Filled arcylate and methacrylate films

• US 5,051,298 A
• Filed: 03/20/1989
• Issued: 09/24/1991
• Est. Priority Date: 03/20/1989
• Status: Expired due to Term

• Current Assignee: Eastman Kodak Company
• Original Assignee: Eastman Kodak Company
• Inventors: Coltrain, Bradley K., Landry, Christine J. T.
• Primary Examiner(s): NOT, DEFINED
• Assistant Examiner(s): NOT, DEFINED
• Application Number:
  US07/326,359
• Time in Patent Office: 918 Days
• Field of Search: 524/493, 524/560, 427/376.2, 428/331, 428/220, 264/2.6, 264/204, 264/331.18
• US Class Current: 428/220
• CPC Class Codes: C08J 2333/06 of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
• CPC Class Codes: C08J 5/18 Manufacture of films or sheets
• CPC Class Codes: C08K 3/36 Silica
• CPC Class Codes: C08L 33/06 of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
• CPC Class Codes: Y10T 428/259 Silicic material

Abstract

Free standing, optically clear, poly(acrylate) or poly(methacrylate) film having dispersed therein silica which is produced in situ from an alkoxysilane, using acid catalysis and a substantially stoichiometric amount of water for hydrolysis. The film forming process comprises a drying and curing step conducted in an open system. The temperatures and pH employed determine the nature and morphology of the dispersed silica phase. The film-forming process is conducted in the substantial absence of a polymerizable substance other than the alkoxysilane.

Claims

1. A free standing, optically clear, film having a thickness of about 1 to about 500 microns, said film consisting essentially of a poly(acrylate) or poly(methacrylate) polymer, having substantially uniformly dispersed therein, particles of an in situ produced, silicon oxide, said particles having a size less than about 0.1 micron;

the concentration of said particles in said film being in the range of from about 10 to about 65 weight percent based on the weight of the polymer;

said film being further characterized by having no designed covalent linkage between said silicon oxide and said polymer;

said film having been derived by a process comprising (a) hydrolyzing and condensing a tetra(lower alkyl)orthosilicate (i) in the substantial absence of a polymerizable substance other than said silicate, (ii) using acidic hydrolysis, (iii) and using a stoichiometric or substantially stoichiometric amount of water for hydrolysis, (iv) and in an organic solution of said polymer, the solvent in said solution having a relatively low boiling point, a fairly high volatility, and being substantially inert and miscible with water; and

(b) subsequently coating the composition thereby produced on a heated non-sticking surface having a temperature of about 30°

to about 35°

C.;

(c) drying and curing the coat on said surface to produce said film; and

(d) subsequently removing said film from said surface.

2. A film in accordance with claim 1 wherein said polymer is poly(methyl methacrylate).

3. A film in accordance with claim 2 wherein the concentration of said silicon oxide is from about 20 to about 50 weight percent.

4. Process for the preparation of an optically clear, free standing film, said process comprising (a) hydrolyzing and condensing a tetra(lower alkyl)orthosilicate (i) in the substantial absence of a polymerizable substance other than said silicate, (ii) using acidic hydrolysis, (iii) and using a stoichiometric or substantially stoichiometric amount of water for hydrolysis, (iv) and in an organic solution of a polymer selected from the group consisting of poly(acrylates) and poly(methacrylates), the solvent in said solution having a relatively low boiling point, a fairly high volatility, and being substantially inert and miscible with water;

(b) and subsequently coating the composition thereby produced on a heated non-sticking surface having a temperature of about 30°

to about 35°

C.;

(c) drying and curing the coat on said surface to produce said film; and

(d) subsequently removing said film from said surface.

5. Process of claim 4 wherein said polymer is poly(methyl methacrylate).

6. The process of claim 4 wherein said orthosilicate is selected from the group consisting of tetramethylorthosilicate and tetraethylorthosilicate.

7. The process of claim 4 wherein the concentration of said polymer in said organic solution is from about 1 to about 50 weight percent.

8. The process of claim 4 wherein the concentration of orthosilicate in said solution is sufficient to yield about 10 to about 65 weight percent (calculated as SiO₂) of an inorganic dispersed phase in said film.

9. Process of claim 4 wherein said organic film comprises tetrahydrofuran as a solvent.