This readme.txt file was generated on <2023-07-30> by Recommended citation for the data: Shen, Liyang; Diaz Gorbea, Gabriela; Danielson, Evan; Cui, Shuquan; Ellison, Christopher J; Bates, Frank S. (2023). Data for Threading-the-Needle: Compatibilization of HDPE/iPP blends with butadiene-derived polyolefin block copolymers. Retrieved from the Data Repository for the University of Minnesota, https://doi.org/10.13020/3h6p-zn30. ------------------- GENERAL INFORMATION ------------------- 1. Title of Dataset: Data for "Threading-the-Needle: Compatibilization of HDPE/iPP blends with butadiene-derived polyolefin block copolymers 2. Author Information Principal Investigator Contact Information Name: Frank S. Bates Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: bates001@umn.edu Principal Investigator Contact Information Name: Christopher J. Ellison Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: cellison@umn.edu Associate or Co-investigator Contact Information Name: Liyang Shen Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: shen0481@umn.edu Associate or Co-investigator Contact Information Name: Gabriela Diaz Gorbea Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: diaz0276@umn.edu Associate or Co-investigator Contact Information Name: Evan Danielson Institution: University of Minnesota Address: Department of Chemical Engineering and Materials Science, 421 Washington Ave SE, Minneapolis, Minnesota 55455 Email: dani0968@umn.edu Associate or Co-investigator Contact Information Name: Shuquan Cui Institution: University of Minnesota Address: Department of Chemistry, 207 Pleasant St SE, Minneapolis, Minnesota 55455 Email: cui00123@umn.edu 3. Date published or finalized for release: 4. Date of data collection (single date, range, approximate date) : 20211101-20221101 5. Geographic location of data collection (where was data collected?): University of Minnesota 6. Information about funding sources that supported the collection of the data: Funding for this work was provided by the Center for Sustainable Polymers, a NSF-supported Center for Chemical Innovation (CHE- 1901635). Parts of the work were carried out in the Characterization Facility, University of Minnesota, which receives partial support from the NSF through the MRSEC (Award Number DMR-2011401) and the NNCI (Award Number ECCS- 2025124) programs. 7. Overview of the data (abstract): Management of the plastic industry is a momentous challenge, one that pits enormous societal benefts against an accumulating reservoir of nearly indestructible waste. A promising strategy for recycling polyethylene (PE) and isotactic polypropylene (iPP), constituting roughly half the plastic produced annually worldwide, is melt blending for reformulation into useful products. Unfortunately, such blends are generally brittle and useless due to phase separation and mechanically weak domain interfaces. Recent studies have shown that addition of small amounts of semicrystalline PE-iPP block copolymers (ca. 1 wt%) to mixtures of these polyolefns results in ductility comparable to the pure materials. However, current methods for producing such additives rely on expensive reagents, prohibitively impacting the cost of recycling these inexpensive commodity plastics. Here, we describe an alternative strategy that exploits anionic polymerization of butadiene into block copolymers, with subsequent catalytic hydrogenation, yielding E and X blocks that are individually melt miscible with PE and iPP, where E and X are poly(ethylene-ran-ethylethylene) random copolymers with 6% and 90% ethylethylene repeat units, respectively. Cooling melt blended mixtures of PE and iPP containing 1 wt% of the triblock copolymer EXE of appropriate molecular weight, results in mechanical properties competitive with the component plastics. Blend toughness is obtained through interfacial topological entanglements of the amorphous X polymer and semicrystalline iPP, along with anchoring of the E blocks through cocrystallization with the PE homopolymer. Signifcantly, EXE can be inexpensively produced using currently practiced industrial scale polymerization methods, o?ering a practical approach to recycling the world¡¯s top two plastics. -------------------------- SHARING/ACCESS INFORMATION -------------------------- Licenses/restrictions placed on the data: CC0 1.0 Universal Links to publications that cite or use the data: https://doi.org/10.1073/pnas.2301352120 Was data derived from another source? N/A If yes, list source(s): Terms of Use: Data Repository for the U of Minnesota (DRUM) By using these files, users agree to the Terms of Use. https://conservancy.umn.edu/pages/drum/policies/#terms-of-use Links to other publicly accessible locations of the data:N/A Links/relationships to ancillary data sets:N/A --------------------- DATA & FILE OVERVIEW --------------------- Purpose Statement: This document describes all data in figures associated with Shen et al. " Threading-the-Needle: Compatibilization of HDPE/iPP blends with butadiene-derived polyolefin block copolymers". File List 1. Filename: Fig. 2 AFM Short description: AFM images 2. Filename: Fig. 3 mechanical PE rich blends Short description: Data for 3(a) stress strain curves, 3(b) strain at break ¡¡¡¡¡¡¡¡ 3. Filename: Fig. 4 mechanical PP rich blends Short description: Data for 4(a) stress strain curves, 4(b) strain at break 4. Filename: Fig. 5 SEM Short description: SEM images 5. Filename: Fig. 6 stress strain varied cooling Short description: Data for 6(b) stress strain curves at varied cooling rate 6. Filename: Fig. S1-S2 SEC unsaturated Short description: SEC Data for unsaturated PB polymer 7. Filename: Fig. S3 NMR unsaturated Short description: NMR Data for unsaturated PB polymer 8. Filename: Fig. S4 high T SEC Short description: high T SEC Data for saturated BCP 9. Filename: Fig. S5 high T NMR Short description: high T NMR Data for saturated BCP 10. Filename: Fig. S6 BCP DSC Short description: DSC Data for saturated BCP 11. Filename: Fig. S7-S10 Rheology Short description: Rheology Data for saturated BCP 12. Filename: Fig. S11 size distribution PE rich Short description: size distribution of PE rich AFM images 13. Filename: Fig. S12 size distribution PP rich Short description: size distribution of PP rich AFM images 14. Filename: Fig. S13 PE_PP Blends DSC Short description: DSC Data for PE_PP Blends 15. Filename: Fig. S14 Mechanical parameter Short description: Mechanical Data (yield stress, Young¡¯s modulus) for PE_PP Blends 16. Filename: Fig. S15 stress strain curves PE rich Short description: stress strain curves for individual PE rich Blend samples 17. Filename: Fig. S16 stress strain curves PE rich Short description: stress strain curves for individual PP rich Blend samples 18. Filename: Fig. S17 DSC PE_E blends cocrytallization Short description: DSC Data for PE_E Blends 19. Filename: Fig. S18 DSC PE_E blends cocrytallization varied cooling Short description: DSC Data for PE_E Blends at varied cooling rate 20. Filename: Fig. S19 stress strain PE_PP varied cooling Short description: stress strain curves for PE PP at varied cooling rate 21. Filename: Fig. S20 DSC PE_PP crystallization varied cooling Short description: DSC Data for PE_PP Blends at varied cooling rate 22. Filename: Fig. S21 stress strain blends varied cooling Short description: stress strain curves for compatibilized at varied cooling rate Additional related data collected that was not included in the current data package: None. Are there multiple versions of the dataset? N -------------------------- METHODOLOGICAL INFORMATION -------------------------- Description of methods used for collection/generation of data: Details of polymer synthesis were provided in paper " Threading-the-Needle: Compatibilization of HDPE/iPP Blends with Butadiene-derived Polyolefin Block Copolymers ". Molecular characterization The molecular weight and dispersity of the PB compounds were determined using room temperature size exclusion chromatography (SEC) at a concentration of 3-5 mg/mL with THF as the mobile phase and calibrated with polystyrene standards. The eluent flow rate is 1 mL/min, and the sample injection volume is 100 ¦ÌL. The Mark-Houwink parameters used for the universal calibration are KPB= 2.52 ¡Á 10?2 mL/g, ¦ÁPB = 0.727, KPS = 8.63 ¡Á 10?3 mL/g, and ¦ÁPS = 0.736.(55) The composition of the 1,4-PB and 1,2-PB blocks were determined by 1H NMR spectra obtained from 10% (w/w) CDCl3 solutions at 30 ¡ãC using a Bruker HD500 NMR spectrometer. The polybutadiene precursors and the hydrogenated products were examined by high-temperature SEC in trichlorobenzene at 135 ¡ãC using an Agilent PL-220 instrument equipped with a refractive index detector to confirm a lack of chain degradation, and 1H NMR spectroscopy was performed with a Bruker HD500 instrument at 90 ¡ãC using deuterated toluene solutions to establish the extent of polymer saturation. Blend Preparation and Tensile Test. Blends of PE, iPP, and 0.5-5 wt% block copolymers (weight fraction based on the weight of neat PE/iPP blends) were prepared using a recirculating 5 mL DSM Xplore twin-screw microcompounder, with mixing for 8 min at 130 rpm at 190 ¡ãC. The blended materials were molded into 0.5 mm thick films at 180 ¡ãC employing a pressure of 4 MPa for 5 min with a Carver hot press. Unless otherwise stated, cooling water was used for quenching (~20 ¡ãC/min). Dumbbell-shaped tensile bars were prepared with a die cutter (ASTM D1708, 5 mm gauge width, 22 mm gauge length). All tensile tests were conducted at room temperature (22 ¡ãC) using an Instron 5966 Universal Testing System operated at a crosshead speed of 22 mm/min (100%/min strain rate). Atomic Force Microscopy. The morphology of neat and compatibilized PE:iPP blends were imaged using atomic force microscopy in dynamic mode (AFM; Bruker Nanoscope V Multimode 8, Digital Instruments Santa Barbara, CA open-loop system). Smooth imaging surfaces were obtained on pressed and annealed films using a cryo-ultramicrotome (Leica UC6) operated at -120 ¡ãC, first using a glass knife to create a cutting face, followed by sectioning of 500 nm thick slices with a diamond knife (Diatome), which were mounted on a silicon wafer. Samples were scanned in the repulsive regime using an n-type silicon tip cantilever (resonant frequency = 166 Hz, spring constant = 2 N/m, and radius = 8 nm). Captured images were processed using Gwyddion 2.56 open-source software to level the data, align rows, correct scarring, and adjust the contrast via histogram. Fractography. Dogbone tensile specimens were cryo-fractured in liquid nitrogen, and the resulting cross sections were examined using a JEOL 6500 field emission SEM with 2 kV accelerating voltage and approximately 10 mm working distance. Specimens were affixed with carbon tape to a 90-degree pin stub mount and sputter coated with a 5 nm thick platinum conducting layer before imaging. Thermal Analysis. Glass transition, melting and crystallization temperatures were determined using differential scanning calorimetry (DSC). 5?10 mg of sample was sealed in an aluminum pan and loaded in a TA Q1000 DSC instrument under a nitrogen atmosphere at gas flow rate 50 mL/min. Rheology. Bulk rheological data were acquired for the three saturated block copolymers (E91X93, E28X34E28, and E65X88E65) using an ARES-G2 rheometer (Thermal Analysis Instruments, New Castle, DE) under nitrogen gas purge employing an 8 mm parallel plate geometry and a 0.5 mm gap. Frequency sweeps spanning 0.1 - 100 rad/s at a constant strain amplitude of 2% were conducted from 120 to 240 ¡ãC in 20 ¡ãC increments with 10 minutes between measurements for temperature equilibration. Master curves, referenced to 180 ¡ãC, were prepared using time-temperature superposition. People involved with sample collection, processing, analysis and/or submission: L.S., G.D.G., E.D., and S.C. collect and processing data; L.S., G.D.G., E.D., C.J.E., and F.S.B. analyzed data. ---------------------------- Directory Structure ---------------------------- +---Fig. 2 AFM | PErich_E28X34E28.PNG | PErich_E65X88E65.PNG | PErich_E91X93.PNG | PErich_noBCP.PNG | PPrich_E28X34E28.PNG | PPrich_E65X88E65.png | PPrich_E91X93.PNG | PPrich_noBCP.PNG | +---Fig. 3 mechanical PE rich blends | 3 (a) PE rich stress strain.xlsx | 3 (b) PE rich strain at break.xlsx | +---Fig. 4 mechanical PP rich blends | 4 (a) PP rich stress strain.xlsx | 4 (b) PP rich strain at break.xlsx | +---Fig. 5 SEM | PEiPP_7030_neat.png | PE_iPP_7030_EXE.png | +---Fig. 6 stress strain varied cooling | 6(b) stress strain varied cooling.xlsx | +---Fig. S1-S2 SEC unsaturated | S1 (a).xlsx | S1 (b).xlsx | S1 (c).xlsx | S2 (a).xlsx | S2 (b).xlsx | +---Fig. S11 size distribution PE rich | DropMeasure_PE_Rich_1wt_E28X34E28.csv | DropMeasure_PE_Rich_1wt_E65X88E65.csv | DropMeasure_PE_Rich_1wt_E91X93.csv | DropMeasure_PE_Rich_NoCompat.csv | +---Fig. S12 size distribution PP rich | DropMeasure_PP_Rich_1wt_E28X34E28.csv | DropMeasure_PP_Rich_1wt_E65X88E65.csv | DropMeasure_PP_Rich_1wt_E91X93.csv | DropMeasure_PP_Rich_NoCompat.csv | +---Fig. S13 Blends DSC | S13 (a) PE rich.xlsx | S13 (b) PP rich.xlsx | +---Fig. S14 Mechanical parameter | S14 (a) PE rich yield stress.xlsx | S14 (b) PE rich modulus.xlsx | S14 (c) PP rich yield stress.xlsx | S14 (d) PP rich modulus.xlsx | +---Fig. S15 stress strain curves PE rich | S15 (a) no BCP.xlsx | S15 (b) 1%E91X93 .xlsx | S15 (c) 3%E91X93.xlsx | S15 (d) 5%E91X93.xlsx | S15 (e) 0.5%E65X88E65.xlsx | S15 (f) 1%E65X88E65.xlsx | S15 (g) 3%E65X88E65.xlsx | S15 (h) 5%E65X88E65.xlsx | S15 (i) 1%E28X34E28.xlsx | S15 (j) 3%E28X34E28.xlsx | S15 (k) 5%E28X34E28.xlsx | +---Fig. S16 stress strain curves PP rich | S16 (a) no BCP.xlsx | S16 (b) 0.5%E91X93.xlsx | S16 (c) 1%E91X93.xlsx | S16 (d) 3%E91X93.xlsx | S16 (e) 5%E91X93.xlsx | S16 (f) 0.5%E65X88E65.xlsx | S16 (g) 1%E65X88E65.xlsx | S16 (h) 3%E65X88E65.xlsx | S16 (i) 5%E65X88E65.xlsx | S16 (j) 1%E28X34E28.xlsx | S16 (k) 3%E28X34E28.xlsx | S16 (l) 5%E28X34E28.xlsx | +---Fig. S17 DSC PE_E blends cocrytallization | S17 (a) PE_E35.xlsx | S17 (b) PE_E65.xlsx | +---Fig. S18 DSC PE_E blends cocrytallization varied cooling | S18 (a) PE_E35.xlsx | S18 (b) PE_E65.xlsx | +---Fig. S19 stress strain PE_PP varied cooling | S19 stress strain PE_PP varied cooling.xlsx | +---Fig. S20 DSC PE_PP crystallization varied cooling | S20 (a) cooling scan cooled at 1C_min.xlsx | S20 (b) heating scan cooled at 1C_min.xlsx | S20 (c) cooling scan cooled at 20C_min.xlsx | S20 (d) heating scan cooled at 20C_min.xlsx | +---Fig. S21 stress strain blends varied cooling | S21 (a) slow.xlsx | S21 (b) slow - fast.xlsx | S21 (c) fast - slow.xlsx | +---Fig. S3 NMR unsaturated | E28X34E28 1,4PB first block.csv | E28X34E28 diblock.csv | E65X88E65 1,4PB first block.csv | E65X88E65 diblock.csv | E91X93 1,4PB first block.csv | E91X93 diblock.csv | +---Fig. S4 high T SEC | E28X34E28.xlsx | E65X88E65.xlsx | E91X93.xlsx | +---Fig. S5 high T NMR | E65X88E65 90C Toluene-D8.csv | PB Toluene-D8.csv | +---Fig. S6 BCP DSC | BCP DSC.xlsx | \---Fig. S7-S10 Rheology E28X34E28_SAOS.xlsx E28X34E28_TempRamp.xlsx E65X88E65_SAOS.xls E65X88E65_TempRamp.xls E91X93_SAOS.xlsx E91X93_TempRamp.xls