在固體酸催化劑上2-（1，1-二甲基乙基）-1，4-苯二酚的合成及HPLC分析的研究.pdf

1、甫開(kāi)‘大學(xué)不沉士學(xué)七立論文摘要叔丁基對(duì)苯二酚是一種較新的酚類油溶性抗氧劑，廣泛應(yīng)用于油料、脂肪、食用品和化妝品等的添加劑。由于其高效、安全及其它的優(yōu)良性能，現(xiàn)已有包括我國(guó)在內(nèi)的20多個(gè)國(guó)家批準(zhǔn)其作為食品和飼料添加劑使用。本文采用樹(shù)脂催化劑合成叔丁基對(duì)苯二酚，找到了一種催化活性較好的樹(shù)脂催化劑，并進(jìn)對(duì)反應(yīng)工藝條件進(jìn)行了優(yōu)化，取得了較好的結(jié)果。本文主要工作如下:1本文對(duì)六種樹(shù)脂催化劑進(jìn)行了篩選，找到了一種活性較高的NK2型樹(shù)脂催化劑。該樹(shù)脂

2、催化劑在氫醒烷基化合成叔丁基對(duì)苯二酚的應(yīng)用上尚沒(méi)見(jiàn)報(bào)道。2本文以NK2型樹(shù)脂為催化劑研究了叔丁醇和對(duì)苯二酚反應(yīng)的工藝條件，并找到了最佳工藝條件:當(dāng)對(duì)苯二酚加入量為5.5克時(shí)，反應(yīng)溫度為1000C，樹(shù)脂催化劑用量2克，溶劑甲苯30毫升，乙酸丁醋10毫升，無(wú)水硫酸鈉5克，叔丁醇與對(duì)苯二酚摩爾比在0.51之間，叔丁醇滴加時(shí)間為90分鐘一150分鐘，從滴加叔丁醇開(kāi)始的總反應(yīng)時(shí)間為3小時(shí)。在最佳工藝條件上進(jìn)行了實(shí)收反應(yīng)，收率為53.6%，TBHQ

3、選擇性為82.1%，副產(chǎn)物25一二叔丁基對(duì)苯二酚收率為10.2，超過(guò)了文獻(xiàn)報(bào)道同溫度條件下的收率49.2%.3本文研究了磷酸催化下，叔丁醇和對(duì)苯二酚反應(yīng)的工藝條件，找出了最佳工藝:當(dāng)對(duì)苯二酚加入量為28克時(shí)，反應(yīng)溫度為1000C，甲苯用量在60毫升~100毫升之間，磷酸催化劑用量40毫升，叔丁醇與對(duì)苯二酚摩爾比為1左右，叔丁醇滴加時(shí)間在60分鐘一90分鐘，從滴加叔丁醇開(kāi)始的總反應(yīng)時(shí)間為2小時(shí)。本文在最佳工藝條件基礎(chǔ)上，進(jìn)行了實(shí)收反應(yīng)，收

4、率為70.3%TBHQ選擇性為85.5%，副產(chǎn)物25一二叔丁基對(duì)苯二酚收率為9.5%。超過(guò)了專利文獻(xiàn)收率(62.2%11.7%)a4采用高效液相色譜法(HPLC)分析叔丁基對(duì)苯二酚純度和雜質(zhì)含量。采南升‘大學(xué)b頤dt學(xué)位論文AbstracttButylhydroquinoneisusedasanantioxidantincosmeticproductsoilsfatsandmeatproductstopreventrancidityan

5、dasapolymerizationinhibitorforvariouspolyunsaturatedpolyesters.Nowtbutylhydroquinonehasbeenapprovedtobeusedasanantioxidantinfoodproductsandfeedstufinmorethantwentycountiesforitshigheficiencylowtoxicityandothervirtues.Int

6、histhesisakindofionexchangeresinwasfoundwithhighcatalyticactivity.Themaincontentshavebeendrawnasfollows:1.Inthisthesissixkindsofionexchangeresinswerestudiedonekindofionexchangeresin一ModelNK2withhighcatalyticactivityforsy

7、nthesizingtbutylhydroquinonewasfound.Thiskindofresinwasnotreportedbyliterature.2.TheprocessingconditionsinsynthesistbutylhydroquinonewithModelNK2ionexchangeresincatalystwerestudied.Theoptimumprocessingconditionswerefound

8、:hydroquinone5.5greactiontemperature100℃，modelNK2ionexchangeresin2gtoluene30mlbutylacetate10m1anhydroussodiumsulfate5gratioofM_butylalroholangMhydroqutnone:0‘一1thetimefordroppingtbutylalcohol:90minutes一150minutesthereact

9、iontimeis3hours.Inthisconditiontheyield(53.6%)oftbutylhydroquinoneismorethantheyield(49.2%)reportedbyliteraturesatthesamereactiontemperature.3.Theprocessingconditionsinsynthesistbutylhydroquinonewithphosphoricacidcatalys

10、twerestudied.Theoptimumconditions:hydroquinone28greactiontemperature1000Ctoluene60100mlphosphoricacid40m1ratioofMt.butylzlcoholandMhydrognnme:Ithetimedroppingtbutylalcohol:60minutes一90minutesthereactiontimeis2hours.Inthi