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改性云母的制備及在聚丙烯中的應用

發(fā)布時間:2018-06-02 19:12

  本文選題:云母 + 聚丙烯 ; 參考:《河北大學》2017年碩士論文


【摘要】:云母(Mica)具有徑厚比高、抗壓、抗拉強度大,作為無機填充劑應用在高聚物中,能改善高聚物的機械強度。然而云母的表面極性大,與高聚物的相容性差,易團聚且分散不均勻,因此就需要對云母的表面進行改性,以提高云母與高聚物的相容性。本文主要以KH550/石蠟(KP)和KH550/癸二酸(KS)為復合改性劑,分別采用濕法(W)與干法(D)技術改性云母,然后將改性云母與聚丙烯(PP)共混,探討了改性云母對PP復合材料力學性能的影響,并用錫酸鋅(ZS)包覆云母,得到云母基阻燃劑,以進一步拓展云母的應用范圍。具體內容如下:第一部分:采用濕法技術改性云母,制備了W-KP和W-KS兩種改性云母,研究了改性劑用量和改性時間對云母的影響,采用SEM、FTIR和接觸角儀對改性云母進行表征。研究表明:改性后,云母的親油性和分散性顯著提高,其中W-KP的改善效果最佳。當改性劑用量為7%,改性時間為120 min時,W-KP的沉降值由未改性云母的2 mL提高到9.5 mL,接觸角由0°提高到20.1°,吸油值由1.7 mL/g降低到1.05 mL/g。將改性前后的云母與PP共混制得PP復合材料,主要分析了PP復合材料的力學性能。發(fā)現與未改性PP/Mica復合材料相比,改性PP/W-KP和PP/W-KS復合材料的力學性能得到有效改善,其中PP/W-KP的改善效果最佳。PP/W-KP的斷裂伸長率比PP/Mica提高了23.4%,拉伸強度提高了13.4%,缺口沖擊強度提高了12.5%,熔融指數提高到9.9g/10min,且收縮率最小降低到1.23%。第二部分:采用干法技術改性云母,制備了D-KP和D-KS兩種改性云母,分析了改性劑用量和研磨時間對云母的影響,通過SEM、FTIR、接觸角儀和激光粒度儀對改性云母進行表征。結果表明:改性后,云母的親油性和分散性得到明顯改善,云母的層狀結構保持良好,粒徑有輕微的變化,其中D-KS的綜合改善效果最好。當改性劑用量為7%,研磨時間為15 min時,D-KS的沉降值由未改性云母的2 mL提高到17.5 mL,接觸角由0°提高到51.3°,吸油值由1.7 mL/g降低到0.85 mL/g。將改性前后的云母與PP共混制得PP復合材料并分析了其力學性能。發(fā)現與未改性PP/Mica復合材料相比,PP/D-KP和PP/D-KS復合材料的力學性能得到明顯改善,其中PP/D-KP的改善效果最佳。PP/D-KP的斷裂伸長率比PP/Mica提高了14.9%,拉伸強度提高了13.2%,缺口沖擊強度提高了27.8%,熔融指數提高到6.6 g/10min,且收縮率最小降低到1.20%。對比兩種改性效果可以得知,干法所得改性云母的沉降值、吸油值和力學性能優(yōu)于濕法,但可能會影響云母的粒徑大小,破壞材料的結構,而濕法改性云母的熱穩(wěn)定性好。第三部分:通過共沉淀法制備了錫酸鋅包覆云母(ZS/Mica),然后用KP和KS改性表面得到云母基阻燃劑,采用XRD、FTIR和SEM-EDS對產物進行表征,之后將云母基阻燃劑應用在PP中制得PP阻燃材料,通過LOI、UL-94、TG、DTG、Cone研究了PP阻燃材料的阻燃性能、熱穩(wěn)定性能和力學性能。研究表明:ZS可包覆在云母表面上,云母基阻燃劑的加入有助于改善PP阻燃材料的阻燃性能、燃燒性能、熱穩(wěn)定性能和力學性能。當云母基阻燃劑添加量為Sb2O3的50%時,PP阻燃材料的垂直燃燒等級保持不變,氧指數提高到24.3%,且PP阻燃材料的熱釋放總量、熱釋放速率、煙釋放總量和CO2釋放速率均有改善,初始熱分解溫度、殘余質量和Tmax略有增加,Rmax降低。且PP阻燃材料的力學性能也得到明顯改善,其中經過KP改性PP阻燃材料的力學性能最佳,其斷裂伸長率最大提高到583%,拉伸強度提高到37.2 MPa,缺口沖擊強度提高到14.2 kJ/m~2,彎曲強度提高到48.3 MPa。
[Abstract]:Mica (Mica) has high diameter thickness ratio, high compressive strength and tensile strength. As an inorganic filler used in polymer, it can improve the mechanical strength of polymer. However, the surface of mica has large surface polarity and poor compatibility with polymers. It is easy to be reunited and disperse unevenly. Therefore, the surface of mica needs to be modified to improve the phase of mica and polymer. In this paper, KH550/ paraffin (KP) and KH550/ sebacic acid (KS) were used as compound modifiers. Wet method (W) and dry method (D) were used to modify mica. Then the modified mica was blended with polypropylene (PP), and the effect of modified mica on the mechanical properties of PP composite was investigated. The mica was coated with zinc stannate (ZS), and the mica flame retardant was obtained. The application scope of mica is expanded step by step. The specific contents are as follows: in the first part, two kinds of modified mica, W-KP and W-KS are prepared by wet technique, and the effect of modifier dosage and modification time on mica is studied. SEM, FTIR and contact angle meter are used to characterize the modified mica. When the dosage of the modifier is 7% and the modification time is 120 min, the settlement value of W-KP is increased from 2 mL to 9.5 mL, the contact angle is increased from 0 degrees to 20.1 degrees, the oil absorption value is reduced from 1.7 mL/g to 1.05 mL/g., and the mixture of mica and PP before and after modification is analyzed, the main analysis is the main analysis. It is found that the mechanical properties of the modified PP/W-KP and PP/W-KS composites are improved effectively compared with the unmodified PP/Mica composites. The best improvement effect of PP/W-KP is 23.4%, the tensile strength is increased by 23.4%, the tensile strength is increased by 13.4%, the impact strength of the notch is increased by 12.5%, and the melting finger is improved. The number was increased to 9.9g/10min, and the minimum shrinkage rate was reduced to 1.23%. second. Two modified mica was prepared by dry technique, D-KP and D-KS were prepared. The effect of the modifier dosage and grinding time on mica was analyzed. The modified mica was characterized by SEM, FTIR, contact angle meter and laser particle size analyzer. The results showed that after modification, mica was modified. The hydrophobicity and dispersity of the mica have been improved obviously. The layer structure of mica is good and the particle size has a slight change. The comprehensive improvement effect of D-KS is the best. When the dosage of the modifier is 7% and the grinding time is 15 min, the settlement value of the D-KS is raised from 2 mL to 17.5 mL by the unmodified mica, the contact angle is increased from 0 to 51.3, and the oil absorption value is 1.7 mL/g. It is reduced to 0.85 mL/g. to blend the mica and PP before and after the modification to obtain the PP composite and analyze its mechanical properties. It is found that the mechanical properties of PP/D-KP and PP/D-KS composites are obviously improved compared with the unmodified PP/Mica composites, and the best improvement effect of PP/D-KP is 14.9% higher than that of PP/Mica, which is better than that of PP/Mica. The tensile strength increased by 13.2%, the notch impact strength increased by 27.8%, the melting index increased to 6.6 g/10min, and the minimum shrinkage rate was reduced to the 1.20%. contrast effect. It was found that the sedimentation value, the oil absorption value and the mechanical properties of the modified mica obtained by dry method are better than the wet method, but it may affect the size of the mica and destroy the structure of the material. The thermal stability of wet modified mica is good. Third part: Zinc Stannate Coated mica (ZS/Mica) was prepared by coprecipitation method. Then the mica based flame retardant was obtained by KP and KS modified surface. XRD, FTIR and SEM-EDS were used to characterize the products. Then the mica based flame retardant was used in PP to produce PP flame retardant, and it was studied through LOI, UL-94, TG, DTG, and DTG. The flame retardancy, thermal stability and mechanical properties of the PP flame retardant materials are investigated. The study shows that ZS can be coated on the mica surface, and the addition of mica based flame retardant helps to improve the flame retardancy, combustion, thermal stability and mechanical properties of the PP flame retardant. When the addition of mica based flame retardant is 50% of Sb2O3, the vertical of PP flame retardant material The oxygen index increased to 24.3%, and the total amount of heat release, the heat release rate, the total amount of smoke release and the release rate of CO2 were improved, the initial thermal decomposition temperature, the residual mass and the Tmax increased slightly, and the Rmax decreased, and the mechanical energy of the PP flame retardant material was also improved obviously, in which the KP modified PP flame retardant material was improved. The mechanical properties of the material are the best, the maximum elongation at break increases to 583%, the tensile strength increases to 37.2 MPa, the notch impact strength increases to 14.2 kJ/m~2, and the bending strength increases to 48.3 MPa..
【學位授予單位】:河北大學
【學位級別】:碩士
【學位授予年份】:2017
【分類號】:TQ325.14;TB332

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