共查询到19条相似文献,搜索用时 171 毫秒
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以降冰片烯二酸酐为起始原料, 经水解中和和催化加氢制备了双环[2.2.1]-庚烷-2,3-二羧酸钠。通过研究催化加氢步骤中催化剂种类、催化剂用量、反应温度和反应压力等关键因素对双环[2.2.1]-庚烷-2,3-二羧酸钠的收率和纯度的影响, 获得了适宜的反应条件。实验结果表明:催化剂雷尼镍可代替文献报道的价格昂贵的钯/炭催化剂完成催化加氢反应, 在反应温度为60℃、反应压力为5MPa的条件下进行催化加氢, 双环[2.2.1]-庚烷-2,3-二羧酸钠的收率大于95%;红外光谱及核磁共振分析表明, 所得加氢产物与双环[2.2.1]-庚烷-2,3-二羧酸钠结构特征吻合。 相似文献
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以环戊二烯与顺丁烯二酸酐为原料,通过Diels-Alder反应合成了聚丙烯成核剂中间体二环[2.2.1]庚-5-烯-2,3-二酸酐。通过实验确定了合成二环[2.2.1]庚-5-烯-2,3-二酸酐的优化条件为:顺丁烯二酸酐与环戊二烯摩尔比1.000∶1.050;溶剂石油醚与乙酸乙酯等体积混合,溶剂用量占进料总质量的46%;环戊二烯滴加温度控制在10~15℃,滴加30 min;升至60℃,继续反应20 min。在优化条件下,二环[2.2.1]庚-5-烯-2,3-二酸酐的收率大于95%。熔点、元素分析、红外光谱及X射线衍射分析均表明合成产物为目标产物。 相似文献
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以丙烯腈、莰烯和发烟硫酸为原料,合成了2-丙烯酰胺基-7,7-二甲基-1-磺酸甲基二环[2.2.1]庚烷;在适量的添加剂存在下,可提高产率到72%。并借助红外光谱、核磁共振和质谱确定了产物的结构。结果表明,2-丙烯酰胺基-7,7-二甲基-1-磺酸甲基二环[2.2.1]庚烷分子中含有"C═C"、二环[2.2.1]庚烷和磺酸基团,可以作为水溶性聚合物功能单体。 相似文献
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二环[2.2.1]庚烷二羧酸盐和二环[2.2.2]庚烷二羧酸盐是重要的分散型聚丙烯成核剂,HPN-68是最优秀的商业化产品。该类成核剂最大的特点是可以提高聚丙烯的结晶温度和改性PP收缩的各向同性。详细介绍了该类成核剂的结构、制备方法和在聚丙烯中的应用。 相似文献
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以聚四苯基卟啉(P-TPP)为敏化剂,研究了2,3-二羧基-双环[2.2.1]-2,5-庚二烯(N)的光化学价键异构化反应,在0.1mol/L的碳酸钠甲醇溶剂中,在适量的P-TPP存在下,可见光照射时,N可以定量地转化为2,3-二羧基四环[2.2.1.0~(2,6).0~(3,5)]庚烷(Q),Q在聚四苯基卟啉钴络合物(Co-P-TPP)催化剂的作用下,又可定量地异构化返回N.分别研究了敏化剂和催化剂用量对反应的影响.通过反应物之间激发态能量的比较及N对P-TPP荧光的猝灭试验,证明光异构化反应是通过电子转移反应机制进行的. 相似文献
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以对苯醌和乙酸酐为起始原料,浓硫酸为催化剂,在常温常压下经Thiele反应生成1,2,4-苯三酚三乙酸酯;然后以浓硫酸为催化剂和脱水剂,将1,2,4-苯三酚三乙酸酯与苹果酸经Pechmann反应生成6,7-二羟基色烯-2-酮;再与3-氯环氧丙烷环合最终生成目标化合物2-羟甲基-2,3-二氢-1,4-二噁英并[2,3-g]色烯-7-酮,总收率为43.7%(以对苯醌计)。目标化合物的结构经IR、1H NMR和MS初步确证。该合成路线具有操作简单,反应条件温和、选择性高、成本低、环境友好。 相似文献
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The relative reactivity of 2,3‐dicarbomethoxy‐5‐norbornenes in metathesis polymerization using the original n‐chelating ruthenium carbene complex 下载免费PDF全文
1H NMR spectroscopy is used to study the kinetics of metathesis copolymerization of three isomeric 2,3‐dicarbomethoxy‐5‐norbornenes using the original N‐chelating ruthenium carbene complex. Based on the experimental data the copolymerization constants of isomeric 2,3‐dicarbomethoxy‐5‐norbornenes are calculated. It is shown that the relative reactivity of endic acid dimethyl ester—(1R,2S,3R,4S)‐dimethyl bicyclo[2.2.1]hept‐5‐ene‐2,3‐dicarboxylate is almost two times lower than the corresponding values for (1R,2R,3S,4S)‐dimethyl bicyclo[2.2.1]hept‐5‐ene‐2,3‐dicarboxylate, which confirms earlier findings of steric hindrance in the orientation of the monomer due to the carbene catalyst. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40130. 相似文献
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The mechanical and optical properties of iPP nucleated with bicyclo[2.2.1]heptenedicarboxylate salts (BCHED) have been investigated. The results showed that aluminum bicyclo[2.2.1]heptenedicarboxylate (BCHE13) is the most effective nucleating agent to improve the mechanical and optical properties. Then the effects of the BCHE13 concentration on mechanical and optical properties and crystallization behaviors were studied. The results indicated that the saturated concentration of BCHE13 is about 0.2 wt %, at which nucleated iPP showed the better comprehensive mechanical and optical properties and high crystallization peak temperature. Nonisothermal crystallization kinetics of iPP nucleated with different BCHE13 contents have been investigated by Caze method. The results indicated Avrami exponents of nucleated iPP gradually increased with the increasing of BCHE13 concentration. The results can be explained that crystallization and growth model of nucleated iPP is heterogeneous nuclei followed by more than three‐dimension spherical growth during nonisothermal crystallization, which can be proved by agglomeration of BCHE13 in melt iPP. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 相似文献
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A series of novel thieno[2,3-b]pyridines were prepared from the reaction of the appropriate bromoacetylbenzofurans or bromoacetylbenzothiazole with the corresponding pyridinethione derivatives in ethanolic sodium ethoxide at reflux. Moreover, new bis(thieno[2,3-b]pyridine) derivatives have also been synthesized by the reaction of the appropriate bis-bromoacetyl derivatives with the corresponding pyridinethiones in the presence of sodium ethoxide. Attempts to synthesize the target bis(thieno[2,3-b]pyridine) derivatives by bis-alkylation of the corresponding (thieno[2,3-b]pyridin-2-yl)(hydroxyphenyl)methanone with the appropriate dihaloalkanes using a mild base were unsuccessful. 相似文献
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A highly active novel β-nucleating agent for isotactic polypropylene (iPP), cadmium bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylate (BCHE30), was found and its effects on the mechanical properties, the content of β-crystal, and crystallization behavior of iPP were investigated, respectively. The results show that the impact strength and crystallization peak temperature of nucleated iPP are greatly increased, while the spherulite size of nucleated iPP is dramatically decreased than that of pure iPP. The content of β-form of nucleated iPP (kβ value) can reach 87% with 0.1 wt% BCHE30. The Caze method was used to study the non-isothermal crystallization kinetics of nucleated iPP and the crystallization active energy was achieved by Kissinger method. 相似文献
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离子液体N-甲基咪唑对甲苯磺酸盐催化剂的制备及应用 总被引:1,自引:0,他引:1
采用一步法制备Brφnsted酸性离子液体N-甲基咪唑对甲苯磺酸盐催化剂([Hmjm]TsO),并对其进行了红外光谱、拉曼光谱等表征。将其应用于醋酸和正丁醇的酯化反应,详细考察了离子液体用量、反应时间、醇酸物料比、反应温度等因素对酯化反应的影响,并确定了较佳反应条件为:温度95~98℃,n(丁醇):n(醋酸):1.2:1,离子液体用量为反应物总质量的20.O%,反应时间6h,酯化率可达到85.0%。同时,[Hmim]TsO离子液体循环使用6次后,酯化率仍可达到78.2%。 相似文献
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降冰片烯衍生物的开环易位聚合具有反应条件温和、反应速率快及尺寸可控等优点,且因其独特的结构使得聚合物主链具有良好的热稳定性及耐酸碱性能。本文通过开环易位聚合法制备了降冰片烯基苯磺酰氯(NBSC)与5-降冰片烯-2,3-二羧酸二甲酯(DCNM)的新型二元无规共聚物。通过FT-IR、NMR表征了单体和共聚物的化学结构,并通过设计对比实验探究了最佳反应条件。GPC数据显示,当两单体配比1:1,催化剂用量为单体总物质的量1/450,反应时间30 min,反应温度40℃时,共聚物的相对分子质量最大,分子量分布较窄,产率最高,此条件为最佳反应条件。DSC表明,DCNM单体均聚物的Tg为60℃,与NBSC共聚后,Tg升高至80℃左右。TGA数据显示共聚物质量分解5%时对应的温度为145℃,最大分解速率时的温度为245℃,证明该聚合物具有良好的热稳定性。综合考虑其各项性能,这种新型的聚合物有望用于燃料电池质子交换膜领域的研究。 相似文献
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以季铵盐和氢氧化钠为原料,经Hofmann消除反应合成了[2,2]-对二甲苯环二体及其氯代物。考察了催化剂种类、反应物料摩尔比、反应温度、反应时间等因素对收率的影响。合成[2,2]-对二甲苯环二体的较优工艺条件为:苯醌为催化剂,n(NaOH):n(季铵盐)=5:1,120℃反应12h,[2,2]-对二甲苯环二体的收率为51.2%。合成氯代-[2,2]-对二甲苯环二体的较优工艺条件为:苯醌为催化剂,n(NaOH):n(季铵盐)=5:1,采用将氢氧化钠溶液滴入季铵盐的反滴工艺,110℃反应14h,氯代-[2,2]-对二甲苯环二体的收率为48.6%。用IR、1HNMR对产物结构进行了表征。 相似文献
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采用改进的Rose汽液平衡釜,测定了在12.0kPa压力下的乙烯基降冰片烯精馏体系中环己烷(CH)-乙烯基环己烯(VCH),环己烷(CH)-乙烯基降冰片烯(VNB),环己烷(CH)-四氢茚(THI)的汽液平衡数据,并进行了热力学一致性验证,由所测数据回归出三组用于该体系Wilson方程的配偶参数,并证明了Wilson方程可以较好地关联环己烷-乙烯基降冰片烯体系的汽液平衡.为乙烯基降冰片烯精馏体系的开发与设计提供了基础数据. 相似文献