(CN107497479) Method for preparation of methyl methoxyacetate from beta molecular sieve synthesized with cordierite as carrier 机翻标题: 暂无翻译,请尝试点击翻译按钮。

源语言标题
(CN107497479) Method for preparation of methyl methoxyacetate from beta molecular sieve synthesized with cordierite as carrier
公开号/公开日
CN107497479CN107497479 / 2020-06-232017-12-22
申请号/申请日
CN201710593246 / 2017-07-20
发明人
SHI LEIWANG YANZHANG DONGXI;
申请人
SHENYANG UNIVERSITY OF CHEMICAL TECHNOLOGY;
主分类号
IPC分类号
B01J-029/70 B01J-035/10 C07C-067/36 C07C-069/708
摘要
(CN107497479) The invention relates to a method for preparation of methyl methoxyacetate from a beta molecular sieve synthesized with cordierite as the carrier. The method includes: taking a cordierite ceramic honeycomb as the carrier, daubing a silicon source to the carrier surface by ultrasonic impregnation method, conducting drying and roasting, then stirring the obtained substrate, an aluminum source, an alkali solution and a template agent at normal temperature for certain period of time, transferring the mixed solution into a stainless steel hydrothermal synthesis kettle with a polytetrafluoroethylene liner, also performing mesoporous modification on the synthesized Hbeta/cordierite molecular sieve with acid and alkali solution respectively, and applying the synthesized molecular sieve to methylal carbonylation reaction to prepare methyl methoxyacetate. Compared with the Hbeta/cordierite molecular sieve, the molecular sieve subjected to mesoporous modification can achieve obviously increased methylal conversion rate, and the product methyl methoxyacetate has obviously improved mass selectivity. The method has the advantages of simple process, convenient raw material sources, few by-product, simple reaction aftertreatment and small environmental pollution, and provides a new thinking and method for large-scale industrial production.
机翻摘要
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地址
代理人
(CN107497479B) ZHANG ZHIGANG ; SHENYANG JILIAN PATENT AGENCY CO. LTD. Reg. Nb: 21205
代理机构
;
优先权号
2017CN-0593246
主权利要求
(CN107497479) 1.一种堇青石为载体合成β分子筛制备甲氧基乙酸甲酯方法,其特征在于,所述方法包括以下步骤:   1)对堇青石基体进行预处理,在室温下,将堇青石浸泡在2mol.L-1的酸溶液中,再经过烘干和焙烧制得备用的堇青石蜂窝陶瓷基体;   2)将焙烧后的堇青石蜂窝陶瓷基体放置在2mol.L-1的SiO2凝胶中,利用超声浸渍法将硅源均匀的附着在基体表面,浸渍时间1h;将基体放置于烘箱中60℃烘干、马弗炉550℃焙烧4h后得到过渡涂层的基体;   3)将表面附着有SiO2的过渡基体、3mol.L-1铝酸钠、TEAOH及0.5mol.L-1NaOH溶液按照一定的比例在常温下充分搅拌1~2h;   4)将溶液转移到具有聚四氟内衬的不锈钢水热合成釜内,120℃晶化4天,反应时间到,水热合成釜冷却至室温并对溶液抽滤,水洗至中性;   5)在烘箱中于110~120℃下干燥10-12 h;   6)将干燥后的催化剂前体在马弗炉中于550-650℃下焙烧3-5 h,得到Na-β分子筛或β分子筛;   7) Na-β分子筛需要在60~100℃下与1mol.L-1NH4NO3或NH4Cl溶液离子交换,经过抽滤、水洗、烘干、焙烧后的到Hβ/堇青石分子筛   制备介孔β:   用酸性溶液脱除分子筛骨架中的Al,将5g Hβ/堇青石分子筛加入到200mL浓度为2mol.L-1的盐酸、硝酸、醋酸、磷酸、硫酸、或柠檬酸中在100℃回流装置下反应3h,再经过抽滤、水洗至中性,连续交换3次后,将分子筛放置烘箱中120℃烘干12h;   将烘干后的分子筛再与120mL氢氧化钠或氨水溶液反应,脱除骨架中的Al;碱溶液浓度为0.1mol.L-1,在80℃回流装置下反应1h,经过抽滤、水洗至中性后与烘箱中120℃烘干12h,再经过马弗炉550℃焙烧5h,此时制备出来的分子筛记为H-meso-β;   在固定床反应器中,分别装入上述制备的催化剂1 g,反应管内压强为5Mpa;流量为50mL/min 99.9999% CO在25℃下通过装有98wt%甲缩醛的不锈钢反应罐携带DMM的饱和蒸气混合进入反应管,通过调节背压阀以维持反应管压力恒定;反应温度为90℃,DMM转化率为99.45%,产物MMAc选择性为92.22%。
法律状态
GRANTED
专利类型码
BA
国别省市代码
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