从光棒废料中获取较高吸油值的白炭黑

Obtaining White Carbon Black with Higher Oil Absorption Value from Fiber Preform Waste

吸油值是表征白炭黑结构性的重要参数，之前本研究组通过对光纤预制棒湿废料进行烘干、破碎、研磨、煅烧、酸处理后烘干得到白炭黑，其绝大部分技术参数已基本符合化工标准HGIT3061-2009，但吸油值只有1．10mL／g，远小于标准2．00mL／g。为了提高从光纤预制棒废料中回收的白炭黑的吸油值，本文采用把光棒湿废料进行乙醇浸泡，然后烘干、研磨、煅烧、酸处理、醇浸泡，最后烘干的新工艺路线，研究光棒湿废料的浸泡乙醇溶液浓度、煅烧温度、酸处理并醇洗后进行烘干的温度等因素对吸油值的影响，探索出回收高吸油值白炭黑的工艺条件。实验结果表明：在乙醇溶液浸泡实验中，乙醇的浓度越高越好；煅烧的最佳温度为500℃；较优工艺路线为：先向湿废料中加无水乙醇（固液质量比1：（3-4）），搅拌均匀并浸泡24h，然后把浸泡溶液离心后土黄色固体在110℃下烘干并研磨，再在500℃下煅烧1h，接着用20％的盐酸回流1．5h，离心后水洗、醇洗并用乙醇浸泡（固液质量比1：3）24h，最后离心并于850℃下烘干，吸油值可提高至1．74mL／g。

Oil absorption value is an important parameter for the characterization of the white carbon black structure. The white carbon black was obtained from the optical fiber preform wet waste by drying, smashing, grinding, calcination, acid treatment and drying before. Its most technical parameters were in line with the chemical industry standard HG/T 3061-2009. But the oil absorption value of the sample was only 1. 10 mL/g, far less than the HG/T 3061- 2009 standard of 2. 00 mL/g. In order to enhance the optical fiber preform wet waste was soaked by using the oil absorption value, a new process route was adopted that the ethanol solution firstly, followed by drying, smashing, grinding, calcination, acid treatment, ethanol soaking, and finally the sample was dried. The effect of the ethanol solution concentration for soaking, calcination temperature, drying temperature after acid treatment and alcohol soaking on the oil absorption value was studied, in order to explore the optimized process conditions to get the white carbon black with the higher oil absorption value. The experimental results showed that higher ethanol concentration in the soaking experiment was better, the best calcination temperature was 500 ℃. The good process route was as follows： the wet waste was immersed for 24 h by using absolute alcohol with the solid-liquid mass ratio of 1 ： （3 - 4）, and the solution was centrifuged and the yellow solid was dried at 110 ℃ and grinded, the sample was calcined at 500 ℃ for 1 h and treated by the reflux in 20% hydrochloric acid for 1.5 h, after that the solution was centrifuged and the white solid was washed by water and by absolute ethanol, and soaked for 24 h in the ethanol with the solid-liquid mass ratio 1 ： 3, it was dried after eentrifugation at 850 ℃, the oil absorption value of the product was increased to 1.74 mL/g.