【摘要】：為了制備出用于膨脹阻燃體系的可膨脹石墨和導(dǎo)電防腐涂料體系的納米石墨薄片,本文研究了以H_2SO_4/H_3PO_4、HClO_4/H_3PO_4兩種混合酸,氧化插層法制備阻燃可膨脹石墨的工藝,探討了制備工藝各因素對可膨脹石墨性能的影響,并通過正交實(shí)驗(yàn)法優(yōu)選了可膨脹石墨的最優(yōu)制備工藝;用HClO_4/H_3PO_4混合酸氧化插層和超聲剝分法研究了導(dǎo)電納米石墨薄片的制備工藝,得出工藝各因素對組織結(jié)構(gòu)與導(dǎo)電性能影響作用。采用掃描電鏡、X-射線衍射、激光粒度儀、原子力顯微鏡技術(shù)對優(yōu)化工藝制備的可膨脹石墨和納米石墨薄片進(jìn)行結(jié)構(gòu)形貌表征。實(shí)驗(yàn)結(jié)果表明:1.以H_2SO_4/H_3PO_4混酸制備的阻燃可膨脹石墨,在反應(yīng)溫度35℃,反應(yīng)時(shí)間60 min,C(g):H_2SO_4(mL):H_3PO_4(mL):K_2Cr_2O_7(g)=1:2:2:0.12的條件下,制備出可膨脹石墨的膨脹容積為223 mL/g。添加5 g的該可膨脹石墨可以使EPS的氧指數(shù)由18%提高到26.3%。2.以HClO_4/H_3PO_4混酸制備的阻燃可膨脹石墨,在反應(yīng)溫度35℃,反應(yīng)時(shí)間80 min,C(g):HClO_4(mL):H_3PO_4(mL):KMnO_4(g)=1:3:2:0.1的條件下,制備出可膨脹石墨的膨脹容積為235 mL/g。添加5 g的該可膨脹石墨可以使EPS的氧指數(shù)由18%提高到22.7%。3.采用微波膨脹法制備膨脹石墨,當(dāng)微波功率350 W,微波時(shí)間15 s時(shí),得到的膨脹容積為360 mL/g。與高溫膨脹法相比,膨脹容積大且孔徑更加密集、均勻。4.納米石墨薄片的最佳剝分條件為:乙醇(g):膨脹石墨(g)=150:1,超聲功率為400 W,超聲時(shí)間為4 h~6 h,得到的納米石墨薄片具有較大的徑厚比,其平均粒度范圍在17μm~10μm之間,厚度范圍在50 nm~150 nm之間。添加到環(huán)氧樹脂E51涂料中,當(dāng)納米石墨薄片的質(zhì)量含量為20%時(shí),涂料的體積電阻率為320Ω·cm。
[Abstract]:In order to prepare expandable graphite for intumescent flame retardant system and nano-graphite sheet for conductive anticorrosive coating system, this paper studied two kinds of mixed acids, H2SO4 / H3PO4 / HClOSP 4. The process of preparing flame retardant and expandable graphite by oxidation intercalation method was discussed. The influence of various factors on the properties of expandable graphite was discussed, and the optimum preparation process of expandable graphite was selected by orthogonal experiment. The preparation process of conductive nano-graphite sheet was studied by HClO_4/H_3PO_4 mixed acid oxidation intercalation and ultrasonic stripping method. Scanning electron microscopy (SEM), X-ray diffraction (XRD), laser particle size analyzer (LGA) and atomic force microscopy (AFM) were used to characterize the structure and morphology of the expandable graphite and nano-graphite wafer prepared by the optimized technology. The experimental results show that: 1. Flame retardant intumescent graphite prepared from H_2SO_4/H_3PO_4 mixed acid at 35 鈩，

本文編號(hào)：2357833