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分子筛催化合成2,6-二异丙基萘的初步研究

Study on the Synthesis of 2,6-Diisopropylnaphthalene Using Zeolite as Catalyst

【作者】 杨长喆

【导师】 王成扬;

【作者基本信息】 天津大学 , 化学工艺, 2004, 硕士

【摘要】 2,6-二异丙基萘(2,6-DIPN)是合成新型聚酯树脂聚萘二甲酸乙二醇酯 PEN和聚萘二甲酸丁二醇酯 PBN 以及液晶高分子聚合物 LCP 的重要原料 而且合成 2,6-DIPN 的原料萘和丙烯都是常见的化工原料 所以将 2,6-DIPN 的生产工业化最近几年成为国内外研究的重点 目前研究的重点仍然是找到高活性和高选择性的催化剂 以及优化反应条件提高收率 为此 在本文中首先以国产的催化剂 型分子筛入手 探讨反应条件对反应结果的影响 然后合成新型的大孔径硅磷酸铝分子筛 并进行初步的活性研究具体研究内容如下 1.建立了分析产物的方法 气相色谱法 对产物的色谱峰进行了确定 2.以 型分子筛为催化剂 研究了原料配比 萘与丙烯的比例 催化剂用量 反应温度和反应时间对于萘的转化率 目的产物 2,6-DIPN 的收率和选择性的影响 并通过正交实验确定了该催化剂体系下的最佳反应条件为 原料配比 萘 丙烯 =1:2 催化剂用量 6% 反应温度 270 反应时间控制在 4h 左右 3.通过 XRD 对催化剂反应前后催化剂样品的相对结晶度进行了比较 利用红外光谱法 比表面积法对催化剂进行了表征 4.研究了分子筛的处理方法酸处理脱铝法和液相沉积法对反应结果的影响结果发现分子筛催化剂通过液相沉积法 有效的阻止了萘与丙烯烷基化反应中副反应的进行 5.采用水热法合成新型的硅磷酸铝分子筛 SAPO-5 并通过实验确定了SAPO-5 分子筛的最佳合成条件 AlOOH 为铝源 磷酸为磷源 正硅酸乙酯为硅源 三乙胺为模板剂 R 带有四氟乙烯衬的晶化釜 晶化温度为 200 晶化时间 24h 适宜的物料比为 0.6~2.4SiO2:1.00Al2O3:1.00P2O5:1.00R:40H2O 6.将合成出来的硅磷酸铝分子筛用于萘与丙烯的烷基化反应 进行了活性的研究

【Abstract】 2,6-diisopropylnaphthalene(2,6-DIPN) is a potentially useful raw material forproduction of polyethylene naphthalate (PEN), polybutylene naphalate(PBN) andliquid crystalline polymers (LCP) with superior properties. It can be synthesized fromtwo common chemicals, naphthalene and propylene. How to industrialize the processof producing 2,6-DIPN is getting more and more studied in the world recently. Mostof these studies focused on looking for new catalysts with high activity and selectivityand optimizing the reaction conduction to raise the yield. Therefore, in this paper, the effect of reaction conductions on reaction resultswere studied when β zeolite was used as catalyst. After then, silicoaluminophosphatemolecular sieve with bigger pore diameter was synthesized and the primary activitytests were carried out. The researching content was as follows: 1.Gas chromatography (GC) was employed to determine the concentration ofmost products . 2.When β zeolite was used as catalyst, the effects of the ratio of propylene andnaphthalene, catalyst concentration, reaction temperature and reaction time on theconversion (based on naphthalene), yield and selectivity (both based on 2,6-DIPN)were discussed. In addition, by orthogonal experiment, the optimum reactionconditions were determined at the same time. The optimum reaction conditions :the molar ratio of propylene and naphthalene =1:2, catalyst concentration=6%,reaction temperature was 270 , reaction time was about 4h. 3.By XRD, the relative crystallinity of samples was compared. In addition,catalyst was analyzed by FI-IR and BET. 4.The influence of catalyst treatment, such as acid –dealumizition and liquiddeposition, were researched. At last, it was found that by liquid deposition thesubsidiary reaction was prevented efficiency during isopropylation of naphthalenewith propylene. 5.The silicoaluminophosphate molecular sieve (SAPO-5) with relative biggerpore diameter was synthesized hydrothermally. The optimum synthesis condition wasdetermined through experiments which were as follows: AlOOH as the aluminumsource, orthophosphoric acid as the phosphor source, triethylamine as the templateagent (R), a stainless steel autoclave with Teflon liner as the crystallizing kettle,crystallization temperature is 200 , crystallization time is 24h. The gel composition II<WP=5>is 0.6~2.4SiO2:1.00Al2O3:1.00P2O5:1.00R:40H2O 6.The catalytic activity of SAPO-5 sieve was studied in the alkylation of naphth-alene with propylene .

  • 【网络出版投稿人】 天津大学
  • 【网络出版年期】2004年 04期
  • 【分类号】O643.3
  • 【被引频次】2
  • 【下载频次】315
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