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题名:
丙烯酸酯与1-辛烯的共聚研究
作者: 陈莉
答辩日期: 2014-05-22
导师: 吾满江·艾力
专业: 有机化学
授予单位: 中国科学院大学
授予地点: 北京
学位: 硕士
关键词: 润滑油 ; 1-辛烯 ; 丙烯酸异辛酯 ; 共聚 ; 转化率
摘要:

本论文以1-辛烯和丙烯酸酯的自由基共聚反应制备高性能润滑油基础油为研究内容,并测试合成的润滑油基础油的理化指标,通过优化反应工艺条件,获得了粘度指数高、分子量分布较窄、具有粘度指数改进剂功能的润滑油基础油。本论文的主要研究内容和结论如下: ⑴ 引发剂对1-辛烯与丙烯酸异辛酯发生共聚合的影响 分别采用过氧化二异丙苯(DCP)、过氧化苯甲酸叔丁酯(TBPB)、过氧化二叔丁基(DTBP)为引发剂,引发1-辛烯与丙烯酸异辛酯的共聚反应。用凝胶渗透色谱仪(GPC)测试聚合产物的分子量和分子量分布。分析结果表明,以过氧化二叔丁基(DTBP)为引发剂,1-辛烯能够参与共聚反应,并且可以获得分子量分布最窄的聚合产物。因此,过氧化二叔丁基是本论文最为适宜的引发剂。 ⑵ 1-辛烯与丙烯酸异辛酯本体聚合制备润滑油基础油 以过氧化二叔丁基(DTBP)为引发剂,研究了引发剂用量、反应温度、反应时间、反应物摩尔比等对聚合产物的收率及其性能的影响。实验结果表明,引发剂用量大于3%(质量分数),反应温度高于110℃时,1-辛烯能较好地参与共聚反应,反应在12h基本完成,较好的反应条件是反应温度为130℃,引发剂用量为6%。凝胶渗透色谱(GPC)测定结果显示,聚合产物的重均分子量为7800~61100,分子量分布在2.3左右。聚合产物的粘度指数在200~380之间,证明其可用作粘度指数改进剂。同时,闪点、倾点测试的结果表明此共聚物可以用作良好的润滑油基础油 ⑶ 提高1-辛烯转化率的探索 升高反应温度、增加引发剂的用量、减小反应物中1-辛烯的比例均可以提高1-辛烯的转化率。在此基础上,尝试通过改变引发剂的加入方式以及聚合方法来 提高1-辛烯转化率。结果表明,将引发剂一次加入以及使用溶液聚合体系均能提高1-辛烯的转化率,溶液聚合中溶剂对1-辛烯的转化率、共聚物的粘度、分子量及分子量分布等性能也有较大的影响,其中最适宜的溶剂是二甲苯。在二甲苯中,1-辛烯的转化率最高,可达到97.8%,所得聚合产物粘度指数较高,倾点最低,碘值为零。以上结果表明,提高1-辛烯的转化率要综合投料比、反应温度、引发剂用量及加入方式、聚合反应体系这几方面的因素。

英文摘要:

This thesis focuses on the free radical copolymerization between 1-octene and acrylate to prepare high performance base oils, and the physical and chemical properties of the synthetic base oils were tested. The base oils with high-viscosity index and narrow molecular weight distribution were synthesized, which could be used as viscosity index improver. The main contents and conclusions of this paper are listed as follows: (1) Effects of the initiators on the copolymerization between 1-octene and acrylate Dicumyl peroxide (DCP), t-butyl perbenzoate (TBPB), di-tert-butyl peroxide (DTBP) were selected as the initiators to initiate the copolymerization between 1-octene and iso-octyl acrylate, respectively. The products obtained in this paper were characterized via gel permeation chromatography (GPC). The results show that 1-octene can participate in the copolymerization reaction when DTBP used as the initiator, and the product with the most narrow molecular weight distribution was obtained. Therefore, DTBP is the best initiator in this paper. (2) Preparation of base oil via the bulk polymerization between 1-octene and iso-octyl acrylate Effects of the reaction parameters including the dosage of initiator (DTBP), reaction temperature, reaction time, the mole ratio of 1-octene to iso-octyl acrylate on the yield of the products and its performances were investigated. It was found that the high conversion of 1-octene was obtained at reaction time 12h, with reaction temperature above 110℃ and the amounts of initiators more than 3.0 w.t% (counted by all reagents). The optimum condition was as follows: reaction temperature 130 ℃, dosage of the initiator 6.0 w.t%. Under these conditions, the weight-average molecular weight of these polymers are from 7800 to 61100 and the molecular weight distribution index 2.3. The viscosity index of synthesized base oils range from 200 to 380 were produced, which hold great promise as lubricating base oils and viscosity index improvers. (3) Optimization of the reaction conditions to improve the conversion of 1-octene The conversion of 1-octene could be improved by raising reaction temperature, increasing the dosage of initiator, reduction of the mole ratio of 1-octene to acrylate as the experiment data suggested. Besides, the way of adding the initiator and the solution polymerization system were studied. It was confirmed that the conversion of 1-octene could be improved via solution polymerization system instead of the bulk polymerization and adding all the initiator at one time, and the copolymer’s properties such as viscosity, molecular weight and molecular weight distribution were also changed. The best solvent is xylene, in which the conversion of 1-octene could reach 97.8% and the product with high viscosity index, the lowest pour point, with iodine value zero. Therefore,it is necessary to give overall consideration of the factors such as the mole ratio of 1-octene to acrylate, reaction temperature, dosage of initiator and its adding method, polymerization system to obtain a high conversion of 1-octene.

内容类型: 学位论文
URI标识: http://ir.xjipc.cas.cn/handle/365002/3420
Appears in Collections:新疆维吾尔自治区精细化工工程技术研究中心_学位论文

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作者单位: 中国科学院新疆理化技术研究所

Recommended Citation:
陈莉. 丙烯酸酯与1-辛烯的共聚研究[D]. 北京. 中国科学院大学. 2014-05-22.
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