Polyester polymer nanocomposites
Aspects of the present disclosure include compositions of and methods for producing a polymer-polysaccharide nanocomposite resin, including polymerizing an alkane diol monomer and an alkane diacid agent monomer in a mixture comprising dispersed polysaccharide nanocrystals, a catalyst and one or more optional additives under conditions sufficient to produce a polymer-polysaccharide nanocomposite resin. Aspects of the present disclosure further include compositions of and methods for producing a polybutylene succinate nanocomposite, including dispersing cellulose nanocrystals in 1,4 butanediol (BDO) to form a cellulose-BDO dispersion and esterifying the cellulose-BDO dispersion and succinate anhydride to form a plurality of polybutylene succinate oligomers. The polybutylene succinate oligomers are condensed to form a polybutylene succinate nanocomposite.
1 . A method for producing a polymer-polysaccharide nanocomposite resin, the method comprising the steps of:
a) preparing and heating a mixture comprising a diacid agent monomer and 1,4-butane diol at a first temperature to esterify the diacid agent monomer and 1,4-butane diol;
b) contacting the heated mixture of step a) with a nanocellulose crystal (NCC) dispersion after esterification of the monomers to produce a NCC oligomeric composition; and
c) heating a second mixture comprising the NCC oligomeric composition and a catalyst at a second temperature and under reduced pressure to polycondense the NCC oligomeric composition and produce a polymer-cellulose nanocomposite resin.
2 . The method of claim 1 , wherein the first temperature is from 150° C. or more.
3 . The method of claim 1 , wherein the second temperature is from 200° C. or more.
4 . The method of claim 1 , wherein the diacid agent monomer is selected from succinic acid, monoalkyl succinate, dialkyl succinate, dimethyl succinate, diethyl succinate, and succinic anhydride.
5 . The method of claim 1 , wherein the NCC dispersion comprises 1,4-butanediol.
6 . The method of claim 1 , wherein the NCC dispersion comprises a 1,4-butanediol or a glycol solution.
7 . The method of claim 1 , wherein the NCC dispersion does not comprise water.
8 . The method of claim 1 , wherein the first temperature is 150° C. to 200° C.
9 . The method of claim 1 , wherein the second temperature is greater than the first temperature, and the second temperature is 200° C. to 250° C.
10 . The method of claim 1 , wherein the NCC oligomeric composition comprises oligomers having an average MW of 500 Da or more.
11 . The method of claim 4 , wherein the diacid agent monomer is selected from succinic acid, dimethyl succinate, and succinic anhydride.
12 . The method of claim 1 , wherein NCC oligomeric composition comprises a butylene succinate repeating unit and has an average MW of 1,000 to 10,000 Da.
13 . The method of claim 1 , wherein the second mixture of step c) further comprises an epoxidized oil.
14 . The method of claim 1 , wherein step a) or step b) further comprises the addition of a catalyst.
15 . The method of claim 14 , wherein the catalyst is added at the beginning of step a) or during step a).
16 . The method of claim 14 , wherein the catalyst is added at the beginning or during step b).
17 . The method of claim 1 , wherein the catalyst is a mixed metal oxide catalyst.
18 . The method of claim 17 , wherein the catalyst comprises zirconium.
19 . The method of claim 18 , wherein the catalyst comprises zirconium in an amount of 100 to 500 ppm.
20 . The method of claim 19 , wherein the catalyst comprises zirconium in an amount of 470 ppm.
21 . An article comprising the nanocomposite resin of claim 1 , wherein the article is manufactured from the nanocomposite resin using melt spinning, wherein the article is yarn or fiber.
22 . The method of claim 11 , wherein:
the first temperature is 150° C. to 200° C.; and
the second temperature is 200° C. to 250° C.
23 . The method of claim 22 , wherein the second mixture of step c) further comprises an epoxidized oil.
24 . The method of claim 23 , wherein step a) or step b) further comprises the addition of a catalyst.
25 . The method of claim 24 , wherein the catalyst is a mixed metal oxide catalyst comprising zirconium.