Characterization for Industrial Use of Sustainable Materials - Challenge of Urushi to Realize Carbon Neutrality –

Purpose of this webinar

In this webinar, Dr. Miyakoshi will first talk about the industrial use of Urushi (natural lacquer), followed by an introduction to natural lacquer characterization methods by our employees. The characterization methods include monomer component analysis, hardening process analysis, thermal degradation analysis, and analysis of trace components in the natural lacquer film.

Properties of uruhi, hybridization and nano-modification of urushi sap

Urushi is a tree. It is planted in soil and grown. And the sap obtained from the tree is used as paint, adhesive material, and plastic material. Maki-e (Japanese lacquer decoration technique) and Raden(mother-of-pearl inlay) using urushi sap are elegant and beautiful, and become representatives of Japan’s fine arts and crafts. The use of plant resource, Urushi has been re-evaluated, in relation to green chemistry and SDGs. This presentation will give an outline about the properties of Urushi, industrial coating by using hybrid technology and nano-sized urushi, as well as a new application into industrial design.

Analysis of monomer component
- Application of FT-IR, MS -

This time, we isolated the monomer component from the natural lacquer and identified it. Here, an identification of 3-pentadecylcatechol, which is a saturated component, is introduced as an example. First, we analyzed the functional group by using FT-IR, and then analyzed the structure by using mass spectrometry (MS). While explaining the MS analysis, introduction of ionization methods and analysis methods of mass spectrum will be also covered.

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Analysis of monomer components
- Application of NMR -

The NMR analysis of 3-pentadecylcatechol (a saturated component of urushiol), one of the monomer components of natural lacquer, is presented here: based on the identification of functional groups by FT-IR and molecular weight information by MS, the chemical shifts, signal integration and J-couplings, which are information obtained by NMR measurements, were analyzed to estimate the carbon skeleton structure. The NMR structure analysis included ¹H-NMR for the number of protons, ¹³C-NMR for the number of carbons, and DEPT135 for the determination of the atomic group. In 2D NMR, HMQC and HSQC were used to determine the proton-carbon connection. Furthermore, ¹H connections were analyzed in COSY. Finally, HMBC was used to confirm the connection between the benzene ring and the root of the alkyl chain, which has no proton connection.

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Analysis of Natural Lacquer during Hardening
- Application of XPS -

The hardening process of urushi(film formation) was observed using pencil hardness testing and XPS.
The results of pencil hardness testing indicate that the hardness of urushi (natural lacquer) film was hardened to 7H, 50 days after film formation. In addition, the composition analysis and chemical bonding state analysis by XPS exemplify that oxidative polymerization of urushiol (monomer component of urushi) proceeded considerably.

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Thermal degradation analysis
- Application of SEM, TG/MS, PyGC/MS

The process of thermal degradation of natural lacquer film was analyzed by using SEM, TG/MS, PyGC/MS.
It was found that many micropores were produced on the surface of natural lacquer film by heating, by using the morphological observation by SEM. On the other hand, from the TG/MS analyses, it was found that the weight of the natural lacquer film gradually decreased between 200°C and 400°C, and there is a sharp decrease in the weight between 400°C and 500°C. In addition, PyGC/MS detected pyrolysis products of sugar protein and urushiol polymer.

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Thermal Degradation Analysis - Application of ESR -

The temperature dependence of radicals in the natural lacquer film when heated was evaluated using ESR, which is capable of observation of radicals in samples without pretreatment. We heated the sample gradually from 50°C to 300°C. The g-value of ESR spectrum suggested phenoxyl radical at room temperature, changed to suggest alkoxyl radical at 50°C、and at 200°C to suggest alkyl radical which is a sign of main chain scission. Furthermore, it was found that the radicals was increased from 200°C to 300°C, suggesting the start of pyrolysis at 200°C. These results indicate a good consistency with the aforementioned results by TG/MS and PyGC/MS.

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Analysis of Trace Component(polysaccharide) in Natural Lacquer Film

Trace polysaccharides in natural lacquer film were analyzed by TEM, Py/MS, and solid NMR. The morphological observation of natural lacquer section by TEM confirmed precipitates of polysaccharide in micropore. In addition, pyrolysis products of polysaccharide were detected by Py/MS analysis. Here, measurements were carried out using the hard ionization method EI and the soft ionization method FI, and the characteristics of each will also be explained. Furthermore, peaks characteristic of the polysaccharide component (COOH, C1 to C6) could be identified by a solid-state NMR analysis.

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