吸附脱除四氯化碳中氯代异丁腈杂质技术研究

发布时间：2018-06-06 06:55

本文选题：氯代异丁腈 + 分子筛　；参考：《浙江工业大学》2017年硕士论文

【摘要】：宁化公司原料四氯化碳总量约3.5万吨/年,其中含有氯代异丁腈杂质约1-3%。在公司现有产业链布局中,要将甲烷氯化物装置中副产四氯化碳必须全部转化为四氯乙烯产品,造成四氯乙烯产品中三氯丙烯腈的含量约为0.5-1%左右。四氯乙烯产品中存在三氯丙烯腈杂质对用四氯乙烯生产制冷剂HCF125装置的反应催化剂Cr2O3影响非常大,当含量超过15 ppm时能造成催化剂中毒,并不可逆。因此HCF125厂商要求此种杂质在四氯乙烯产品中的含量小于15 ppm。考虑到从原料四氯化碳分离杂质氯代异丁腈比从产品四氯乙烯中去除三氯丙烯腈杂质更容易,因此开发研究出高效、对环境友好的氯代异丁腈脱除技术具有很大社会与经济效益。比较分析现有氯代异丁腈脱除方法存在的弊端,本文提出利用吸附法脱除四氯化碳中氯代异丁腈杂质。通过考察不同类型的吸附剂对原料四氯化碳中腈类杂质的吸附性能,筛选出具有高选择性、高吸附容量吸附分离氯代异丁腈杂质的吸附剂,并对吸附剂的吸附工艺条件进行了优化。8#分子筛类吸附剂是一种对氯代异丁腈杂质具有良好吸附脱除效果的吸附剂,当吸附温度为60℃和90℃时,均可将原料四氯化碳中的氯代异丁腈脱除至检测限以下,且四氯化碳的纯度明显提高。随着吸附温度与四氯化碳进料空速的提高,8#分子筛类吸附剂对氯代异丁腈的吸附脱除效果减弱。8#分子筛类吸附剂的再生过程中,第二阶段再生温度控制在260-280℃左右,其再生性能最佳;且空气对吸附剂再生性能优于氮气。8#分子筛类吸附剂不管经历多少次吸附与脱附,都能基本恢复其原有的良好吸附脱除性能。经过50次累积实验,每克8#分子筛类吸附剂可以累积处理504克四氯化碳,累积吸附8.62克氯代异丁腈。总之,8#分子筛类吸附剂对氯代异丁腈吸附脱除具有良好效果,在工业上可以多次、重复使用。
[Abstract]:The total amount of carbon tetrachloride in Ninghua company is about 35 thousand tons per year, with chloroisobutadiene nitrile impurities containing about 1-3%. in the existing industrial chain layout of the company. The by-product of carbon tetrachloride in the methane chloride device must be converted to four chloroethylene products, and the content of three chloroacrylonitrile in four chloroethylene products is about 0.5-1%. Four chloroethylene The presence of three chloroacrylonitrile impurities in the product has a great influence on the reaction catalyst Cr2O3 for the HCF125 unit with four vinyl chloride production. When the content exceeds 15 ppm, the catalyst is intoxication and is not reversible. Therefore, the HCF125 manufacturer requires that the content of this impurity in the four chloroethylene product is less than 15 ppm., considering the carbon tetrachloride from raw material. The impurity chloroisobutyl nitrile is easier to remove from the four chloroacrylonitrile from the product of the product of chloroacrylonitrile from the product. Therefore, it has great social and economic benefits for the development and study of the environmentally friendly chloroisobutadiene removal technology. The disadvantages of existing chloroisobutyl nitrile removal methods are compared and analyzed. The removal of four chlorination by adsorption method is proposed in this paper. The adsorption properties of nitrile impurities in carbon tetrachloride were investigated by different types of adsorbents. The adsorbents with high selectivity and high adsorption capacity for separation of chloro isobutyl nitrile were screened, and the adsorption process conditions of the adsorbents were optimized by.8# molecular sieve sorbent as a kind of pair of chlorinated agents. Isobutadiene nitrile impurities have good adsorption and removal effect. When the adsorption temperature is 60 and 90, the chloroisobutadiene nitrile in carbon tetrachloride can be removed to the detection limit, and the purity of carbon tetrachloride is obviously improved. With the increase of the adsorption temperature and the air speed of the carbon tetrachloride feed, the 8# molecular sieve adsorbents to chloroisobutadiene nitrile. In the process of regeneration of.8# molecular sieve adsorbents, the second stage regeneration temperature was controlled at about 260-280, and the regeneration performance of the adsorbent was best, and the regeneration performance of air to adsorbents was better than that of nitrogen.8# molecular sieve adsorbents. No matter how many sorbents were experienced and desorption, the good adsorption and removal of adsorbents could be recovered. After 50 cumulative experiments, each 8# molecular sieve adsorbent can accumulate 504 grams of carbon tetrachloride and accumulate 8.62 grams of chloroisobutyl nitrile. In a word, 8# molecular sieve adsorbents have good effect on the adsorption and removal of chloroisobutadiene, and can be repeated and reused in industry.
【学位授予单位】：浙江工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O647.3;TQ222.423

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