(中南大學(xué) 粉末冶金國家重點(diǎn)實(shí)驗(yàn)室,長沙 410083)
摘 要: 采用熱重法(TG)和差示掃描量熱法(DSC)研究了新型炭材料用糠酮樹脂的固化過程,分析固化劑含量及升溫速率對(duì)固化反應(yīng)的影響,確定磷酸/糠酮樹脂固化體系的固化工藝,計(jì)算固化反應(yīng)表觀活化能和反應(yīng)級(jí)數(shù),得到了糠酮樹脂固化反應(yīng)動(dòng)力學(xué)方程。并利用熱重-質(zhì)譜聯(lián)用技術(shù)(TG-MS)研究樹脂在固化過程中的氣態(tài)產(chǎn)物。結(jié)果表明:糠酮樹脂的固化反應(yīng)是一個(gè)復(fù)雜的反應(yīng)過程,升溫速率和固化劑含量對(duì)固化反應(yīng)都會(huì)產(chǎn)生重要的影響。對(duì)于本固化體系,固化劑含量以7%(質(zhì)量分?jǐn)?shù))為最佳,該固化體系固化反應(yīng)起始溫度和最佳固化溫度分別為102.32和159.07 ℃,反應(yīng)活化能為73.33 kJ/mol,反應(yīng)級(jí)數(shù)為0.9;糠酮樹脂的固化反應(yīng)氣態(tài)產(chǎn)物以H2O為主,另有少量的CO、CH4和CO2。
關(guān)鍵字: 新型炭材料;糠酮樹脂;固化反應(yīng)動(dòng)力學(xué);氣態(tài)產(chǎn)物
(State Key Laboratory of Powder Metallurgy, Central South University, Changsha 410083, China)
Abstract:The curing process of furfural acetone resin used for new carbon materials was studied by thermogravimetry-differential scanning calorimetry technology (TG-DSC) and thermogravimetry-mass spectrometric coupling technique (TG-MS). The effects of curing agent content and heating rate on curing reaction were analyzed; the curing mechanism of furfural acetone resin and gaseous products evolved during curing process were investigated. The results show that the curing agent content and heating rate both have great influence on curing reaction. In this experiment, the optimal curing agent content is 7% (mass fraction) of phosphorus acid, and for this system the initial curing temperature and the optimal curing temperature are 102.32 and 159.07 ℃, respectively; the apparent activation energy is 73.33 kJ/mol and the order of curing reaction is 0.9; the main gaseous products during the curing reaction are H2O and small amount of CO, CH4 and CO2.
Key words: new carbon materials; furfural acetone resin; curing kinetics; gaseous products


