboxylic acid or its corresponding half anhydride or dianhydride having the structural formula ##EQU7## wherein R' is a tetravalent aromatic or cycloaliphatic radical wherein each of the four carboxyl groups is attached directly to a carbon atom present in a ring of said aromatic or cycloaliphatic radical in a position which is ortho or peri to another carbon atom to which another of said carboxyl groups is also directly attached; the improvement of conducting said condensation with agitation at a temperature of about 300° to 450°C. in the presence of a major concentration of a liquid aryl sulfone which is inert under the reaction conditions, with said BBB type polymer upon formation assuming the configuration of a particulate solid having an unusually high surface area of 100 to 500 square meters per gram and an inherent viscosity of at least 0.2 dl./gram.
Claim 3
Dependent Claim 27 words
A process according to claim 1 wherein said organic tetra-amine and said tetracarboxylic acid or its corresponding half anhydride or dianhydride are provided in substantially stoichiometric concentrations.
Claim 4
Dependent Claim 22 words
A process according to claim 1 wherein said BBB type polymer is a condensation product of 3,3'-diamino benzidine and 1,4,5,8-naphthalene tetracarboxylic acid.
Claim 5
Dependent Claim 15 words
A process according to claim 1 wherein said condensation is conducted at substantially atmospheric pressure.
Claim 6
Dependent Claim 42 words
A process according to claim 1 wherein said liquid aryl sulfone possesses a boiling point in excess of the reaction temperature and is a solvent for said condensation reactants and a non-solvent for said BBB type polymer product at the reaction temperature.
Claim 7
Dependent Claim 26 words
A process according to claim 1 wherein said liquid aryl surfone is selected from the group consisting of diphenyl sulfone, 4,4' ditolyl sulfone and methylphenyl sulfone.
Claim 8
Dependent Claim 35 words
A process according to claim 1 wherein said condensation reactants are provided in a total concentration of about 5 to 25 percent by weight based upon total weight of said condensation reactants and said sulfone.
Claim 9
Dependent Claim 77 words
A process according to claim 1 wherein a low boiling organic solvent for said condensation reactants and for said aryl sulfone having a boiling point below about 200°C. and which is inert to said condensation reactants and said aryl sulfone initially is provided in admixture therewith prior to raising the temperature of said condensation reactants to said reaction temperature with said low boiling organic solvent being substantially volatilized prior to said condensation reactants reaching said reaction temperature.
Claim 10
Dependent Claim 34 words
A process according to claim 8 wherein said low boiling organic solvent is provided in a concentration of about 20 to 70 percent by weight based upon the total weight of said condensation reactants.
Claim 11
Dependent Claim 26 words
A process according to claim 1 wherein said condensation reactants are maintained at a temperature of about 300° to 450°C. for about 2.5 to 5 hours.
Claim 12
Dependent Claim 139 words
In a process for forming poly(bisbenzimidazobenzophenanthroline) comprising condensing with intimate admixture substantially stoichiometric amounts of (1) 3,3'-diamino benzidine and (2) 1,4,5,8-naphthalene tetracarboxylic acid; the improvement of conducting said condensation with agitation while at substantially atmospheric pressure and at a temperature of about 325° to 420°C. in the presence of a major concentration of a liquid aryl sulfone selected from the group consisting of diphenyl sulfone, 4,4'-ditolyl sulfone and methylphenyl sulfone, with said condensation reactants being provided in a total concentration of about 5 to 25 percent by weight based upon the total weight of said condensation reactants and said sulfone and with said BBB type polymer upon formation assuming the configuration of a particulate solid having an unusually high surface area of 100 to 500 square meters per gram and an inherent viscosity of about 0.4 to 2.5 dl./gram.
Claim 13
Dependent Claim 139 words
In a process for forming poly(bisbenzimidazobenzophenanthroline) comprising condensing with intimate admixture substantially stoichiometric amounts of (1) 3,3'-diamino benzidine and (2) 1,4,5,8-naphthalene tetracarboxylic acid; the improvement of conducting said condensation with agitation while at substantially atmospheric pressure and at a temperature of about 325° to 420°C. in the presence of a major concentration of a liquid aryl sulfone selected from the group consisting of diphenyl sulfone, 4,4'-ditolyl sulfone and methylphenyl sulfone, with said condensation reactants being provided in a total concentration of about 5 to 25 percent by weight based upon the total weight of said condensation reactants and said sulfone and with said BBB type polymer upon formation assuming the configuration of a particulate solid having an unusually high surface area of 100 to 500 square meters per gram and an inherent viscosity of about 0.4 to 2.5 dl./gram.
Claim 14
Dependent Claim 26 words
A process according to claim 11 wherein said sulfone is diphenyl sulfone and said condensation is carried out at a temperature of about 350° to 380°C.
Claim 15
Dependent Claim 76 words
A process according to claim 11 wherein a low boiling organic solvent for said condensation reactants and said aryl sulfone having a boiling point below about 200°C. and which is inert to said condensation reactants and said aryl sulfone initially is provided in admixture therewith prior to raising the temperature of said condensation reactants to said reaction temperature with said low boiling organic solvent being substantially volatilized prior to said condensation reactants reaching said reaction temperature.
Claim 16
Dependent Claim 23 words
A process according to claim 13 wherein said low boiling organic solvent is selected from the group consisting of para-xylene, chlorobenzene, and cumene.
Claim 17
Dependent Claim 34 words
A process according to claim 13 wherein said low boiling organic solvent is provided in a concentration of about 35 to 65 percent by weight based upon the total weight of said condensation reactants.
Claim 18
Dependent Claim 26 words
Particulate BBB type polymer having a surface area of about 200 to 350 square meters per gram formed in accordance with the process of claim 1.

References Cited (Backward Citations)

US3804804A Cited
US3784517A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-07-13 1980-01-12 1980-07-13 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-07-13 1984-01-12 1984-07-13 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-07-13 1988-01-12 1988-07-13 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag