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用煤沥青和造纸黑液中的木质素制备电磁屏蔽材料的中试研究

Pilot-scale Study on Produce to Electromagnetic Shielding with Coal Tar Pitch and Lignin from Paper-making Black Liquor

【作者】 陈飞飞

【导师】 王光辉;

【作者基本信息】 武汉科技大学 , 化工工艺, 2005, 硕士

【摘要】 本中试试验采用造纸废液中的木质素和中温煤沥青为原料,通过添加适量镍、钙催化剂催化碳化制备电磁屏蔽材料,并用XRD、SEM等检测手段对碳化产物进行表征。造纸废液经酸析、除硅后得到木质素,并对此木质素用FT-IR、TG进行表征,后在木质素中添加不同含量镍、钙催化剂并进行催化碳化。实验表明:在Ni8wt%、Ca6wt%、碳化温度为900℃的实验条件下木质素可以生成具有完善层状结构的石墨结晶碳。将原煤沥青(CTP)使用四氢呋喃萃取分离得到四氢呋喃可溶物(THFS)和四氢呋喃不溶物(THFI)两部分。并对添加了适量镍、钙催化剂的CTP、THFS、THFI进行催化碳化,得出了THFI、碳化温度、镍、钙催化剂添加量对THFS碳化产物的Lc值、d002值的影响规律。实验结果表明:当钙添加量为1.6wt%时,随着镍添加量的增加,碳化产物中结晶碳的Lc值随之增加; 当保持镍添加量为7wt%增加钙含量,Lc值随之增加,但钙添加量超过1.6wt%时,Lc值反而有所下降; 碳化温度从700℃上升到900℃,碳化产物结晶碳Lc值也趋于增加。由小试实验可知:当碳化产物中结晶碳尺寸(Lc值)达到60 ?以上时制备得到的电磁屏蔽材料的EMS性能就可超过实际应用标准(30dB),故本中试试验预期可得到具有良好电磁屏蔽性能的电磁屏蔽材料。

【Abstract】 In this pilot-scale study, lignin from black liquor of papermaking and medium pitch which used as the raw materials were carbonized to produce electromagnetic shielding material after loading nickel and calcium. The crystal structure of chars was checked with XRD and SEM. Lignin was obtained from black liquor of papermaking by two step process (sulphur dioxide, silica removal), which was analyzed by FT-IR、TG. Then lignin was carbonized by loading various amounts of nickel and calcium. The results revealed that, optimal condition were Ni8wt%, Ca6wt%, 900℃ carbonisation temperature in the pilot-scale study. The coal tar pitch was separated into two fractions (THF-insoluble, THFI; THF-soluble, THFS) by solvent exaction using tatrahydrofuran (THF). The coal tar pitch (CTP) and its two fractions ( THFI and THFS) were carbonized, which reveals that The effects of THFI, carbonization temperature, the amount of nickel, and the type and amount of calcium on the crystallite sizes (Lc) of various chars with nickel and calcium loading. The results showed that Lc for the chars with 1.6wt% calcium increased with increasing amount of nickel loaded; Lc for the chars with an equal loading of 7wt% nickel increased with increasing amount of calcium added and then decreased and that, with an equal co-loading of 7 wt% nickel and 1.6 wt% calcium, also increased with increasing carbonisation temperature, from 700 to 900 ℃. The present study demonstrated that the EMS capacities exceeded a practical standard of EMS capacities when Lc of chars exceeded 60 ?, so the EMS materials with excellent EMS capacities would be obtained.

  • 【分类号】TB34;X793
  • 【下载频次】193
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