中国油脂
中國油脂
중국유지
CHINA OILS AND FATS
2015年
4期
60-63
,共4页
孙悦%李雪%任铁强%乔庆东%贾卓慧
孫悅%李雪%任鐵彊%喬慶東%賈卓慧
손열%리설%임철강%교경동%가탁혜
磷钼钒杂多酸%酯化反应%油酸甲酯
燐鉬釩雜多痠%酯化反應%油痠甲酯
린목범잡다산%지화반응%유산갑지
molybdovanadophosphoric heteropoly acid%esterification reaction%methyl oleate
采用二水钼酸钠、十二水磷酸氢二钠和偏钒酸钠为原料,制备了磷钼钒杂多酸( H4PMo11VO40)催化剂。利用紫外可见吸收光谱、红外光谱和热重分析方法对H4PMo11VO40的化学结构和化学热稳定性进行了表征,并将H4 PMo11VO40作为催化剂用于油酸与甲醇的酯化反应中。结果表明:H4 PMo11VO40红外谱图含有明显P—O键、Mo—O键和Mo—O—Mo桥键特征吸收峰;该杂多酸在308 nm处有明显紫外吸收峰;该杂多酸热稳定性在209℃以上。在酸醇摩尔比1∶6、反应时间7 h、催化剂用量为油酸质量9%的条件下,油酸酯化率为90.7%;H4PMo11VO40催化剂循环使用5次后,油酸酯化率仍在85%以上。因此,该磷钼钒杂多酸可循环使用,且易与产物分离。
採用二水鉬痠鈉、十二水燐痠氫二鈉和偏釩痠鈉為原料,製備瞭燐鉬釩雜多痠( H4PMo11VO40)催化劑。利用紫外可見吸收光譜、紅外光譜和熱重分析方法對H4PMo11VO40的化學結構和化學熱穩定性進行瞭錶徵,併將H4 PMo11VO40作為催化劑用于油痠與甲醇的酯化反應中。結果錶明:H4 PMo11VO40紅外譜圖含有明顯P—O鍵、Mo—O鍵和Mo—O—Mo橋鍵特徵吸收峰;該雜多痠在308 nm處有明顯紫外吸收峰;該雜多痠熱穩定性在209℃以上。在痠醇摩爾比1∶6、反應時間7 h、催化劑用量為油痠質量9%的條件下,油痠酯化率為90.7%;H4PMo11VO40催化劑循環使用5次後,油痠酯化率仍在85%以上。因此,該燐鉬釩雜多痠可循環使用,且易與產物分離。
채용이수목산납、십이수린산경이납화편범산납위원료,제비료린목범잡다산( H4PMo11VO40)최화제。이용자외가견흡수광보、홍외광보화열중분석방법대H4PMo11VO40적화학결구화화학열은정성진행료표정,병장H4 PMo11VO40작위최화제용우유산여갑순적지화반응중。결과표명:H4 PMo11VO40홍외보도함유명현P—O건、Mo—O건화Mo—O—Mo교건특정흡수봉;해잡다산재308 nm처유명현자외흡수봉;해잡다산열은정성재209℃이상。재산순마이비1∶6、반응시간7 h、최화제용량위유산질량9%적조건하,유산지화솔위90.7%;H4PMo11VO40최화제순배사용5차후,유산지화솔잉재85%이상。인차,해린목범잡다산가순배사용,차역여산물분리。
Molybdovanadophosphoric heteropoly acid ( H4 PMo11VO40 ) catalyst was synthesized using Na2MoO4·2H2O, Na2HPO4·12H2O and NaVO3 as raw materials. The chemical structure and thermal stability of H4 PMo11VO40 were characterized by UV-Vis, FTIR and TG-DTG and it was used as catalyst in the esterification of oleic acid and methanol. The results showed that the characteristic absorption peaks of P—O bond, Mo—O bond and Mo—O—Mo bridge bond could be observed obviously in FTIR spectra of H4 PMo11VO40;H4 PMo11VO40 had a clear ultraviolet absorption peak at 308 nm;it was provided with high thermal stability above 209℃. When the molar ratio of oleic acid to methanol was 1∶6 , the dosage of catalyst was 9% ( based on the mass of oleic acid) and the reaction time was 7 h, the esterifi-cation rate of oleic acid reached 90. 7%. After the catalyst was reused for five times, the esterification rate of oleic acid was still above 85%. Therefore, heteropoly acid H4 PMo11VO40 could be repeatedly used and easily separated from the product.