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季戊四醇下游产品的开发研究

The Exploration of the Downstream Products of Pentaerythritol

【作者】 林裕

【导师】 曲济方;

【作者基本信息】 山西大学 , 应用化学, 2009, 硕士

【摘要】 结合山西省煤化工产业结构调整,为扩大煤化工产业链,对季戊四醇高附加值的下游产品开发进行了两方面的应用研究:1、由季戊四醇制备双季戊四醇:探讨了在现有季戊四醇间歇生产工艺的反应体系中添加季戊四醇制备双季戊四醇的工艺条件,实验考察了10个方面的影响因素,筛选出了较佳工艺条件:(1)原料投料比为:n(季戊四醇):n(氢氧化钠):n(甲醛):n(乙醛)=1:1.2:4.1:1,采用无碱底液法,底液由季戊四醇、水及整体投料甲醛的25%组成,其中m(季戊四醇):m(水)=1:2。(2)采用二级控温生产,第一阶段反应控温于20℃,将氢氧化钠、甲醛和乙醛混合液同时分别注入,投料时间75 min。第二阶段反应控温于80℃,反应时间2h。该工艺在较低浓度甲醛(31%)和乙醛(40%)的条件下,单程季戊四醇收率为41.14%,双季戊四醇收率为37.26%,与国内近期最佳研究结果相比,季戊四醇消耗量减少1/6,降低了生产成本,有较好的经济效益。2、以季戊四醇为中心核的紫外光固化水性超支化聚酯的合成及性能研究由季戊四醇与2,2-二羟甲基丙酸反应制备了8个端羟基的多元醇,并用丁二酸酐进行羧基封端,再用甲基丙烯酸缩水甘油酯与部分羧基反应接枝,最后用三乙醇胺中和其余羧基。通过调整紫外光固化和亲水性基团的比例,合成了三种紫外光固化水性超支化聚酯,并考察了这三种聚酯的相关性质。结果表明:所得聚酯水溶液具有固含量高、粘度低、易涂布的特点,而且储存稳定性良好,光固化时间短,耐溶剂性好,具有潜在应用价值。

【Abstract】 In view of the coal chemical industrial restructuring in Shanxi province, two kinds of downstream products of pentaerythritol with the high added value was explored for expending coal chemical industry chains:1.Preparation of dipentaerythritol from pentaerythritolOne systhetic process for dipentaerythritol,in which pentaerythritol was added into the reaction system of the present intermittent production of pentaerythritol,was proposed.The ten factors were studied and the optimal conditions were obtained:The molar ratio of raw materials:n(pentaerythritol):n(sodium hydroxide):n(formaldehyde):n(aldehyde) = 1:1.2:4.1:1.The substrate which was alkali-free consisted of pentaerythritol,water and 25%in the overall formaldehyde,and the mass ratio of pentaerythritol to water was one second.The reaction was carried out successively in two-level temperature. The temperature for the first stage was keeped at 20℃.Sodium hydroxide, and the mixture of formaldehyde and acetaldehyde was added simultaneous -ly within 75 min.The temperature for the second stage raised up to80℃and was maintained for 2 h.41.14%of one-way yield of pentaerythritol and 37.26%of one-way yield of dipentaerythritol could be obtained using the developed process under the conditions of low concentrations of formaldehyde(31%) and acetaldehyde(40%).Compared with the recent domestic results,the consumption of pentaerythritol was reduced by one sixth reduction.Thus, the cost of production was lowered.Therefore,those findings could bring about better cost-effectiveness and was really meaningful to small and medium-sized manufacturers.2.Study on synthesis and performance of UV-curable waterborne hyperbranched polyester using pentaerythritol as core Hydroxy-terminated 8-polyols was prepared by reaction of pentaeryth -ritol and 2,2-dimethylolpropionic acid.And the polyols was end-capped with succinic anhydride,and then the resulting carboxy groups partially reacted with glycidyl methacrylate.Finally,the rest of carboxy groups were neutralized by triethanolamine.By adjusting the molar ratio of UV-curable and hydrophilic groups,three kinds of UV-curable hyperbran -ched waterborne polyester were synthesized,and their properties were investigated.The results showed that the aqueous solution of obtained polyester had the properties of a high solid content,low viscosity, easy-coating,and had good storage stability,short UV-curable time and good solvent resistance,which had potential application value.

  • 【网络出版投稿人】 山西大学
  • 【网络出版年期】2011年 S1期
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