山东化工
山東化工
산동화공
SHANDONG CHEMICAL INDUSTRY
2012年
6期
3-6
,共4页
庞胜兰%陈玉琴%牟海燕%朱小猛
龐勝蘭%陳玉琴%牟海燕%硃小猛
방성란%진옥금%모해연%주소맹
邻苯基苯酚%双OPP-A%2,2-双(3-苯基-4羟基苯基)丙烷%合成
鄰苯基苯酚%雙OPP-A%2,2-雙(3-苯基-4羥基苯基)丙烷%閤成
린분기분분%쌍OPP-A%2,2-쌍(3-분기-4간기분기)병완%합성
o - phenylphenol%bis OPP - A%2,2 - bis ( 3 - phenyl - 4 - hydroxyphenyl ) propane%synthesis
以主催化剂对甲苯磺酸及助催化剂巯基丙磺酸来催化丙酮和邻苯基苯酚,经过缩合反应合成了2,2-双(3-苯基-4-羟基苯基)丙烷(双OPP-A),实验过程中研究了原料配比、反应温度、催化剂用量、反应时间等因素对产物的影响,得到合成2,2-双(3-苯基-4-羟基苯基)丙烷的最优工艺条件为:丙酮、邻苯基苯酚、对甲苯磺酸和巯基丙磺酸物质的量比为1:4:O.25:O.25,最佳反应时间为7h、最佳反应温度为60℃,2,2-双(3-苯基-4-羟基苯基)丙烷收率达到74.2%,经重结晶纯度达99.5%。通过红外光谱、核磁共振和熔点等分析手段对产物结构进行了确证。
以主催化劑對甲苯磺痠及助催化劑巰基丙磺痠來催化丙酮和鄰苯基苯酚,經過縮閤反應閤成瞭2,2-雙(3-苯基-4-羥基苯基)丙烷(雙OPP-A),實驗過程中研究瞭原料配比、反應溫度、催化劑用量、反應時間等因素對產物的影響,得到閤成2,2-雙(3-苯基-4-羥基苯基)丙烷的最優工藝條件為:丙酮、鄰苯基苯酚、對甲苯磺痠和巰基丙磺痠物質的量比為1:4:O.25:O.25,最佳反應時間為7h、最佳反應溫度為60℃,2,2-雙(3-苯基-4-羥基苯基)丙烷收率達到74.2%,經重結晶純度達99.5%。通過紅外光譜、覈磁共振和鎔點等分析手段對產物結構進行瞭確證。
이주최화제대갑분광산급조최화제구기병광산래최화병동화린분기분분,경과축합반응합성료2,2-쌍(3-분기-4-간기분기)병완(쌍OPP-A),실험과정중연구료원료배비、반응온도、최화제용량、반응시간등인소대산물적영향,득도합성2,2-쌍(3-분기-4-간기분기)병완적최우공예조건위:병동、린분기분분、대갑분광산화구기병광산물질적량비위1:4:O.25:O.25,최가반응시간위7h、최가반응온도위60℃,2,2-쌍(3-분기-4-간기분기)병완수솔체도74.2%,경중결정순도체99.5%。통과홍외광보、핵자공진화용점등분석수단대산물결구진행료학증。
The 2,2 - bis ( 3 - phenyl - 4hydroxypheny) propane ( bis OPP - A) was synthesized from o - phenyl phenol (OPP) and acetone by using p -Toluenesulfonic acid as main catalyst and 3 - mercaptopropanesulfonic acid as promoter. The effects of the reaction temperature and reaction time, the dosages of p - toluene sulfuric acid and 3 - mercaptopropanesulfonic acid , the molar ratio of OPP to acetone on the yield of bis OPP - A were studied. The optimum conditions were found as follows: n (acetone) :n( o - phenyl phenol) : n( p - Toluenesulfonic cid) : n( 3 - mercaptopropanesulfonic acid) = 1:4:0.25:0.25, reaction time is 7h and reaction temperature is 60℃, and the yield of 2,2 -bis (3 - phenyl - 4hydroxypheny) propane is 74.2%, the purity of the product is 99.5%. The structure of obtained bisOPP- A was characterized by melting point, IR and 1H -NMR.