Poly(meth)acrylimide having improved optical and color properties, particularly under thermal load
View Patent ↗Process for preparing molding materials MM with improved optical and color properties, consisting of a polymer PM which contains units of the formula I in which R 1 and R 2 are each hydrogen and methyl and R 3 is hydrogen, C 1 -C 18 -alkyl, C 5 -C 8 -cycloalkyl, C 6 -C 10 -aryl, C 6 -C 10 -aryl-C 1 -C 4 -alkyl, where these radicals may be up to trisubstituted by radicals selected from the group consisting of C 1 -C 4 -alkoxy and halogen, prepared in an imidation reaction known per se in a reactive extruder, in which, on completion of the imidation reaction, an amount of one or more reducing phosphorus compounds P which is effective for color stabilization is added to the polymer PM, characterized in that the phosphorus compounds are organic phosphorus compounds OP selected from the group consisting of compounds of the formula II in which R 4 and R 5 are each independently hydrogen or an aromatic 6-membered ring which may be up to pentasubstituted by a C 1 -C 4 -alkyl and/or C 5 -C 8 -cycloalkyl groups. Shaped bodies obtainable by the process, especially light waveguides, have a low tendency to yellowing under thermal stress, coupled with a low haze, and also a stable and high transparency.
1. A process for preparing a stabilized molding composition, the molding composition comprising:
a polymer comprising units of formula I:
wherein
R 1 and R 2 are each hydrogen or methyl and
R 3 is hydrogen, optionally substituted C 1 -C 18 -alkyl, optionally substituted C 5 -C 8 -cycloalkyl, optionally substituted C 6 -C 10 -aryl, or optionally substituted C 6 -C 10 -aryl-C 1 -C 4 -alkyl, optionally substituted with up to trisubstituted by radicals selected from the group consisting of C 1 -C 4 -alkoxy and halogen, and
at least one reducing organic phosphorous compound
of formula II:
wherein
R 4 is hydrogen or an aromatic 6-membered ring optionally up to pentasubstituted by at least one of C 1 -C 4 -alkyl and C 5 -C 8 -cycloalkyl groups,
R 5 is an aromatic 6-membered ring optionally up to pentasubstituted by at least one of C 1 -C 4 -alkyl and C 5 -C 8 -cycloalkyl groups,
and
R 6 is hydrogen, an alkali metal, an alkaline earth metal, aluminum, ammonium or ammonium optionally substituted with up to four of at least one selected from C 1 to C 4 alkyl and C 5 to C 8 cycloalkyl groups;
the process comprising:
adding the at least one reducing organic phosphorous compound to the polymer after completion of an imidation reaction from which the polymer is obtained.
2. The process according to claim 1 , wherein the at least one reducing organic phosphorus compound is added in an amount of 0.005 to 1% by weight, based on the polymer weight.
3. The process according to claim 2 , wherein the amount of the at least one reducing organic phosphorus compound is from 0.005% to 0.3% by weight, based on the polymer.
4. The process according to claim 1 , wherein the at least one reducing organic phosphorus compound of formula (II) is benzenephosphinic acid.
5. The process according to claim 1 , wherein the at least one reducing organic phosphorus compound of formula (II) comprises benzenephosphinic acid and sodium benzenephosphinate.
6. The process according to claim 1 , wherein the at least one reducing organic phosphorus compound is added in alcoholic solution.
7. The process according to claim 2 , wherein the at least one reducing organic phosphorus compound is added to a particulate form of the polymer by mixing, optionally with a cavity transfer mixer.
8. The process according to claim 1 , wherein the at least one reducing organic phosphorus compound is added to a melt of the polymer wherein the polymer is freed of volatile constituents.
9. The process according to claim 8 , wherein the at least one reducing organic phosphorus compound is added continuously to a vented extruder connected downstream of a reaction extruder.
10. A shaped body obtained by molding the stabilized molding composition prepared according to claim 1 .
11. The shaped body according to claim 10 , wherein a yellowness index is less than 2.
12. The shaped body according to claim 11 , wherein a haze value is less than 1.5%.
13. The shaped body according to claim 12 , wherein the haze value is less than 1%.
14. The shaped body according to claim 10 , wherein a transparency of the shaped body is from greater than 89% to 92%.
15. The shaped body according claim 14 wherein the transparency is from greater than 90.5% to 92%.
16. The shaped body according to claim 10 , wherein the shaped body is a light waveguide.
17. The process according to claim 2 , wherein the at least one reducing organic phosphorus compound is benzenephosphinic acid.
18. The process according to claim 3 , wherein the at least one reducing organic phosphorus compound is benzenephosphinic acid.
19. The process according to claim 2 , wherein the at least one reducing organic phosphorus compound comprises benzenephosphinic acid and sodium benzenephosphinate.
20. A process for preparing molding materials, the molding material consisting of a polymer comprising units of formula I
wherein
R 1 and R 2 are each independently hydrogen or methyl and
R 3 is hydrogen, C 1 -C 18 -alkyl, C 5 -C 8 -cycloalkyl, C 6 -C 10 -aryl, or C 6 -C 10 -aryl-C 1 -C 4 -alkyl, optionally, up to trisubstituted by radicals selected from the group consisting of C 1 -C 4 -alkoxy and halogen, prepared in an imidation reaction in a reactive extruder,
the process comprising, on completion of the imidation reaction,
adding to the polymer an amount of at least one reducing phosphorus compound effective for color stabilization, the at least one phosphorus compound being an organic phosphorus compound selected from the group consisting of compounds of formula II
wherein
R 4 is hydrogen or an aromatic 6-membered ring which may be up to pentasubstituted by a C 1 -C 4 -alkyl and/or C 5 -C 8 -cycloalkyl groups,
R 5 is an aromatic 6-membered ring optionally up to pentasubstituted by at least one of C 1 -C 4 -alkyl and C 5 -C 8 -cycloalkyl groups,
and
R 6 is hydrogen, an alkali metal, an alkaline earth metal, aluminum, ammonium or ammonium optionally substituted with up to four of at least one selected from C 1 to C 4 alkyl and C 5 to C 8 cycloalkyl groups.