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Synthesis of phenolic resin amines and solid-state NMR of phenolic resins in NASA rocket motors.

机译：NASA火箭发动机中酚醛树脂胺的合成和酚醛树脂的固态NMR。

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摘要

Phenol-formaldehyde (PF) resol resins, formed from formaldehyde and phenol, are used mainly in applications related to the wood industry, thermal insulation, and molding. Prior studies in our laboratories have studied methylolphenolic model compounds. Ammonia catalyzed production of resol phenol formaldehyde resins produces appreciable amounts of hydroxybenzylamine compounds. Attempts to produce low density carbon cloth phenolic for the NASA shuttle program provide additional incentive to study amine formation. Thus, some model hydroxybenzylamine compounds, including 2-, and 4-hydroxybenzylamines, 2,2'-, and 4,4'-dihydroxydibenzylamines, 2,2',2 ''-, 4,4',4'' -, 2,2',4''-, and 2,4',4''-trihydroxytribenzylamines and benzoxazine were prepared for NMR study.; The primary amines were prepared by two ways. One was from their corresponded hydroxybenzylalcohols, the other was from the reduction of cyanophenols by LiAlH4. The dihydroxydibenzylamines were synthesized from the hydrogenation of cyanophenols using 5% Rh/C. A general synthetic method was developed for the synthesis of trihydroxytribenzylamines. The reaction of the secondary amines with acid chlorides, followed by the LiAlH4 reduction formed the tertiary amines. Benzoxazine was obtained directly from the reaction of phenol with hexamethylenetetramine. 1H and 13C liquid NMR spectra were obtained on the hydroxybenzylamine model compounds in acetone-d6 with 0.03% TMS as internal standard. The C-13 chemical shifts of the methylene carbons of these compounds, including some benzylamines, were characterized. These compounds can be used for qualitative identification by comparison of their spectra with those of the phenolic resins, but also can be good internal standards for further quantitative analysis.; Solid-state CP/MAS 13C NMR was carried out to analyze the phenolic resins in NASA rocket motors, since the final cured resol resin is insoluble and hard. A total number of sixteen samples were analyzed. The NMR data for these samples were obtained, and the precision of the measurements were calculated. A chemical structural model of a cured phenolic resin using a formaldehyde/phenol ratio (F/P) of 1.30 has been developed. This study shows that the solid-state NMR is a powerful tool for phenolic resin analysis.; In this dissertation, the synthesis of the hydroxybenzylamines was discussed. Also, the solid-state NMR methodology for the solid phenolic resins was discussed.
机译：由甲醛和苯酚形成的酚醛（PF）甲阶酚醛树脂主要用于与木材工业，隔热和成型相关的应用中。我们实验室的先前研究已经研究了羟甲基酚模型化合物。氨催化的甲阶酚醛树脂的生产会产生大量的羟基苄胺化合物。尝试为NASA航天飞机计划生产低密度的酚醛碳布提供了进一步的动机来研究胺的形成。因此，一些模型羟基苄胺化合物，包括2-和4-羟基苄胺，2,2'-和4,4'-二羟基二苄胺，2,2'，2''-，4,4'，4''-，制备了2,2'，4''-和2,4'，4''-三羟基三苄胺和苯并恶嗪用于NMR研究。伯胺是通过两种方法制备的。一种来自其相应的羟基苄醇，另一种来自LiAlH4还原氰基酚。使用5％Rh / C由氰基苯酚加氢合成二羟基二苄基胺。开发了用于合成三羟基三苄基胺的通用合成方法。仲胺与酰氯的反应，然后用LiAlH4还原，形成叔胺。苯并恶嗪直接由苯酚与六亚甲基四胺反应制得。以0.03％TMS为内标，在丙酮-d6中的羟基苄胺模型化合物上获得1H和13C液体NMR光谱。表征了这些化合物（包括一些苄胺）的亚甲基碳的C-13化学位移。这些化合物可通过将其光谱与酚醛树脂的光谱进行比较而用于定性鉴定，但也可以作为进一步定量分析的良好内标。由于最终固化的可熔酚醛树脂不溶且坚硬，因此进行了固态CP / MAS 13C NMR分析NASA火箭发动机中的酚醛树脂。分析了总共十六个样品。获得了这些样品的NMR数据，并计算了测量精度。已经开发出使用1.30的甲醛/苯酚比（F / P）的酚醛树脂固化物的化学结构模型。这项研究表明，固态NMR是用于酚醛树脂分析的强大工具。本文讨论了羟基苄胺的合成。此外，还讨论了用于固体酚醛树脂的固态NMR方法。

著录项

  • 作者

    Lu, Jinqi.;

  • 作者单位

    Mississippi State University.;

  • 授予单位 Mississippi State University.;
  • 学科 Chemistry Organic.
  • 学位 Ph.D.
  • 年度 1998
  • 页码 107 p.
  • 总页数 107
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 有机化学;
  • 关键词

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