Method for producing polyamide-imide film

Patent metadata

Field	Value
Publication number	US-11433573-B2
Application number	US-201816480853-A
Country	US
Kind code	B2
Filing date	Feb 6, 2018
Priority date	Feb 8, 2017
Publication date	Sep 6, 2022
Grant date	Sep 6, 2022

Abstract

An embodiment can provide a method for producing a polyamide-imide film which is colorless and transparent and has excellent mechanical properties, the method comprising: a step of producing a polyamide-imide polymer solution by polymerizing an aromatic diamine compound, an aromatic dianhydride compound, and a dicarbonyl compound; a step of producing a gel sheet by extruding, casting and drying the polymer solution; and a step of producing a polyamide-imide film by heat-treating the gel sheet, wherein the viscosity of the polymer solution is 100,000 to 500,000 cps, and the polyamide-imide film has a yellowness index of 5 or lower, a haze of 2% or lower, a transmittance of 85% or above and a modulus of 5.0 GPa or above, at a thickness of 20 μm to 75 μm.

First claim

The invention claimed is:

1. A process for preparing a polyamide-imide film, which comprises:
polymerizing an aromatic diamine compound, an aromatic dianhydride compound, and a part of a dicarbonyl compound to produce a first polymer solution that has viscosity of 1,000 to 100,000 cps;
further adding the remaining part of the dicarbonyl compound to the first polymer solution to produce a polyamide-imide polymer solution that has viscosity of 100,000 to 500,000 cps;
extruding and casting the polymer solution and then drying the cast polymer solution to prepare a gel sheet; and
thermally treating the gel sheet to produce the polyamide-imide film,
wherein the polyamide-imide film has a yellow index of 5 or less, a haze of 2% or less, a transmittance of 85% or more, and a modulus of 5.0 GPa or more based on a thickness of 20 μm to 75 μm.

2. The process for preparing a polyamide-imide film of claim 1 , wherein in the step of preparing the polymer solution, the polymer solution comprises the polyamide-imide polymer and an organic solvent, and the content of the polyamide-imide polymer is 5% by weight to 20% by weight based on the total weight of the polymer solution.

3. The process for preparing a polyamide-imide film of claim 1 , wherein the polymer solution is cast at a rate of about 0.5 m/min to about 15 m/min and in a thickness of 300 to 600 μm onto a casting body.

4. The process for preparing a polyamide-imide film of claim 1 , wherein the polyamide-imide polymer solution comprises the aromatic dianhydride compound in an amount of 20% by mole to 50% by mole and the dicarbonyl compound in an amount of 50% by mole to 80% by mole based on the total moles of the aromatic dianhydride compound and the dicarbonyl compound.

5. The process for preparing a polyamide-imide film of claim 1 , wherein one kind of aromatic diamine is used as the aromatic diamine compound, and one kind of aromatic dianhydride is used as the aromatic diamine compound.

6. The process for preparing a polyamide-imide film of claim 1 , wherein the aromatic diamine compound comprises 2,2′-bis(trifluoromethyl)-4,4′-diaminobiphenyl (TFDB), and the aromatic dianhydride compound comprises 2,2′-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride (6-FDA).

7. The process for preparing a polyamide-imide film of claim 1 , wherein the dicarbonyl compound is at least one selected from the group consisting of 1,1′-biphenyl-4,4′-dicarbonyl dichloride (BPDC) and terephthaloyl chloride (TPC).

8. The process for preparing a polyamide-imide film of claim 1 , wherein the dicarbonyl compound comprises a first dicarbonyl compound and a second dicarbonyl compound, and
the step of preparing the polymer solution comprises polymerizing the aromatic diamine compound, the aromatic dianhydride compound, the first dicarbonyl compound, and the second dicarbonyl compound in an organic solvent to produce a first polymer solution; and
further adding the second dicarbonyl compound to the first polymer solution to produce a second polymer solution that has a viscosity of 100,000 to 500,000 cps.

9. The process for preparing a polyamide-imide film of claim 8 , wherein the step of producing the first polymer solution comprises simultaneously or sequentially polymerizing the aromatic diamine compound, the aromatic dianhydride compound, the first dicarbonyl compound, and the second dicarbonyl compound.

10. The process for preparing a polyamide-imide film of claim 9 , wherein the step of producing the first polymer solution comprises polymerizing the aromatic diamine compound and the aromatic dianhydride compound to produce a polyamic acid solution; and adding the first dicarbonyl compound and the second dicarbonyl compound to the polyamic acid solution to polymerize them.

11. The process for preparing a polyamide-imide film of claim 2 , wherein the organic solvent is at least one selected from the group consisting of dimethylformamide (DMF), dimethylacetamide (DMAc), N-methyl-2-pyrrolidone (NMP), m-cresol, tetrahydrofuran (THF), and chloroform.

12. The process for preparing a polyamide-imide film of claim 8 , wherein the first dicarbonyl compound and the second dicarbonyl compound are aromatic dicarbonyl compounds different from each other.

13. The process for preparing a polyamide-imide film of claim 8 , wherein the weight ratio of the second dicarbonyl compound added in the step of obtaining the first polymer solution to the second dicarbonyl compound added in the step of obtaining the second polymer solution is 90:10 to 99:1.

14. The process for preparing a polyamide-imide film of claim 8 , wherein the second dicarbonyl compound added in the step of obtaining the second polymer solution is in the form of a solution in which the second dicarbonyl compound is dissolved in an organic solvent at a concentration of 5 to 20% by weight.

15. The process for preparing a polyamide-imide film of claim 1 , wherein the viscosity of the polymer solution is 150,000 to 350,000 cps.

16. A process for preparing a polyamide-imide film, which comprises:
polymerizing an aromatic diamine compound, an aromatic dianhydride compound, and a dicarbonyl compound to prepare a polyamide-imide polymer solution;
extruding and casting the polymer solution and then drying the cast polymer solution to prepare a gel sheet; and
thermally treating the gel sheet to produce the polyamide-imide film,
wherein the step of preparing the polymer solution comprises:
polymerizing the aromatic diamine compound, the aromatic dianhydride compound, a part of the dicarbonyl compound to produce a first polymer solution that has a viscosity of 1,000 to 100,000 cps; and
further adding the remaining part of the dicarbonyl compound to the first polymer solution to produce a second polymer solution that has a viscosity of 150,000 to 350,000 cps;
the polymer solution comprises the polyamide-imide polymer and an organic solvent, the content of the polyamide-imide polymer is 5% by weight to 20% by weight based on the total weight of the polymer solution, and
the polyamide-imide film has a yellow index of 5 or less, a haze of 2% or less, a transmittance of 85% or more, and a modulus of 5.0 GPa or more based on a thickness of 20 μm to 75 μm.

17. The process for preparing a polyamide-imide film of claim 16 , wherein
the dicarbonyl compound comprises a first dicarbonyl compound and a second dicarbonyl compound, and
the part of the dicarbonyl compound in the step of producing the first polymer solution comprises the first dicarbonyl compound, and
the remaining part of the dicarbonyl compound in the step of producing the second polymer solution comprises the second dicarbonyl compound.

18. The process for preparing a polyamide-imide film of claim 17 , wherein the second dicarbonyl compound comprises terephthaloyl chloride.

Assignees

• Skc Co Ltd

Inventors

• Oh Dae Seong
• Jeong Dawoo
• Kim Sunhwan
• Lee Jin Woo
• Lim Dong Jin
• Kim Cheol Ho

Classifications

• B29K2079/085

  Thermoplastic polyimides, e.g. polyesterimides, PEI, i.e. polyetherimides, or polyamideimides; Derivatives thereof · CPC title

• C08L79/08

  Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors · CPC title

• B29C39/006 Primary

  Monomers or prepolymers (by reaction injection moulding B29C67/246) · CPC title

• B29C48/001

  Combinations of extrusion moulding with other shaping operations · CPC title

• C08G73/10 Primary

  Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors · CPC title