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Low-oxygen hafnium titanium carbon ceramic precursor and preparation method thereof
The invention provides a low-oxygen hafnium-titanium-carbon ceramic precursor and a preparation method thereof, and belongs to the technical field of ceramic materials.The method comprises the steps that under nitrogen protection, hafnium dichloride and a reagent 1 are subjected to a reaction and suction filtration, and a hafnium intermediate 1 is obtained; under the protection of nitrogen, stirring hafnium dichloride, and reacting the reagent 2 with polyolefin to obtain a hafnium intermediate 2; reacting an organic solvent, the hafnium intermediate 1 and the hafnium intermediate 2 under anhydrous and anaerobic conditions to obtain alkane-based hafnium metallocene; the method comprises the following steps: reacting titanocene dichloride with a reagent 1 under the protection of nitrogen, and carrying out suction filtration to obtain a titanium intermediate 1; under the protection of nitrogen, reacting titanocene dichloride, a reagent 2 and polyolefin under the action of hydrogen to obtain a titanium intermediate 2; the method comprises the following steps: reacting an organic solvent, a titanium intermediate 1 and a titanium intermediate 2 under anhydrous and anaerobic conditions to obtain alkane-based titanocene; stirring and heating alkane hafnium metallocene, an organic solvent and alkane titanium metallocene, and carrying out reduced-pressure suction filtration; the hafnium titanium carbon ceramic precursor is low in oxygen content.
本发明给出了一种低氧铪钛碳陶瓷前驱体及其制备方法，属于陶瓷材料技术领域，该方法包括：在氮气保护下，将二氯二茂铪和试剂1反应，抽滤，得到铪中间体1；在氮气保护下，将二氯二茂铪搅拌、试剂2和聚烯烃反应，得到铪中间体2；在无水无氧条件下，将有机溶剂、铪中间体1和铪中间体2反应，得到烷烃基茂化铪；在氮气保护下，将二氯二茂钛和试剂1反应，抽滤，得到钛中间体1；在氮气保护下，将二氯二茂钛、试剂2和聚烯烃在氢气的作用下反应，得到钛中间体2；在无水无氧条件下，将有机溶剂、钛中间体1和钛中间体2反应，得到烷烃基茂化钛；将烷烃基茂化铪、有机溶剂和烷烃基茂化钛搅拌升温和减压抽滤。本发明的铪钛碳陶瓷前驱体含氧量低。
Low-oxygen hafnium titanium carbon ceramic precursor and preparation method thereof
The invention provides a low-oxygen hafnium-titanium-carbon ceramic precursor and a preparation method thereof, and belongs to the technical field of ceramic materials.The method comprises the steps that under nitrogen protection, hafnium dichloride and a reagent 1 are subjected to a reaction and suction filtration, and a hafnium intermediate 1 is obtained; under the protection of nitrogen, stirring hafnium dichloride, and reacting the reagent 2 with polyolefin to obtain a hafnium intermediate 2; reacting an organic solvent, the hafnium intermediate 1 and the hafnium intermediate 2 under anhydrous and anaerobic conditions to obtain alkane-based hafnium metallocene; the method comprises the following steps: reacting titanocene dichloride with a reagent 1 under the protection of nitrogen, and carrying out suction filtration to obtain a titanium intermediate 1; under the protection of nitrogen, reacting titanocene dichloride, a reagent 2 and polyolefin under the action of hydrogen to obtain a titanium intermediate 2; the method comprises the following steps: reacting an organic solvent, a titanium intermediate 1 and a titanium intermediate 2 under anhydrous and anaerobic conditions to obtain alkane-based titanocene; stirring and heating alkane hafnium metallocene, an organic solvent and alkane titanium metallocene, and carrying out reduced-pressure suction filtration; the hafnium titanium carbon ceramic precursor is low in oxygen content.
本发明给出了一种低氧铪钛碳陶瓷前驱体及其制备方法，属于陶瓷材料技术领域，该方法包括：在氮气保护下，将二氯二茂铪和试剂1反应，抽滤，得到铪中间体1；在氮气保护下，将二氯二茂铪搅拌、试剂2和聚烯烃反应，得到铪中间体2；在无水无氧条件下，将有机溶剂、铪中间体1和铪中间体2反应，得到烷烃基茂化铪；在氮气保护下，将二氯二茂钛和试剂1反应，抽滤，得到钛中间体1；在氮气保护下，将二氯二茂钛、试剂2和聚烯烃在氢气的作用下反应，得到钛中间体2；在无水无氧条件下，将有机溶剂、钛中间体1和钛中间体2反应，得到烷烃基茂化钛；将烷烃基茂化铪、有机溶剂和烷烃基茂化钛搅拌升温和减压抽滤。本发明的铪钛碳陶瓷前驱体含氧量低。
Low-oxygen hafnium titanium carbon ceramic precursor and preparation method thereof
一种低氧铪钛碳陶瓷前驱体及其制备方法
YE MINGXIN (Autor:in) / SHEN JIANFENG (Autor:in) / YE CHUMING (Autor:in) / LI NA (Autor:in) / REN ZHOUHONG (Autor:in) / LI SHUANGWEN (Autor:in)
15.11.2024
Patent
Elektronische Ressource
Chinesisch
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