ЯМР томография процессов массопереноса и химических превращений в гетерогенных системах тема автореферата и диссертации по химии, 02.00.15 ВАК РФ

1. Введение

1.1. Общие замечания.

1.2. Получение изображения.

1.3. Пространственное разрешение метода.

1.4. Специфика, достоинства и недостатки метода.

1.5. Механизмы контраста изображения и информативность метода.

1.6. Содержание обзора.

2. Структура и свойства материалов, содержащих жидкости

2.1. Общие замечания.

2.2. Модельные и синтетические пористые материалы.

2.3. Горные породы.

2.4. Полимеры, гели.

2.5. Суспензии, эмульсии, компакты.

2.6. Пищевые продукты и растения.

2.7. Другие материалы.

3. ЯМР порометрия

3.1. Общие замечания.

3.2. Релаксационная порометрия.

3.3. Криопорометрия.

4. Процессы сорбции в пористых материалах

4.1. Общие замечания.

4.2. Исследование процессов сорбции.

5. Набухание полимеров и угля при сорбции растворителей

5.1. Общие замечания.

5.2. Процессы набухания.

6. Сушка

6.1. Общие замечания.

6.2. Сушка материалов и пленок.

7. Диффузия

7.1. Общие замечания.

7.2. Методы изучения диффузии.

7.3. Применение градиента концентрации меток и меченых соединений.

7.4. Исследования диффузии без использования меченых соединений.

7.5. Эффект выделения краев.

8. Применение МРТ для изучения потоков

8.1. Общие замечания.

8.2. Методы исследования потоков.

8.3. Течение жидкостей в различных геометриях.

8.4. Фильтрация.

8.5. Движение твердых гранулированных материалов.

8.6. Течение газов.

9. Химические реакции

9.1. Общие замечания.

9.2. Термическая полимеризация.

9.3. Полимеризация под действием света или ионизирующего излучения.

9.4. Реакция Белоусова-Жаботинского.

9.5. Другие реакции.

10. ЯМР термометрия

11. Отображение плотности электрического тока

12. ЯМР томография газов

12.1. Общие замечания.

12.2. Газы с равновесной поляризацией.

12.3. Гиперполяризованные газы.

13. ЯМР томография твердых материалов

16. Процессы течения и фильтрации179

16.1. Общие замечания.179

16.2. Течение жидкостей и газов в каналах.180

16.3. Фильтрация жидкостей и газов.194

16.4. Фильтрация твердых гранулированных материалов.212

17. Процессы транспорта при сушке капиллярно-пористых тел220

17.1. Общие замечания.220

17.2. Удаление воды из капилляров.221

17.3. Экспериментальные исследования сушки единичного зерна.225

17.4. Моделирование процессов сушки единичного зерна.227

17.5. Внешний массообмен при сушке блочных структур.231

17.6. Адсорбционно-контактная сушка блочных структур.236

17.7. Экспериментальные исследования сушки зернистого слоя.237

17.8. Сушка древесины.238

18. Процессы транспорта при адсорбции влаги пористыми материалами240

18.1. Общие замечания.240

18.2. Экспериментальные исследования адсорбции влаги единичной гранулой.244

18.3. Моделирование процессов адсорбции единичной гранулой.248

18.4. Экспериментальные исследования адсорбции влаги зернистым слоем.250

18.5. Моделирование адсорбции зернистым слоем.253

18.6. Экспериментальные исследования адсорбции консолидированным слоем в отсутствие воздуха.258

18.7. Капиллярное впитывание воды блоками.264

18.8 Перераспределение активного компонента при приготовлении нанесенных катализаторов.266

19. Взаимодействие процессов транспорта и химического превращения270

19.1. Общие замечания.270

19.2. Реакция Белоусова-Жаботинского.272

19.3. Каталитическое гидрирование.276

19.4. Каталитическое разложение перекиси водорода.284

20. Заключение287

21. Экспериментальная часть288

22. Список работ, опубликованных по теме диссертации301

23. Литература307

24. Благодарности362

25. Приложение I364

Часть I. Метод ЯМР томографии и его физико-химические приложения

1. Введение

1.1. Общие замечания

Метод ЯМР томографии (МРТ) уже давно и рутинно используется в медицине и биологии, при этом применение метода вышло далеко за рамки диагностики многочисленных заболеваний и в настоящее время охватывает, в частности, такие области как оперативный контроль за неинвазивным и инвазивным лечением рада заболеваний и изучение функциональной активности головного мозга. В последние годы метод МРТ начинает приобретать популярность и при исследовании самых разнообразных неживых объектов. Существующий арсенал методик современного многоядерного магнитного резонанса позволяет получать изображения внутренней структуры различных объектов и исследовать широчайший спектр свойств материалов и процессов с пространственным разрешением в сотни и даже десятки микрон.

Метод МРТ [1-4] своим возникновением безусловно обязан созданию и развитию радиоспектроскопии как экспериментальной дисциплины, и прежде всего - первым успешным экспериментам Завойского по ЭПР [5] в 1944 году и работам групп Блоха [6] и Перселла [7] по наблюдению сигнала ЯМР в конденсированной среде в 1945 г. Большое значение для МРТ имели выполненные в 50-х годах работы Хана [8] по исследованию спинового эха, на регистрации которого основаны многие МРТ эксперименты. В 1966 году Эрнст и Андерсон показали [9] перспективность применения преобразования Фурье для извлечения спектральной информации, сделав важный шаг на пути к современному импульсному ЯМР [10-12], который составляет основу ЯМР томографии. Осознание необходимости использования компьютера для получения, обработки и представления данных привело к тому, что уже в начале 70-х годов серийные спектрометры ЯМР стали комплектоваться компьютерами. На сегодняшний день сложность экспериментов и объемы получаемой информации возросли настолько, что без компьютера обойтись невозможно. В 1971 году Джинер ввел в ЯМР идею двумерного преобразования Фурье, заложив основы многомерной ЯМР спектроскопии [13-16]. Фактически МРТ изображение также является многомерным "спектром" ЯМР, и во многих случаях конечное изображение в настоящее время восстанавливается именно с помощью многомерного преобразования Фурье [17]. Более того, ЯМР спектроскопия и МРТ могут рассматриваться как частные случаи многомерного ЯМР эксперимента в едином пространстве координат, частот и времени. В 1973 году Лаутербур опубликовал первое томографическое изображение [18], полученное по сигналу ЯМР !Н, а уже в начале 80-х начался серийный выпуск медицинских ЯМР томографов. Повышение пространственного разрешения на основе развития приборной базы и создания новых методик привело к возникновению ЯМР микротомографии в середине 80-х.

Отметим, что строгой границы между ЯМР томографией (МРТ) и микротомографией (МРМ) не существует. Как и в привычном понимании термина "микроскопия", формальной о границей может служить элемент объема (0.1 мм) , представляющий собой предел разрешения для невооруженного глаза [19]. Тем не менее, даже такое условное разграничение не всегда однозначно, поскольку во многих экспериментах пространственное разрешение анизотропно и часто составляет десятки микрон в плоскости изображения при толщине слоя в несколько миллиметров. Термин МРТ в основном употребляется применительно к медицинским приложениям, но в то же время многие немедицинские приложения также нельзя назвать "микроскопией". Поскольку фактически речь идет об одном и том же методе, в тексте настоящего обзора во многих случаях предпочтение отдано более общему термину МРТ, а термин МРМ использован там, где необходимо подчеркнуть высокое пространственное разрешение или немедицинский характер приложений.

20. Заключение

В работе впервые продемонстрирована и систематически исследована возможность применения метода ЯМР томографии для изучения широкого класса процессов транспорта вещества в модельных реакторах, зернистых слоях и отдельных пористых гранулах, в том числе в условиях протекания каталитической реакции in situ. При этом:

1. Впервые продемонстрировано, что метод ЯМР томографии применим для прямого получения наглядной количественной информации о течении газов в каналах и их фильтрации в пористой среде при нормальном давлении и без использования гиперполяризации ядерных спинов. Получены трехмерные пространственные распределения векторов скоростей течения жидкостей, газов и твердых частиц в модельных объектах сложной геометрии в комбинации с информацией о пространственной структуре, а также распределения по скоростям движения при их фильтрации в модельных зернистых слоях.

2. Исследованы процессы внутреннего транспорта и внешнего массообмена в ходе сушки капиллярно-пористых тел. Получены недоступные для традиционно применяемых методов данные о пространственном распределении влаги и величинах локальных влагосодержаний на разных стадиях процесса сушки. Измерены значения коэффициентов внешнего массообмена и зависимость эффективного коэффициента диффузии от влагосодержания. Продемонстрирована определяющая роль капиллярного транспорта влаги и установлена взаимосвязь величины эффективного коэффициента диффузии с распределением пор по размерам для исследуемого образца.

3. Впервые исследованы процессы транспорта адсорбированной влаги в ходе адсорбции водяного пара сорбентами типа «соль в пористой матрице», получены данные о пространственном распределении влаги в индивидуальных гранулах и зернистых слоях на разных стадиях процесса адсорбции. Показано, что для гранул размером несколько миллиметров и более лимитирующей стадией процесса может быть транспорт адсорбированной влаги в глубь пористого материала, а процесс распространения фронта адсорбции и время защитного действия абсорбера в значительной степени определяются характером транспорта адсорбированной влаги в индивидуальных гранулах сорбента. Получена зависимость коэффициента эффективной диффузии адсорбата от его содержания. На основе систематического исследования влияния химического состава, морфологии и способа приготовления адсорбентов на характер транспорта адсорбированной влаги при адсорбции в вакууме сформулированы практические рекомендации по оптимизации таких сорбентов.

4. Метод ЯМР томографии впервые применен для прямой визуализации пространственного распределения активного компонента в нанесенных катализаторах. Впервые выполнена визуализация перераспределения активных компонентов непосредственно в ходе приготовления нанесенного катализатора на основе платиновых металлов на подложке из оксидного материала, показана возможность контролируемого создания нанесенных катализаторов с заданным макрораспределением активного компонента.

5. Метод ЯМР томографии впервые применен для исследования in situ каталитических реакций в зернистом слое и в отдельной грануле катализатора, в том числе при повышенных температурах (до 170 °С). Впервые экспериментально зарегистрировано изменение пространственного распределения жидкой фазы внутри гранулы катализатора в модельном реакторе с орошаемым зернистым слоем непосредственно в условиях протекания гетерогенной каталитической реакции, сопровождающейся фазовым переходом жидкость-газ. Впервые прямым методом регистрации продемонстрировано влияние протекания каталитической реакции на процессы массопереноса, и в том числе на характер заполнения пористого катализатора жидкостью. Показано, что при протекании экзотермической многофазной реакции распределение жидкой фазы в пористом зерне катализатора определяется не только морфологией зерна, но и полем температур внутри зерна, что позволяет исследовать механизмы возникновения неустойчивых режимов протекания процесса.

21. Экспериментальная часть

Все эксперименты, представленные в настоящей работе, выполнены с регистрацией сигнала ЯМР 'Н на частоте 300 или 299 МГЦ с использованием ЯМР спектрометров MSL-300 и Avance DRX (Bruker), оборудованных сверхпроводящими магнитами с вертикальным рабочим зазором, а также блоками, необходимыми для экспериментов по микротомографии (катушки для создания трех взаимно ортогональных градиентов магнитного поля, градиентные усилители, система охлаждения градиентных катушек). В зависимости от геометрии эксперимента использовались рч катушки с диаметром рабочей области 10 или 25 мм.

В экспериментах по исследованию течения и фильтрации газов использовался бытовой пропан-бутан (сжиженный в 5 л баллонах), ацетилен (для сварочных аппаратов) и бутан для зажигалок (Eurofill, Aerosols B.V., Голландия, 200 мл баллоны, вес нетто 116 г), приобретенный в табачном магазине. Информация о составе или чистоте газов производителями не предоставлялась. 'Н ЯМР спектр пропана выявил наличие примесей (не

288 более нескольких процентов), сигналы ЯМР которых находились в более слабом поле по отношению к основным резонансам (СН2, СНз), в то время как для остальных газов ЯМР не выявил заметного количества примесей. С помощью ГХ-МС анализа бытового пропана-бутана было установлено, что смесь преимущественно содержит н-бутан и н-пропан, а также небольшие количества других газов. Однако состав смеси существенно различается для разных баллонов, и к тому же не оказывает принципиального влияния на результаты, полученные в настоящей работе.

Необходимая скорость течения газа через образец устанавливалась с помощью регулируемого ротаметра (в случае ацетилена и водорода он был установлен после штатного редуктора баллона), который калибровался отдельно для каждого газа как с помощью барабанного газосчетчика ГСБ-400, так и по вытеснению жидкости из сосуда с делениями. Газ в экспериментах подавался в чувствительную область датчика снизу вверх, а вытекание газа происходило через открытый выпускной конец шланга в вытяжной шкаф. Для бутана испарение сжиженного газа приводило к заметному охлаждению небольшого баллона, что вызывало заметное изменение скорости течения газа в ходе эксперимента. Поэтому баллоны с бутаном термостатировались путем погружения в воду, находившуюся в емкости термостата. Для остальных газов из-за значительно большего размера баллонов их заметного охлаждения не наблюдалось. В экспериментах по исследованию течения и фильтрации жидкости использовалась дистиллированная вода. Поток жидкости создавался с помощью насоса лабораторного жидкостного термостата (Lauda А100), а скорость определялась измерением объемного расхода жидкости. В работе не делалось попыток сократить времена спиновой релаксации воды путем допирования воды парамагнитными соединениями или ионами чтобы избежать загрязнения используемых катализаторов.

При исследовании течения жидкости или газа в трубке круглого сечения использовался отрезок пластиковой трубки длиной 5-6 м внутренним диаметром 7.6 мм, а все измерения выполнены на прямом участке трубки. При исследовании течений через блочные катализаторы использовался приблизительно цилиндрический фрагмент блока, который помещался в цилиндрическую фторопластовую ячейку с внутренним диаметром 21 мм. Нижний срез блока располагался на 2 см выше дна кюветы. К ячейке с обеих сторон подсоединялись отрезки полиэтиленовой трубки длиной 2-3 м с внутренним диаметром 4 мм (газ) или 5.5 мм (вода). Диаметр входного отверстия в нижней части ячейки составлял 4 или 5 мм. В экспериментах использованы фрагменты блочных катализаторов из у-АЬОз, имеющих прямые транспортные каналы различной геометрии. Основная часть экспериментов выполнена для блока с удельной поверхностью 62 м /г и средний диаметр пор 14 нм (XII, табл. 6). Его транспортные каналы имели квадратное сечение 4x4 мм и

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