化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2015年
6期
1747-1749,1778
,共4页
成核剂%催化加氢%降冰片烯二酸酐%双环2.2.1-庚烷-2,3-二羧酸钠
成覈劑%催化加氫%降冰片烯二痠酐%雙環2.2.1-庚烷-2,3-二羧痠鈉
성핵제%최화가경%강빙편희이산항%쌍배2.2.1-경완-2,3-이최산납
nucleating agent%catalytic hydrogenation%norbornene dicarboxylic andydride%disodium bicyclo[2.2.1]-heptane-2,3-dicarboxylate
以降冰片烯二酸酐为起始原料，经水解中和和催化加氢制备了双环[2.2.1]-庚烷-2,3-二羧酸钠。通过研究催化加氢步骤中催化剂种类、催化剂用量、反应温度和反应压力等关键因素对双环[2.2.1]-庚烷-2,3-二羧酸钠的收率和纯度的影响，获得了适宜的反应条件。实验结果表明：催化剂雷尼镍可代替文献报道的价格昂贵的钯/炭催化剂完成催化加氢反应，在反应温度为60℃、反应压力为5MPa 的条件下进行催化加氢，双环[2.2.1]-庚烷-2,3-二羧酸钠的收率大于95%；红外光谱及核磁共振分析表明，所得加氢产物与双环[2.2.1]-庚烷-2,3-二羧酸钠结构特征吻合。
以降冰片烯二痠酐為起始原料，經水解中和和催化加氫製備瞭雙環[2.2.1]-庚烷-2,3-二羧痠鈉。通過研究催化加氫步驟中催化劑種類、催化劑用量、反應溫度和反應壓力等關鍵因素對雙環[2.2.1]-庚烷-2,3-二羧痠鈉的收率和純度的影響，穫得瞭適宜的反應條件。實驗結果錶明：催化劑雷尼鎳可代替文獻報道的價格昂貴的鈀/炭催化劑完成催化加氫反應，在反應溫度為60℃、反應壓力為5MPa 的條件下進行催化加氫，雙環[2.2.1]-庚烷-2,3-二羧痠鈉的收率大于95%；紅外光譜及覈磁共振分析錶明，所得加氫產物與雙環[2.2.1]-庚烷-2,3-二羧痠鈉結構特徵吻閤。
이강빙편희이산항위기시원료，경수해중화화최화가경제비료쌍배[2.2.1]-경완-2,3-이최산납。통과연구최화가경보취중최화제충류、최화제용량、반응온도화반응압력등관건인소대쌍배[2.2.1]-경완-2,3-이최산납적수솔화순도적영향，획득료괄의적반응조건。실험결과표명：최화제뢰니얼가대체문헌보도적개격앙귀적파/탄최화제완성최화가경반응，재반응온도위60℃、반응압력위5MPa 적조건하진행최화가경，쌍배[2.2.1]-경완-2,3-이최산납적수솔대우95%；홍외광보급핵자공진분석표명，소득가경산물여쌍배[2.2.1]-경완-2,3-이최산납결구특정문합。
Disodium bicyclo[2.2.1]-heptane-2,3-dicarboxylate is synthesized from norbornene dicarboxylic andydride by neutralization hydrolysis and catalytic hydrogenation. By studying the effects of catalyst type,the amount of catalyst,reaction temperature and hydrogen pressure on the yield and purity of disodium bicyclo[2.2.1]-heptane-2,3-dicarboxylate,the suitable reaction conditions are obtained. The results show that the expensive catalyst of Pd/C can be replaced by inexpensive Renay Ni . The suitable reaction temperature is 60℃ and the suitable reaction pressure is 5MPa. The results of infrared spectrum analysis and nuclear magnetic resonance analysis are identical with the structural features of disodium bicyclo[2.2.1]-heptane-2,3-dicarboxylate.
