Process and formulation for producing a polyamide having low caprolactam concentration and specific relative viscosity
A base polyamide composition comprising a nylon mixture having caprolactam units from 1 wppb to 50 wppm catalyst composition; and greater than 0.75 wt % residual caprolactam, wherein the base polyamide composition has a delta end group level ranging from 30 μeq/gram to 90 μeq/gram.
1. A process for producing a polyamide composition having a low residual caprolactam concentration, the process comprising the steps of:
(a) providing a base polyamide composition, wherein the base polyamide composition has a delta end group level ranging from 30 μeq/gram to 90 μeq/gram, comprising:
a nylon mixture having caprolactam units;
from 1 wppb to 50 wppm of a catalyst composition; and
residual caprolactam, and having an initial residual caprolactam concentration and an initial relative viscosity;
(b) processing the base polyamide composition to form the final polyamide composition having a final residual caprolactam concentration and a final relative viscosity.
2. The process of claim 1 , wherein the initial residual caprolactam concentration is greater than 0.75 wt %, based on the total weight of the base polyamide composition, and wherein the final residual caprolactam concentration is less than 0.75 wt %, based on the total weight of the final polyamide composition.
3. The process of claim 1 , wherein the final relative viscosity ranges from 40 to 350.
4. The process of claim 1 , wherein the processing is conducted for a build time ranging from 2 hours to 30 hours, and a temperature ranging from 150° C.-250° C.
5. The process of claim 1 , wherein the final polyamide composition has a color index ranging from −6 to 5, as measured by ASTM E313 (2018).
6. The process of claim 1 , wherein the final relative viscosity is greater than the initial relative viscosity, wherein the final relative viscosity is at least 10% greater than the initial relative viscosity and the final residual caprolactam concentration is at least 5% less than the initial residual caprolactam concentration.
7. The process of claim 1 , wherein the base polyamide composition has a melting point ranging from 180° C. to 255° C.
8. The process of claim 1 , wherein processing comprises solid state polymerization, which comprises heating the base polyamide.
9. The process of claim 1 , wherein the catalyst composition comprises phosphorous acid; phosphonic acid; alkyl- and aryl-substituted phosphonic acids; 2-pyridylethyl phosphonic acid; hypophosphorous acid; alkyl-, aryl- and alkyl-/aryl-substituted phosphinic acids; phosphoric acid; esters and salts of these phosphorous-containing acids; manganese hypophosphite; sodium hypophosphite; benzene phosphinic acid; monosodium phosphate; or any combinations thereof.
10. The process of claim 1 , wherein the base polyamide composition comprises from 0.1 wppm to 35 wppm catalyst composition, from 1 wt % to 8 wt % residual caprolactam, has a delta end group level ranging from 50 μeq/gram to 75 μeq/gram, and has initial relative viscosity less than 35, and
wherein the final polyamide composition comprises less than 0.6 wt % residual caprolactam and has a final relative viscosity greater than 45.
11. The process of claim 1 , wherein the base polyamide composition comprises from 1 wppb to 15 wppm phosphorus, greater than 1.5 wt % residual caprolactam, a delta end group level greater than 50 μeq/gram and has initial relative viscosity less than 33,
wherein the processing is conducted at a pressure less than atmospheric pressure and a temperature ranging from 175° C. to 185° C., and
wherein the final polyamide composition comprises less than 0.4 wt % residual caprolactam and has a final relative viscosity greater than 55.
12. The process of claim 1 , wherein, during processing, the RV build rate ranges from 1 to 30 RV units/hour.