CN115716917B - 一种制备含锆聚碳硅烷的新方法 - Google Patents
一种制备含锆聚碳硅烷的新方法 Download PDFInfo
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- CN115716917B CN115716917B CN202110987521.0A CN202110987521A CN115716917B CN 115716917 B CN115716917 B CN 115716917B CN 202110987521 A CN202110987521 A CN 202110987521A CN 115716917 B CN115716917 B CN 115716917B
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- zirconium
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 51
- 229920003257 polycarbosilane Polymers 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 12
- 229920000548 poly(silane) polymer Polymers 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000005336 cracking Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 12
- 229910010082 LiAlH Inorganic materials 0.000 claims description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910000077 silane Inorganic materials 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 229910007926 ZrCl Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 4
- 229910008045 Si-Si Inorganic materials 0.000 claims description 2
- 229910006411 Si—Si Inorganic materials 0.000 claims description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 2
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- AZFVLHQDIIJLJG-UHFFFAOYSA-N chloromethylsilane Chemical compound [SiH3]CCl AZFVLHQDIIJLJG-UHFFFAOYSA-N 0.000 claims description 2
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract 1
- 229910004298 SiO 2 Inorganic materials 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 abstract 1
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 12
- 239000000835 fiber Substances 0.000 description 12
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 12
- 229910010271 silicon carbide Inorganic materials 0.000 description 12
- 239000011734 sodium Substances 0.000 description 12
- 229910052708 sodium Inorganic materials 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- NWKBSEBOBPHMKL-UHFFFAOYSA-N dichloro(methyl)silane Chemical compound C[SiH](Cl)Cl NWKBSEBOBPHMKL-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 150000003384 small molecules Chemical class 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- YOBOXHGSEJBUPB-MTOQALJVSA-N (z)-4-hydroxypent-3-en-2-one;zirconium Chemical compound [Zr].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O YOBOXHGSEJBUPB-MTOQALJVSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
Description
碳化硅纤维先驱体组别 | 空气中1500℃处理4h的强度保留率(%) |
聚碳硅烷 | 粉化 |
实施例1 | 51 |
实施例2 | 50 |
实施例3 | 55 |
Claims (4)
Priority Applications (1)
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CN202110987521.0A CN115716917B (zh) | 2021-08-26 | 2021-08-26 | 一种制备含锆聚碳硅烷的新方法 |
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CN202110987521.0A CN115716917B (zh) | 2021-08-26 | 2021-08-26 | 一种制备含锆聚碳硅烷的新方法 |
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CN115716917A CN115716917A (zh) | 2023-02-28 |
CN115716917B true CN115716917B (zh) | 2023-09-26 |
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Citations (9)
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---|---|---|---|---|
US5270429A (en) * | 1992-04-02 | 1993-12-14 | E. I. Du Pont De Nemours And Company | Silicon carbide precursors and their preparation and use |
CN103275326A (zh) * | 2013-06-15 | 2013-09-04 | 厦门大学 | 一种制备液态无氧型聚锆碳硅烷的方法 |
CN103554504A (zh) * | 2013-11-21 | 2014-02-05 | 宿迁澳鑫斯新材料有限公司 | 一种环保、高效的聚碳硅烷制备新方法 |
CN103772709A (zh) * | 2014-01-03 | 2014-05-07 | 航天材料及工艺研究所 | 一种Si/C/Zr陶瓷前驱体及其制备方法 |
CN105237773A (zh) * | 2015-10-23 | 2016-01-13 | 中国人民解放军国防科学技术大学 | 一种耐超高温ZrC/SiC复相陶瓷先驱体的合成方法 |
CN106674528A (zh) * | 2016-11-15 | 2017-05-17 | 杭州师范大学 | 一种聚碳硅烷的制备方法 |
CN109054026A (zh) * | 2018-10-10 | 2018-12-21 | 中国人民解放军国防科技大学 | 一种HfC-SiC超高温陶瓷先驱体的制备方法 |
RU2679145C1 (ru) * | 2017-10-10 | 2019-02-06 | Акционерное общество "Государственный Ордена Трудового Красного Знамени научно-исследовательский институт химии и технологии элементоорганических соединений" (АО "ГНИИХТЭОС") | Способ получения металлополикарбосиланов |
CN112940029A (zh) * | 2019-12-11 | 2021-06-11 | 新特能源股份有限公司 | 一种甲基氯硅烷、制备方法及装置 |
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2021
- 2021-08-26 CN CN202110987521.0A patent/CN115716917B/zh active Active
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5270429A (en) * | 1992-04-02 | 1993-12-14 | E. I. Du Pont De Nemours And Company | Silicon carbide precursors and their preparation and use |
CN103275326A (zh) * | 2013-06-15 | 2013-09-04 | 厦门大学 | 一种制备液态无氧型聚锆碳硅烷的方法 |
CN103554504A (zh) * | 2013-11-21 | 2014-02-05 | 宿迁澳鑫斯新材料有限公司 | 一种环保、高效的聚碳硅烷制备新方法 |
CN103772709A (zh) * | 2014-01-03 | 2014-05-07 | 航天材料及工艺研究所 | 一种Si/C/Zr陶瓷前驱体及其制备方法 |
CN105237773A (zh) * | 2015-10-23 | 2016-01-13 | 中国人民解放军国防科学技术大学 | 一种耐超高温ZrC/SiC复相陶瓷先驱体的合成方法 |
CN106674528A (zh) * | 2016-11-15 | 2017-05-17 | 杭州师范大学 | 一种聚碳硅烷的制备方法 |
RU2679145C1 (ru) * | 2017-10-10 | 2019-02-06 | Акционерное общество "Государственный Ордена Трудового Красного Знамени научно-исследовательский институт химии и технологии элементоорганических соединений" (АО "ГНИИХТЭОС") | Способ получения металлополикарбосиланов |
CN109054026A (zh) * | 2018-10-10 | 2018-12-21 | 中国人民解放军国防科技大学 | 一种HfC-SiC超高温陶瓷先驱体的制备方法 |
CN112940029A (zh) * | 2019-12-11 | 2021-06-11 | 新特能源股份有限公司 | 一种甲基氯硅烷、制备方法及装置 |
Non-Patent Citations (1)
Title |
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氯化反应合成聚甲基氯硅烷的研究;邢欣 等;《功能高分子学报》;第17卷(第2期);第181-184页 * |
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Effective date of registration: 20240724 Address after: Room 401, Building 13, Hengfeng Jiayuan, No. 208, Hengshan Road, Qinchuan Street, Changshu, Suzhou, Jiangsu 215500 Patentee after: Suzhou Xingyun New Materials Partnership Enterprise (Limited Partnership) Country or region after: China Address before: 215163 No.158, Keling Road, science and Technology City, high tech Zone, Suzhou City, Jiangsu Province Patentee before: SUZHOU CERAFIL CERAMIC FIBER CO.,LTD. Country or region before: China |
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