In-Line Chemical Composition Monitoring for the Injection Molding Process of Biodegradable Polymer Blends Using Simultaneous Measurement of Near-Infrared Diffuse Reflectance and Transmission Spectra

Abstract

In the processing of polymer blends and composites, in-line near-infrared (NIR) spectroscopy enables monitoring of the composition and its composite uniformity and contributes to rapid process development and quality control. However, in the injection molding process, the study of the composition of polymer materials has been delayed due to high-pressure conditions. Our research group developed NIR probes for transmission and diffuse reflectance measurements that can withstand high-pressure and temperature conditions up to 130 MPa and 200 °C. In this research, transmission and diffuse reflectance spectra were measured inline during the injection molding process of polymer blends of poly(lactic acid) and polybutylene succinate adipate. The intensity of each polymer band in the second-derivative spectra exhibited a monotonic increase or decrease in response to changes in the blend ratio. Using transmission and diffuse reflectance spectra as explanatory variables of the partial least squares regression model simultaneously, the model showed high estimation accuracy for the entire region of the blend ratio. Finally, this model was applied to monitor the polymer changeover operation, and the change in the blend ratio in the molded product was successfully estimated in line.

Graphical abstract

This is a visual representation of the abstract.

Keywords

In-line monitoring near-infrared spectroscopy NIR spectroscopy injection molding biodegradable polymer blends

Get full access to this article

View all access options for this article.

References

Dean

. “Polymer Blends and Composites from Renewable Resources”. Prog. Polym. Sci. 2006. 31(6): 576–602. https://doi.org/10.1016/j.progpolymsci.2006.03.002

Saini

Arora

Kumar

M.N.V.R.

. “Poly(Lactic Acid) Blends in Biomedical Applications”. Adv. Drug Deliv. Rev. 2016. 107(15): 47–59. https://doi.org/10.1016/j.addr.2016.06.014

Muthuraj

Misra

Mohanty

A.K.

. “Biodegradable Compatibilized Polymer Blends for Packaging Applications: A Literature Review”. J. Appl. Polym. Sci. 2018. 135(24): 45726. https://doi.org/10.1002/app.45726

Kuhnert

Sporer

Brunig

An Tran

N.H.

Rudolph

. “Processing of Poly(Lactic Acid)”. In: Di Lorenzo

M.L.

Androsch

, editors. Industrial Applications of Poly(Lactic Acid). Cham: Springer, 2018. Chap. 1, Pp. 1–33. https://doi.org/10.1007/12_2017_30

Masutani

Kimura

. “Present Situation and Future Perspectives of Poly(Lactic Acid)”. In: Di Lorenzo

M.L.

Androsch

, editors. Synthesis, Structure, and Properties of Poly(Lactic Acid). Cham: Springer, 2018. Chap. 1, Pp. 1–25. https://doi.org/10.1007/12_2016_16

Correlo

V.M.

Boesel

L.F.

Bhattacharya

Mano

J.F.

, et al. “Properties of Melt Processed Chitosan and Aliphatic Polyester Blends”. Mater. Sci. Eng. A. 2005. 403(1–2): 57–68. https://doi.org/10.1016/j.msea.2005.04.055

Bhatia

Gupta

R.K.

Bhaftacharya

S.N.

Choi

H.J.

. “Compatibility of Biodegradable Poly (Lactic Acid) (PLA) and Poly(Butylene Succinate) (PBS) Blends for Packaging Application”. Korea-Aust. Rheol. J. 2007. 19(3): 125–131.

Yokohara

Yamaguchi

. “Structure and Properties for Biomass-Based Polyester Blends of PLA and PBS”. Eur. Polym. J. 2008. 44(3): 677–685. https://doi.org/10.1016/j.eurpolymj.2008.01.008

Ojijo

Rinha Ray

Sadiku

. “Role of Specific Interfacial Area in Controlling Properties of Immiscible Blends of Biodegradable Polylactide and Poly[(Butylene Succinate)-Co-Adipate]”. ACS Appl. Mater. Interfaces. 2012. 4(12): 6690–6701. https://doi.org/10.1021/am301842e

10.

Ojijo

Ray

S.S.

Sadiku

. “Toughening of Biodegradable Polylactide/Poly(Butylene Succinate-Co-Adipate) Blends via In Situ Reactive Compatibilization”. ACS Appl. Mater. Interfaces. 2013. 5(10): 4266–4276. https://doi.org/10.1021/am400482f

11.

Kim

Hikima

Ohshima

. “Millefeuille-Like Cellular Structures of Biopolymer Blend Foams Prepared by the Foam Injection Molding Technique”. J. Appl. Polym. Sci. 2021. 139(14): 51890. https://doi.org/10.1002/app.51890

12.

Rhim

J.W.

Hong

S.-I.

Tan

C.-S.

. “Tensile, Water Vapor Barrier and Antimicrobial Properties of PLA/Nanoclay Composite Films”. LWT-Food Sci. Technol. 2009. 42(2): 612–617. https://doi.org/10.1016/j.lwt.2008.02.015

13.

Jonobi

Harun

Mathew

A.P.

Oksman

. “Mechanical Properties of Cellulose Nanofiber (CNF) Reinforced Polylactic Acid (PLA) Prepared by Twin Screw Extrusion”. Compos. Sci. Technol. 2010. 70(12): 1742–1747. https://doi.org/10.1016/j.compscitech.2010.07.005

14.

Fortunati

Peltzer

Armentano

Torre

, et al. “Effects of Modified Cellulose Nanocrystals on the Barrier and Migration Properties of PLA Nano-Biocomposites”. Carbohydr. Polym. 2012. 90(2): 948–956. https://doi.org/10.1016/j.carbpol.2012.06.025

15.

Rohe

Becker

Krey

Nägele

, et al. “In-Line Monitoring of Polymer Extrusion Processes by NIR Spectroscopy”. J. Near-Infrared Spectrosc. 1998. 6(1): 325–332. https://doi.org/10.1255/jnirs.153

16.

Rohe

Becker

Kölle

Eisenreich

Eyerer

. “Near Infrared (NIR) Spectroscopy for In-Line Monitoring of Polymer Extrusion Processes”. Talanta. 1999. 50(2): 283–290. https://doi.org/10.1016/S0039-9140(99)00035-1

17.

Barnes

S.E.

Sibley

M.G.

Edwards

H.G.M.

Coates

P.D.

. “Process Monitoring of Polymer Melts Using In-Line Spectroscopy”. Trans. Inst. Meas. Control (London). 2007. 29(5): 453–465. https://doi.org/10.1177/0142331207084336

18.

Zhang

Lei

Lin

, et al. “In-Line Characterization of Dispersion Uniformity Evolution During a Twin-Screw Blending Extrusion Based on Near-Infrared Spectroscopy”. Polym. Eng. Sci. 2020. 60(9): 2087–2096. https://doi.org/10.1002/pen.25453

19.

Zhu

Xiao

Wang

Jin

. “The Potential of Near-Infrared Diffuse Reflectance Spectroscopy as a Tool for Characterizing the Particle Size of Dispersion Phase in Polymer Blends”. Polymer. 2023. 283(22): 126289. https://doi.org/10.1016/j.polymer.2023.126289

20.

Reshadat

Desa

Joseph

Mehra

, et al. “In-Line Near-Infrared Monitoring of Polymer Processing. Part I: Process/Monitor Interface Development”. Appl. Spectrosc. 1999. 53(11): 1412–1418. https://doi.org/10.1366/0003702991945768

21.

Apruzzese

Reshadat

Balke

S.T.

. “In-Line Monitoring of Polymer Processing. II: Spectral Data Analysis”. Appl. Spectrosc. 2002. 56(10): 1268–1274. https://doi.org/10.1366/000370202760354713

22.

Watari

Ozaki

. “Calibration Models for the Vinyl Acetate Concentration in Ethylene–Vinyl Acetate Copolymers and Its On-Line Monitoring by Near-Infrared Spectroscopy and Chemometrics: Use of Band Shifts Associated with Variations in the Vinyl Acetate Concentration to Improve the Models”. Appl. Spectrosc. 2005. 59(7): 912–919. https://doi.org/10.1366/0003702054411571

23.

Watari

Ozaki

. “Prediction of Ethylene Content in Melt-State Random and Block Polypropylene by Near-Infrared Spectroscopy and Chemometrics: Influence of a Change in Sample Temperature and Its Compensation Method”. Appl. Spectrosc. 2005. 59(5): 600–610. https://doi.org/10.1366/0003702053946038

24.

Huang

Lei

Wang

Jin

. “In-Line Monitoring of Component Content of Polypropylene/Polystyrene Blends During Melt Extrusion Using Raman Spectroscopy”. J. Raman Spectrosc. 2018. 49(3): 513–519. https://doi.org/10.1002/jrs.5309

25.

Lei

Huang

Guo

Wang

Zhu

, et al. “Application of Raman Spectroscopy for In-Line Measurement of Dispersion Uniformity of Polypropylene–Polystyrene Blends During Melt Extrusion”. Appl. Spectrosc. 2018. 72(10): 1503–1510. https://doi.org/10.1364/AS.72.001503

26.

Fischer

Sahre

Abdelrhim

Voit

, et al. “Process Monitoring of Polymers by In-Line ATR-IR, NIR, and Raman Spectroscopy and Ultrasonic Measurements”. C.R. Chim. 2006. 9(11): 1419–1424. https://doi.org/10.1016/j.crci.2006.06.006

27.

Barnes

S.E.

Brown

E.C.

Sibley

M.G.

Edwards

H.G.M.

, et al. “Vibrational Spectroscopic and Ultrasound Analysis for In-Process Characterization of High-Density Polyethylene/Polypropylene Blends During Melt Extrusion”. Appl. Spectrosc. 2016. 59(5): 611–619. https://doi.org/10.1366/0003702053946001

28.

Dumitrescu

O.R.

Baker

D.C.

Foster

G.M.

Evans

K.E.

. “Near Infrared Spectroscopy for In-Line Monitoring During Injection Moulding”. Polym. Test. 2005. 24(3): 367–375. https://doi.org/10.1016/j.polymertesting.2004.10.003

29.

Ghita

O.R.

Baker

D.C.

Evans

K.E.

. “An In-Line Near-Infrared Process Control Tool for Monitoring the Effects of Speed, Temperature, and Polymer Colour in Injection Moulding”. Polym. Test. 2008. 27(4): 459–469. https://doi.org/10.1016/j.polymertesting.2008.01.010

30.

McLauchlin

A.R.

Ghita

O.R.

Gahkani

. “Quantification of PLA Contamination in PET During Injection Moulding by In-Line NIR Spectroscopy”. Polym. Test. 2014. 38(6): 46–52. https://doi.org/10.1016/j.polymertesting.2014.06.007

31.

Yoshikawa

Hosoe

Hikima

Watari

Ohshima

. “In-Line Monitoring of the Physical Blowing Agent Concentration by Transmission Near-Infrared Spectroscopy with High-Pressure Resistance Fiber Optic Probes for Foam Injection Molding Processes”. Ind. Eng. Chem. Res. 2023. 62(15): 6338–6346. https://doi.org/10.1021/acs.iecr.3c00216

32.

Becker

Inone-Kauffmann

Eckl

Eisenreich

. “Near Infrared Spectroscopy as a Tool for In-Line Control of Process and Material Properties of PLA Biopolymer”. Tech. Mess. 2015. 82(12): 653–662. https://doi.org/10.1515/teme-2015-0041

33.

Ishikawa

Furukawa

Wei

T.T.

Reddy

K.R.

, et al. “High-Speed Monitoring of the Crystallinity Change in Poly(Lactic Acid) During Photodegradation by Using a Newly Developed Wide Area NIR Imaging System (Compovision)”. Anal. Bioanal. Chem. 2015. 407(2): 397–403. https://doi.org/10.1007/s00216-014-8211-z

34.

Savitzky

Golay

M.J.E.

. “Smoothing and Differentiation of Data by Simplified Least Squares Procedures”. Anal Chem. 1964. 36(8): 1627–1639. https://doi.org/10.1021/ac60214a047

35.

Wold

. “Estimation of Principal Components and Related Models by Iterative Least Squares”. In: Krishnajah

P.R.

, editors. Multivariate Analysis. New York: Academic Press, 1966. Pp. 391–420.

36.

Wold

Ruhe

Wold

Dunn

W.J.

III . “The Collinearity Problem in Linear Regression. The Partial Least Squares (PLS) Approach to Generalized Inverses”. SIAM J. Sci. Stat. Comput. 1984. 5(3): 735–743. https://doi.org/10.1137/0905052

37.

Barnes

R.J.

Dhanoa

M.S.

Lister

S.J.

. “Standard Normal Variate Transformation and De-Trending of Near-Infrared Diffuse Reflectance Spectra”. Appl. Spectrosc. 1989. 43(5): 772–777. https://doi.org/10.1366/0003702894202201

38.

Jiang

J.-H.

Berry

R.J.

Siesler

H.W.

Ozaki

. “Wavelength Interval Selection in Multicomponent Spectral Analysis by Moving Window Partial Least-Squares Regression with Applications to Mid-Infrared and Near-Infrared Spectroscopic Data”. Anal. Chem. 2002. 74(14): 3555–3565. https://doi.org/10.1021/ac011177u

Supplementary Material

Please find the following supplemental material available below.

For Open Access articles published under a Creative Commons License, all supplemental material carries the same license as the article it is associated with.

For non-Open Access articles published, all supplemental material carries a non-exclusive license, and permission requests for re-use of supplemental material or any part of supplemental material shall be sent directly to the copyright owner as specified in the copyright notice associated with the article.

0.00 MB

0.27 MB