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1、石油學(xué)報(bào)(石油加22)2012年2月ACTAPETROLEISINICA(PETROLEUMPROCESSINGSECTION)第28卷第1期文章編號(hào):1001—8719(2012)01—0050—05L/MCM一41介微孑L復(fù)合分子篩合成的影響因素王春芳,陳宜假,郭士嶺,張忠東,高雄厚(1.鄭州大學(xué)化工與能源學(xué)院,河南鄭州450001;2.中國石油天然氣股份有限公司石油化工研究院,甘肅蘭州730008)摘要:以十六烷基三甲基溴化銨(CTAB)為模板劑,采用兩步晶化法先合成L分子篩,再合成L/MCM一41復(fù)合分子篩,合成過程中采用了離子交換技術(shù)
2、。用XRD、BET等測(cè)試手段對(duì)合成樣品進(jìn)行表征。考察了合成體系pH值、模板劑用量、晶化溫度對(duì)合成產(chǎn)物的影響。結(jié)果表明,用硫酸調(diào)節(jié)合成體系pH值在1O~11范圍,以及n(CTAB)/n(SiOz)一0.25、120℃晶化2d的條件下,合成得到的L/MCM一41復(fù)合分子篩孔徑比微孔分子篩大,為3.04nm;與水熱晶化法合成的McM41相比,壁厚由0.55nrn增大到1.81nm;水熱穩(wěn)定性也明顯提高,在100℃沸騰狀態(tài)下結(jié)構(gòu)保持時(shí)間由原來的低于2h延長到8h。關(guān)鍵詞:離子交換;復(fù)合分子篩;介一微孔復(fù)合分子篩;L/MCM一41中圖分類號(hào):TQ17,T
3、Q424.25文獻(xiàn)標(biāo)識(shí)碼:Adoi:10.3969/j.issn.1001-8719.2012.01.009InfluenceFactorsofSynthesisofMeso--Micro—-PorousCompositeMolecularSieveofL/MCM-41WANGChunfang,CHENYiliang,GUOShiling,ZHANGZhongdong。,GAOXionghou。(1.SchoolofChemicalEngineering,ZhengzhouUniversity,Zhengzhou450001,China;2.P
4、etrochemicalResearchInstitute,CNPC,Lanzhou730008,China)Abstract:Meso—micro—porousL/MCM一41compositemolecularsievewassynthesizedbytWO—stepcrystallization.ThefirststepwastopreparezeoliteLandthesecondstepwastosynthesizeL/MCM~41compositemolecularsievewithcetyltrimethylammoniumbro
5、mide(CTAB)astemplateandthetechnologyofionexchange.TheproductswerecharacterizedbyX—raydiffraction(XRD)andBET.Theeffectsofthesynthesisconditions,includingpHvalue,(CTAB)/n(SiO2)andcrystallizingtemperaturewerestudied.Itwasindicatedthattheoptimalconditionsofsynthesiswereasfollows
6、:pHvaluerangeof10~11,(CTAB)/n(SiO2)一0.25,crystal1izationtemperatureof12O℃,andcrvstallizationtimeof2d,underwhichtheporediameteroftheobtainedL/MCM一41compositemolecularsievewas3.04nm,biggerthanthatofmicro—porousmolecularsieves.ComparedwithMCM一41synthesizedbyordinaryhydrothermal
7、method,theporewallthicknessoftheobtainedL/MCM一41compositemolecularsievewasraisedfrom0.55nmto1.81nm,andthehydrothermalstabilitywasbetter,thatwas,themeso—porousstructurecouldkeepunchangedfor8hat100℃,insteadof2h.Keywords:ionexchange;compositemolecularsieve;meso—micro—porouscomp
8、ositemolecularsieve:L/MCM一41收稿日期:2010一l2—23基金項(xiàng)目:中國石油天然氣股份有限公司沸石型高性能半再生重整催化劑