一种新型复合型受阻酚抗氧剂的合成及应用
发布时间:2018-05-12 18:05
本文选题:抗氧剂 + 受阻酚 ; 参考:《大连海事大学》2017年硕士论文
【摘要】:高分子材料在使用或者贮存过程中,受光、热、金属离子等外部影响,会出现变色、发粘、变硬发脆、裂纹等老化现象,致使材料力学机械性能降低,最终失去使用价值。为了克服这些问题,延长材料的使用寿命,提高使用价值,人们在高分子材料加工和使用过程中加入了一些物质来延缓老化,这就是抗氧剂。在高分子材料领域应用最多的抗氧剂是受阻酚类抗氧剂。传统受阻酚抗氧剂在使用过程中,一般作为主抗氧剂添加到制品中,同时需要硫醚等辅助抗氧剂的加入来配合使用,二者通过协同作用共同达到抑制聚合物老化的目的。然而,这种多组分的抗氧体系在使用过程中存在较多的缺点,如相容性差,协同效果不好等。本文研究的目的就是旨在解决这一问题。本文从分子水平上设计了一种新型的受阻酚抗氧剂2,4-二叔丁基-6-正辛基硫亚甲基苯酚。对其合成方案进行了考察,最终以2,4-二叔丁基苯酚、多聚甲醛、正辛硫醇等原料合成出目标产物。在此基础之上,对可行的反应催化剂进行筛选,优化反应的各项工艺条件,提高产率,为工业扩大生产提供参考。工艺优化结果结果显示:(1)使用二丙胺为催化剂,2,4-二叔丁基苯酚、正辛硫醇、多聚甲醛的摩尔配比1:1:2,二丙胺用量为反应物总质量的10%,同时添加占反应物总质量1.5%的碳酸氢钾,DMF为溶剂,通入氮气保护,110℃回流反应4小时。在此优化的反应条件下,进行重复性实验,产物收率为86%左右。(2)使用哌啶作为催化剂,反应物2,4-二叔丁基苯酚、正辛硫醇、多聚甲醛的较佳摩尔配比为1:1:2.5,啶用量为反应物总质量的15%,溶剂DMF,通氮气保护,120℃回流反应5小时。在优化条件下进行重复性实验,收率在87.7%左右。将合成的抗氧剂应用在丁苯胶乳的防老中,通过黄变实验,证明其具有优于传统受阻酚抗氧剂BHT的抗氧化性能,并对其使用过程中可能存在的问题提出了参考性建议。
[Abstract]:During the use or storage of polymer materials, due to the external influence of light, heat, metal ions and so on, the aging phenomena such as discoloration, stickiness, hardening and brittle, crack and so on will appear, resulting in the mechanical properties of materials being reduced, and finally losing the use value. In order to overcome these problems, prolong the service life of materials and improve the use value, people add some substances in the process of processing and use of polymer materials to delay aging, which is called antioxidant. Hindered phenolic antioxidants are the most widely used antioxidants in the field of polymer materials. Traditional hindered phenol antioxidants are generally added to the products as main antioxidants and need the addition of auxiliary antioxidants such as sulfides to achieve the purpose of inhibiting the aging of polymers through synergistic effect. However, this multicomponent antioxidant system has many disadvantages in the process of application, such as poor compatibility and poor synergistic effect. The purpose of this paper is to solve this problem. In this paper, a new hindered phenol antioxidant 2o 4- di tert Ding Ji-6 octyl thiomethylphenol was designed at the molecular level. The synthetic scheme was investigated and the target product was synthesized from 2o 4 di tert Ding Ji phenol, paraformaldehyde, n-octyl mercaptan and so on. On the basis of this, the feasible catalyst was screened, the reaction conditions were optimized, the yield was increased, and the reference was provided for the expansion of industrial production. The results of process optimization showed that dipropylamine was used as catalyst for Ding Ji phenol, n-octylmercaptan, and dipropylamine was used as catalyst. The molar ratio of paraformaldehyde is 1: 1: 2, the amount of dipropylamine is 10% of the total mass of reactants, and the solvent of potassium bicarbonate (DMF), which accounts for 1.5% of the total mass of reactants, is added to the reflux reaction at 110 鈩,
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