成果報告書詳細
管理番号20110000000668
タイトル*平成22年度中間年報 グリーン・サステイナブルケミカルプロセス基盤技術開発 廃棄物、副生成物を削減できる革新的プロセス及び化学品の開発 革新的酸化プロセス基盤技術開発(H21~H23)
公開日2011/7/28
報告書年度2010 - 2010
委託先名独立行政法人産業技術総合研究所 昭和電工株式会社 電気化学工業株式会社 チッソ株式会社 荒川化学工業株式会社
プロジェクト番号P09010
部署名環境部
和文要約和文要約等以下本編抜粋:1.研究開発の内容及び成果等 (1)「多官能性基質の酸化技術開発」モデル化合物を用いて反応条件の最適化を行い、タングステン酸ナトリウム~4級アンモニウム塩~燐酸という単純な組み合わせでも、原料の精製を十分に行えば収率80%を超える系を確立できた。生成物の取り出しも再結晶~吸着剤処理の最適化により目標レベルにまで到達することが出来た。この条件でベンチ試験を二回行い、触媒の前処理条件の確立、 pH制御により、発熱制御が可能になり、過酸化水素の異常分解を抑えることが出来た。また中間体、生成物を含むろ液を精製して用いることにより、触媒活性低下を抑制でき、収率80%を達成した。なお、今回の試作で得られた生成物については従来品よりも高融点、低粘度であり低塩素以外にも特長のあることが確認できた。
英文要約1. Technology developments for multi-functional substrates oxidation: Optimizations of re-crystallization conditions and absorbent-treatment procedure for product isolation have succeeded. Under these conditions the target substrate was submitted to bench test twice, where pre-treatment of catalyst system and reaction pH-control have been found very effective for inhibiting non-expected decomposition of hydrogen peroxide and heat generation. The product obtained from these trials exhibits higher melting point and lower viscosity in addition to lower chlorine content than the one produced by the conventional method. Safety tests (toxicological assays) have been conducted for these compounds and for decomposed ones from these compounds.
2. Technology development for polymer substrates oxidation: 1)Cost reduction through re-optimization of total reaction system where perfect consumption of hydrogen peroxide can lead to the same result and 2) expansion of applicable substrates (several functionalized elastomers) have been achieved. The products obtained with these technologies exhibit excellent characters as the next generation polymer modifiers. They can be micro-dispersed into the parent polymer-matrices and the well-mixing was found able to improve the parent polymer’s mechanical characteristics.
3. Technology development for water-susceptible oxidation: Optimizations of oxidation reaction process using ・-pinene, one of the most water-susceptible candidates, has been engaged for scaling up the system in order to manufacture ・-pinene oxide. Scaling up was found affecting the catalysts’ phase transferring rate, which decrease the product yields. Finally, the reaction apparatus has been well-designed to be able to reproduce the results with smaller scale reactions. Bench plant has also been designed based on these findings.
4. Technology development for less reactive substrate oxidation: Both sets of reaction conditions for ketone-oxidation and epoxidation, which were optimized with using each model compound, have been applied to the real target substrates. As to ketone-oxidation reaction the targeted values of the reaction in this project has been accomplished totally, through the re-optimization of additive ratios, reaction temperature and time, etc. As for the catalytic olefins epoxidation, the reaction conditions using recoverable polyoxometalate catalyst have been optimized for the bench trials. Exothermisity trend of the reaction was investigated by using temperature-controllable process reactors to ensure safety in scaling up the reaction.
5. Basic research for innovative oxidation technologies with hydrogen peroxide: Tungsten-based ternary catalytic system has been successfully applied to more characteristic/functionalized substrates by fine-tuning of the reaction conditions. Developments of new catalytic systems have also been engaged. Palladium-catalyzed oxidation of alpha, beta-unsaturated aldehydes to the corresponding acids has been investigated for further improvement. Effective and halogen-free iron-catalyzed epoxidation of styrene derivatives has been successfully achieved by the iron-ligands selection. Reusable platinum black was found to be an effective catalyst for oxidation of tertiary allylic alcohols affording aipha, beta-unsaturated carbonyl compounds through rearrangement/oxidation reaction in one-pot.
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