无机化学学报
無機化學學報
무궤화학학보
JOURNAL OF INORGANIC CHEMISTRY
2009年
1期
104-111
,共8页
周荣飞%付桂云%胡娜%袁慧%林晓%徐南平%陈祥树
週榮飛%付桂雲%鬍娜%袁慧%林曉%徐南平%陳祥樹
주영비%부계운%호나%원혜%림효%서남평%진상수
T型分子筛%微波加热%普通加热%水热合成%机理
T型分子篩%微波加熱%普通加熱%水熱閤成%機理
T형분자사%미파가열%보통가열%수열합성%궤리
zeolite T%conventional heating%microwave heating%hydrothermal crystallization%mechanism
研究了微波场中T型分子筛的结晶过程.考察了微波加热体系中合成参数如合成时间、溶胶组成、反应压力和模板剂用量对分子筛晶化的影响.微波加热的主要优点是减少合成时间.无模板剂的溶胶在普通加热条件下的晶化时间需要120 h,而在微波场中则仅需要20~25 h.另一方面,由于微波的快速加热特性促进了稳定相钙十字沸石的生成,从而减小了次稳定相T型分子筛的结晶区间.在未添加模板剂条件时,100 ℃下微波水热合成T型分子筛的结晶区间为:20≤nsio2/nAl2O3≤22和0.31≤nM2O/nSiO2≤0.33(其中M2O=Na2O+K2O,nNa/nk=3和nsiO2/nH2O=11.70).在普通加热和微波加热合成体系中,添加模板剂均能扩大结晶区间.同时还可以进一步减少合成时间.
研究瞭微波場中T型分子篩的結晶過程.攷察瞭微波加熱體繫中閤成參數如閤成時間、溶膠組成、反應壓力和模闆劑用量對分子篩晶化的影響.微波加熱的主要優點是減少閤成時間.無模闆劑的溶膠在普通加熱條件下的晶化時間需要120 h,而在微波場中則僅需要20~25 h.另一方麵,由于微波的快速加熱特性促進瞭穩定相鈣十字沸石的生成,從而減小瞭次穩定相T型分子篩的結晶區間.在未添加模闆劑條件時,100 ℃下微波水熱閤成T型分子篩的結晶區間為:20≤nsio2/nAl2O3≤22和0.31≤nM2O/nSiO2≤0.33(其中M2O=Na2O+K2O,nNa/nk=3和nsiO2/nH2O=11.70).在普通加熱和微波加熱閤成體繫中,添加模闆劑均能擴大結晶區間.同時還可以進一步減少閤成時間.
연구료미파장중T형분자사적결정과정.고찰료미파가열체계중합성삼수여합성시간、용효조성、반응압력화모판제용량대분자사정화적영향.미파가열적주요우점시감소합성시간.무모판제적용효재보통가열조건하적정화시간수요120 h,이재미파장중칙부수요20~25 h.령일방면,유우미파적쾌속가열특성촉진료은정상개십자비석적생성,종이감소료차은정상T형분자사적결정구간.재미첨가모판제조건시,100 ℃하미파수열합성T형분자사적결정구간위:20≤nsio2/nAl2O3≤22화0.31≤nM2O/nSiO2≤0.33(기중M2O=Na2O+K2O,nNa/nk=3화nsiO2/nH2O=11.70).재보통가열화미파가열합성체계중,첨가모판제균능확대결정구간.동시환가이진일보감소합성시간.
The crystallization of Zeolite T under microwave-heating system was studied. The effects of synthesis parameters such as synthesis time, gel composition, reaction pressure and template on crystallization were investigated.The results show that the crystalline zeolite T is obtained in 20-25 h without template under the microwave hydrothermal treatment in contrast to more than 120 h by conventional heating method. The crystallization fields of the metastable phase of zeolite T is narrowed due to the favored formation of the stable phase of phillipsite by the fast heating of microwave irradiation. The formation fields of zeolite T without template under microwave hydrothermal synthesis are: 20 ≤nsiO2/nAl2O3≤22 and 0.31 ≤nM2O/nsiO2≤0.33(where M2O=Na2O+K2O2,nN/nK=3 and nsio2/nH2o =11.70) at 100C. The addition of template(tetramethylammonium(TMA) cation) will broaden the crystallization field of zeo- lite T and further reduce the synthesis time in both of the microwave-heating system and the conventional-heating system.