Structural materials and components

• US 4,353,998 A
• Filed: 09/28/1981
• Issued: 10/12/1982
• Est. Priority Date: 09/12/1980
• Status: Expired due to Fees

• Current Assignee: Iml Corp. (Itochu Corporation)
• Original Assignee: International Harvester Co. (CNH Industrial N.V.)
• Inventors: Lee, Raymond, Gagliani, John
• Primary Examiner(s): Foelak, Morton
• Application Number:
  US06/306,363
• Time in Patent Office: 379 Days
• Field of Search: 260/37 N, 523/219, 524/600, 521/54, 521/180, 521/183, 521/184, 521/189
• US Class Current: 523/219
• CPC Class Codes: C08K 7/28 Glass
• CPC Class Codes: C08L 79/08 Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors

Abstract

High density structural ("blocking") materials composed of a polyimide filled with glass microballoons. Structural components such as panels which have integral edgings and/or other parts made of the high density materials.

Claims

1. A process of making a blocking material or the like which comprises the steps of forming a polyimide precursor, blending glass microballoons with said precursor, and converting said precursor to a polyimide, said polyimide precursor containing three different primary diamines, one of said diamines being heterocyclic and having nitrogen in the ring, another of said diamines being a para- or meta-substituted aromatic diamine which is free of aliphatic moieties, the third of said diamines being aliphatic, and said precursor being prepared by dissolving the primary diamines and one or more tetracarboxylic acids or anhydrides thereof in essentially stoichiometric proportions in a lower alkyl alcohol or mixture of such alcohols.

2. A process of making a blocking material as defined in claim 1 wherein the tetracarboxylic acid is 3,3'"'"',4,4'"'"'-benzophenonetetracarboxylic acid and said precursor contains from 0.05 to 0.3 mole of aliphatic diamine and from 0.1 to 0.3 mole of heterocyclic diamine per mole of 3,3'"'"',4,4'"'"'-benzophenonetetracarboxylic acid constituent.

3. A process of making a blocking material as defined in either of the preceding claims 1 or 2 wherein the aliphatic diamine in the precursor has from three to twelve carbon atoms.

4. A process of making a blocking material as defined in either of the preceding claims 1 or 2 wherein the aliphatic diamine in the precursor has the formula ##STR2## where x is on the order of 2.6.

7. A process of making a blocking material as defined in either of the preceding claims 1 or 5 wherein the aromatic and heterocyclic diamines in the precursor are selected from the following group:

2,6-diaminopyridine

3,5-diaminopyridine

3,3'"'"'-diaminodiphenyl sulfone

4,4'"'"'-diaminodiphenyl sulfone

4,4'"'"'-diaminodiphenyl sulfide

3,3'"'"'-diaminodiphenyl ether

4,4'"'"'-diaminodiphenyl ether

meta-phenylene diamine

para-phenylene diamine

p,p'"'"'-methylene dianiline

9. A process of making a blocking material as defined in either of the preceding claims 1 or 5 wherein said precursor is diluted with a lower alkyl alcohol in a ratio of 20 to 30 parts of alcohol to 100 parts of precursor before the microballoons are blended with said precursor.

10. A process of making a blocking material as defined in either of the preceding claims 1 or 5 wherein the precursor is converted to a polyimide by heating it at a temperature of 230°

-315°

C. for 15 to 30 minutes.

11. A process of making a blocking material as defined in either of the preceding claims 1 or 5 wherein the precursor is converted to a polyimide by heating it first at a temperature of 104°

to 163°

C. for 15 to 30 minutes and then at a temperature of 288°

to 315°

C. for 30 to 60 minutes.

12. A process of making a blocking material as defined in either of the preceding claims 1 or 5 wherein said precursor is converted to a polyimide by exposing it to microwave radiation for 2 to 12 minutes at a power output of 3.75 to 15 kW.

13. A method of making a blocking material as defined in claim 11 which employs a microwave radiation power output to unit weight of polyimide precursor ratio in the range of 0.6 to 1 kW/kg.

14. A method of making a blocking material as defined in claim 11 wherein the precursor is exposed to pulses of microwave radiation, the duration of the pulses and of the intervals therebetween being on the order of 60 and 20 seconds, respectively.

15. A method of making a blocking material as defined in claim 11 in which the precursor is exposed to microwave radiation in a microwave cavity and wherein the cavity is heated to a temperature of at least 250°

F. and less than 450°

F. while the precursor is exposed to said microwave radiation.

16. A method of making a blocking material as defined in claim 11 wherein a conductive filler is admixed with said precursor prior to exposing it to microwave radiation to promote the conversion of the precursor to a polymeric material.

17. A method of making a blocking material as defined in claim 11 wherein the material produced by exposing the precursor to microwave radiation is thereafter postcured by heating it at a temperature on the order of 250°

-550°

F. for 40 to 200 minutes.

18. A method of making a blocking material as defined in claim 11 wherein, while said precursor is exposed to microwave radiation, it is supported on or confined by an inflexible temperature resistant material that is compatible with such radiation, said material being a polypropylene lined with a fluorocarbon polymer coated glass, a glass based crystalline ceramic, or a glass filled polyimide.

19. A process of making a blocking material as defined in either of the preceding claims 1 or 5 wherein solvent is evaporated from the polyimide precursor-microballoon formulation before the precursor is converted to a polyimide, said evaporation of solvent being effected by heating said formulation at a temperature of 70°

to 93°

C. until from 29 to 31 percent of the solvent has been evaporated.

20. A process of making a blocking material as defined in either of the preceding claims 1 or 5 wherein solvent is evaporated from the polyimide precursor-microballoon formulation before the precursor is converted to a polyimide, said evaporation of solvent being effected by exposing said formulation to microwave radiation for 2 to 12 minutes at a power output of 1.25 to 2.5 kW.

5. A process of making a blocking material or the like which comprises the steps of forming a polyimide precursor, blending glass microballoons with said precursor, and converting said precursor to a polyimide, said polyimide precursor containing two different primary diamines, one of said diamines being heterocyclic and having nitrogen in the ring and the other of said diamines being a para- or meta-substituted aromatic diamine which is free of aliphatic moieties, and said precursor being prepared by dissolving the primary diamines and one or more tetracarboxylic acids or anhydrides thereof in essentially stoichiometric proportions in a lower alkyl alcohol or mixture of such alcohols.

6. A process of making a blocking material as defined in claim 5 wherein the tetracarboxylic acid is 3,3'"'"'4,4'"'"'-benzophenonetetracarboxylic acid and wherein said heterocyclic diamine is present is said precursor in a ratio of 0.3 to 0.6 mole of that diamine per mole of 3,3'"'"',4,4'"'"'-benzophenonetetracarboxylic acid constituent.

8. 6-diamino toluene

2,4-diamino toluene.