论文总字数：25252字

摘 要

石油的需求日益增长，水面溢油事故发生的频率日益增加，严重威胁到生态环境，因此急需开发一种廉价、高效的油水分离材料。PUS拥有独特的三维网络状结构，具有比表面积大、来源广和回弹性好等优点，常被用作油水分离材料。但传统表面疏水改性工艺繁琐且制备成本较高。因此本文针对现有吸油材料大多存在制备工艺复杂、成本较高、吸油效率低等缺点，采用浸渍涂覆和溶剂热法来提高PUS的疏水亲油性。

本论文首先综述了聚氨酯基油水分离材料、凹凸棒和氧化石墨烯的各项性质。实验部分首先以1mol/L的盐酸作为处理剂，对凹凸棒进行预处理，根据同组实验结论，球磨6 h的凹凸棒的分散效果最好，后续实验选择这一样品进行。通过Hummers法制备GO。根据已有实验结论醇水比为1：1、水热温度为90℃的条件下，GO的还原效果和在PUS上的包覆完善度最好，因此选用上述实验条件并利用溶剂热法制备出超疏水的ATP/RGO包覆PUS的多孔材料。应用扫描电镜、接触角测量、红外光谱分析、紫外光谱分析、拉曼光谱分析、力学性能测试等多种方法对多孔材料进行分析表征，研究了ATP：GO的比例对多孔材料改性效果、吸油性能的影响。结果表明:使用溶剂热法成功的制备出了包覆层良好的超疏水型凹凸棒/二维材料/聚氨酯多孔材料，GO:ATP=1:10条件下制备的多孔材料的接触角最高，为141.5°；其包覆层的完善度也是最高的。在吸油实验中，改性后的多孔材料表现出疏水亲油性、以及优异的吸油能力和循环使用能力。GO:ATP=1:10条件下制备的多孔材料对柴油的饱和吸油率达到了43.2g/g，但其对不同油品吸附能力并不相同，对粘度和密度较大的植物油的吸附能力最好，饱和吸油率达到了46.9g/g；对粘度和密度较小的正己烷的吸附能力最差，只有27.7g/g。多孔材料的ATP/RGO包覆层非常稳定，即使循环50次之后，依然能保持良好的吸油能力。海绵材料的机械强度会随着压缩-解压缩次数的增加而减小，受此影响多孔材料在经历50次循环压缩应力应变实验后，在压缩方向上收缩约5%。但总体来说多孔材料在50次压缩循环应力应变实验后，依然可以维持较高的力学强度，展现出优异的可循环使用能力。在文章的最后对实验结果进行了总结，展望了今后油水分离材料和凹凸棒的研究方向和潜在领域。

关键词：凹凸棒 氧化石墨烯 聚氨酯 多孔吸油材料 吸附 吸油性能

Preparation and oil absorption properties of attapulgite/two-dimensional material/polyurethane porous material

Abstract

The increasing demand for oil and the increasing frequency of surface oil spills are a serious threat to the ecological environment. Therefore, it is urgent to develop an inexpensive and efficient oil-water separation material. PUS has a unique three-dimensional network structure, which has the advantages of large specific surface area, wide source and good resilience. It is often used as oil-water separation material. However, the conventional surface hydrophobic modification process is cumbersome and the preparation cost is high. Therefore, most of the existing oil-absorbing materials have the disadvantages of complicated preparation process, high cost and low oil absorption efficiency. The dip coating and solvothermal methods are used to improve the hydrophobic and lipophilicity of PUS.

This paper first reviews the properties of polyurethane-based oil-water separation materials, attapulgite and graphene oxide. In the experimental part, the attapulgite was pretreated with 1 mol/L hydrochloric acid as the treatment agent. According to the conclusions of the same group, the astigmatism of the ball milling for 6 h was the best. The sample was selected in the subsequent experiments. GO was prepared by the Hummers method. According to the existing experimental conclusions, the reduction ratio of GO and the coating perfection on PUS are the best under the conditions of 1:1 water temperature and water temperature of 90 °C. Therefore, the above experimental conditions are selected and prepared by solvothermal method. Superhydrophobic ATP/RGO coated PUS porous material. Scanning electron microscopy, contact angle measurement, infrared spectroscopy, ultraviolet spectroscopy, Raman spectroscopy, mechanical properties testing and other methods were used to analyze and characterize porous materials. The effect of ATP:GO on the modification of porous materials and oil absorption were studied. The impact of performance. The results show that the superhydrophobic attapulgite/two-dimensional material/polyurethane porous material with good coating is successfully prepared by solvothermal method. The contact angle of porous material prepared under the condition of GO:ATP=1:10 is the highest. 141.5°; the finish of the coating is also the highest. In the oil absorption test, the modified porous material exhibits hydrophobic and lipophilic properties, as well as excellent oil absorption capacity and recycling ability. GO: The saturated oil absorption rate of the porous material prepared by ATP=1:10 reached 43.2g/g, but its adsorption capacity to different oils was not the same, and the adsorption capacity of vegetable oil with higher viscosity and density was the most. Well, the saturated oil absorption rate reached 46.9 g/g; the adsorption capacity for n-hexane with lower viscosity and density was the worst, only 27.7 g/g. The ATP/RGO coating of the porous material is very stable and maintains good oil absorption even after 50 cycles. The mechanical strength of the sponge material decreases as the number of compression-decompression increases, and as a result, the porous material shrinks by about 5% in the compression direction after undergoing 50 cycles of compressive stress strain experiments. However, in general, porous materials can maintain high mechanical strength after 50 cycles of stress and strain tests, showing excellent recyclability. At the end of the paper, the experimental results are summarized, and the research directions and potential fields of oil-water separation materials and attapulgite are prospected.

Key Words: Attapulgite; graphene oxide; polyurethane; porous oil absorbing material; adsorption oil; absorption performance

目录

摘要 I

Abstract III

第一章 绪论 1

1.1 前言 1

1.2 聚氨酯基油水分离材料 1

1.2.1 油水分离材料 1

1.2.2 聚氨酯泡沫 1

1.3 凹凸棒 2

1.3.1 凹凸棒的结构 2

1.3.2 凹凸棒的预处理 3

1.3.3 凹凸棒的吸附性及应用 4

1.4 氧化石墨烯 4

1.5 课题的提出及主要研究内容 5

1.5.1 课题的提出 5

1.5.2 主要研究内容 6

第二章 实验部分 7

2.1 实验原料及设备 7

2.2 凹凸棒/二维材料/聚氨酯多孔材料的制备 8

2.2.1 氧化石墨烯的制备 8

2.2.2 凹凸棒的预处理 9

2.2.3 凹凸棒/二维材料/聚氨酯多孔材料的制备 10

2.3 测试与表征 10

2.3.1 傅里叶变换红外光谱(FTIR) 10

2.3.2 拉曼光谱（Raman） 11

2.3.3 扫描电子显微镜(SEM) 11

2.3.4 接触角(WCA) 11

2.3.5 万能试验机 11

2.3.6 紫外-可见光光度计 11

2.3.7 吸油性能 12

第三章 结果与讨论 13

3.1 凹凸棒的预处理 13

3.1.1 预处理前后凹凸棒的红外光谱 13

3.1.2 预处理前后凹凸棒的SEM照片 14

3.2 凹凸棒/二维材料/聚氨酯多孔材料 14

3.2.1 多孔材料的SEM照片 14

3.2.2 多孔材料的接触角 15

3.2.3 合成多孔材料过程中未包覆的ATP、RGO的红外光谱和紫外光谱 16

3.2.4 多孔材料的红外光谱 17

3.2.5 凹凸棒/二维材料/聚氨酯多孔材料的拉曼光谱 18

3.3 吸油性能 19

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