Method for the production of block copolycarbonate/phosphonates and compositions therefrom
View Patent ↗Disclosed is a new method and compositions from the method consisting of block copolycarbonate/phosphonates that exhibit an excellent combination of flame resistance, hydrolytic stability, high Tg, low melt viscosity, low color and high toughness. Also disclosed are polymer mixtures or blends comprised of these block copolycarbonate/phosphonate compositions and commodity and engineering plastics and articles produced therefrom. Further disclosed are articles of manufacture produced from these materials, such as fibers, films, coated substrates, moldings, foams, adhesives and fiber-reinforced articles, or any combination thereof.
1. A method of preparing block copolycarbonate/phosphonates comprising;
obtaining a predominately phenol terminated oligocarbonate, and free bisphenol, in a first step; and
reacting the predominately phenol terminated oligocarbonate, and free bisphenol, with an alkylphosphonic acid diarylester at a temperature of from about 200° C. to about 310° C. under reduced pressure in a melt to make a hydrolytically stable, block copolycarbonate/phosphonate in a second step.
2. The method of claim 1 , wherein the elevated temperature and reduced pressure of the second step are such that volatile components are removed.
3. The method of claim 1 , wherein the method further comprises reacting a polycarbonate with a phenolic compound under conditions such that the phenolic compound is refluxing but is not removed to obtain the predominately phenol terminated oligocarbonate, and free bisphenol.
4. The method of claim 3 , wherein the phenolic compound is phenol.
5. The method of claim 3 , wherein the step of reacting the polycarbonate with the phenolic compound occurs in the presence of the alkylphosphonic acid diarylester.
6. The method of claim 3 , wherein the phenolic compound is provided at a molar ratio of about 0.1 to about 5 of the polycarbonate.
7. The method of claim 1 , wherein the method further comprises reacting diphenyl carbonate, a molar excess of a bisphenol, and a transesterification catalyst at elevated temperature under reduced pressure in a melt to obtain the predominately phenol terminated oligocarbonate, and free bisphenol.
8. The method of claim 7 , wherein the bisphenol is 2,2-bis(4-hydroxyphenyl)propane.
9. The method of claim 1 , wherein the alkylphosphonic acid diarylester is methylphosphonic acid diphenylester.
10. The method of claim 1 , wherein the alkylphosphonic acid diarylester is provided at a molar ratio of from about 0.1 to about 5 of the predominately phenol terminated oligocarbonate.
11. The method of claim 1 , further comprising providing a transesterification catalyst.
12. The method of claim 11 , wherein the transesterification catalyst is selected from sodium phenolate, tetraphenylphosphonium phenolate, or combinations thereof.
13. The method of claim 11 , wherein the transesterification catalyst is provided prior to the step of reacting.
14. The method of claim 11 , further comprising providing transesterification catalyst during the step of reacting.
15. The method of claim 1 , wherein the predominately phenol terminated oligocarbonate is selected from linear oligocarbonates, branched oligocarbonates, and combinations thereof.
16. The method of claim 1 wherein the predominately phenol terminated oligocarbonate has a relative viscosity (η rel ) of from about 1.02 to about 1.18.
17. The method of claim 1 , wherein the elevated temperature and reduced pressure are maintained from about 0.5 to about 24 hours.
18. The method of claim 1 , further comprising the step of heating a mixture resulting from the second step to a temperature of from about 250° C. to about 310° C. for from about 0.5 to about 10 hours.
19. The method of claim 1 , wherein from about 0.1% to about 10% by weight phosphorous is present in the block copolycarbonate/phosphonate.
20. The method of claim 1 , wherein from about 0.1 to about 5% by weight phosphorous is present in the block copolycarbonate/phosphonate.
21. A method for preparing block copolycarbonate/phosphonate comprising:
reacting a polycarbonate, a phenolic compound, and an alkylphosphonic acid diarylester in a first step under conditions such that the phenolic compound is refluxing but is not removed for a first time period; and
reacting a mixture resulting from the first step at a temperature of from about 200° C. to about 310° C. under reduced pressure such that volatile compounds are removed for a second time period to make a hydrolytically stable, block copolycarbonate/phosphonate in a second step.
22. The method of claim 21 , wherein oligocarbonates are formed in the first step.
23. The method of claim 21 , wherein the phenolic compound is phenol.
24. The method of claim 21 , wherein the alkylphosphonic acid diarylester is methylphosphonic acid diphenylester.