CN110743526A - 一种煤油共炼残渣资源化利用工艺 - Google Patents
一种煤油共炼残渣资源化利用工艺 Download PDFInfo
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Abstract
本发明公开了一种煤油共炼残渣资源化利用工艺,该工艺利用化学活化法,将煤油共炼残渣与活化剂通过预处理(残渣与活化剂研磨混合)、炭化、活化、洗涤等步骤制备不同比表面积、不同孔径的残渣基载体,进一步进行改性处理,负载煤油共炼催化剂活性组分,作为煤油共炼催化剂进行循环使用。此工艺具有设备投资低、简单可行的优点,工业化应用前景广阔。
Description
技术领域
本发明属于环境保护和残渣资源化利用技术领域,具体涉及一种煤油共炼残渣资源化再利用工艺。
背景技术
煤与重油共炼(煤油共炼)技术是用石油重油、渣油等重质烃代替经典的溶剂油,将煤和渣油按一定比例混合,在一定压力、温度及催化剂存在下,在加氢反应装置中同时加氢裂解成轻、中质油和少量烃类气体,其实质是以劣质重油作为煤直接液化的供氢溶剂。煤与重油共炼技术的优点是把原本在煤浆制备中需要加入的循环溶剂,用一部分渣油取代,使油品的循环量较小,处理量可以变大。煤的芳香类和重油的石蜡类之间的协同效应,使得煤油共处理时生成的油不需加氢改质工艺,容易加工成为合格的汽油、柴油等油品。由于渣油中的氢元素比煤的氢元素含量高,在煤油共炼时,氢气耗量降低,氢利用率大幅度提高,有利于减少能耗,降低设备的投资。与煤的直接液化一样,煤与重油共炼技术的研究是洁净煤技术项目研究中的一个主要组成部分,该技术具有投资少、能效高等优势,既合理利用石油重油资源,也实现了煤炭清洁利用及重劣质油轻质化。
近年来,煤与重油共炼技术作为煤炭清洁高效转化的有效方式已引起国内外的高度重视,但煤煤油共炼过程中产生的副产物——高含固煤油共炼残渣,因富集了煤灰、催化剂及高沸点碳氢化合物,属于有害、有毒的废渣,易造成环境污染和资源浪费。煤油共炼残渣常用的处理方法有燃烧法、填埋法、溶剂萃取法、焦化法等,但普遍存在处理成本高、设备投资大、操作繁琐、回收利用率低、经济性差等不足,难以推广应用。
根据煤油共炼残渣灰分含量低、富碳、硫和氮等杂质少等特点,结合煤油共炼催化剂的组成以及煤油共炼催化剂的作用机制,依据“以废治废”的资源化可循环利用理念,本发明提出一种煤油共炼残渣资源化利用的工艺。
发明内容
本发明针对目前煤油共炼残渣的现状,提供一种简单的煤油共炼残渣资源化利用工艺。
解决上述技术问题采用的技术方案包括下述步骤:
1、将煤油共炼残渣与活化剂混合均匀后,在惰性气体保护下炭化后,升温活化,所得产物酸洗后水洗至中性,过滤干燥,得到残渣基载体。
2、以步骤1得到的残渣基载体负载煤油共炼催化剂活性组分,制备煤油共炼催化剂。
上述步骤1中,所述活化剂为KOH,优选所述煤油共炼残渣与活化剂的质量比为1:0.5~2。
上述步骤1中,优选炭化的温度为500~600℃,时间为1~2小时。
上述步骤1中,优选活化的温度为850~950℃,时间为1~4小时。
上述步骤1中,优选步骤1中,优选所得产物用稀盐酸洗涤后,水洗至中性。
上述步骤2中,所述催化剂活性组分为α-FeOOH,催化剂的具体制备方法为:将FeSO4·7H2O固体粉末溶于水中,向其中加入残渣基载体,鼓泡,加入氨水控制溶液的pH值为6~7,搅拌反应2~12小时,过滤、干燥,得到残渣基载体负载α-FeOOH催化剂,即煤油共炼催化剂;以催化剂的质量为100%计,α-FeOOH的负载量为5%~15%。
本发明的有益效果如下:
本发明通过预处理、碳化、活化、洗涤等步骤,制备大表面积、大孔径的残渣基载体,负载煤油共炼催化剂活性组分,作为煤油共炼催化剂进行循环使用,实现了煤油共炼残渣“以废治废”的资源化可循环利用。本发明工艺过程所需设备简单、投资少,工业化应用前景广阔。
具体实施方式
下面结合实施例对本发明进一步详细说明,但本发明的保护范围不仅限于这些实施例。
实施例1
1、将3g煤油共炼残渣、6g KOH混合球磨均匀后,在N2保护下于管式炉中550℃炭化1.5h,然后升温至900℃活化2h;所得产物用质量浓度为8%的盐酸洗涤后,用去离子水洗涤至中性,过滤干燥,得到比表面积为2458.75m2/g、平均孔径为0.6nm的微孔型残渣基载体。
2、将3g FeSO4·7H2O固体粉末溶于75mL水中,向其中加入5.6g残渣基载体,同时用导管将空气通入到液面下方使其不断鼓泡;然后加入质量浓度为2%的氨水控制溶液pH值至6.5,搅拌12h后,过滤、干燥,得到残渣基载体负载α-FeOOH催化剂,其中α-FeOOH的负载量为10%。
实施例2
1、将3g煤油共炼残渣、3g KOH混合球磨均匀后,在N2保护下于管式炉中550℃碳化1.5h,然后升温至900℃活化2h;所得产物用质量浓度为8%的盐酸洗涤后,用去离子水洗涤至中性,过滤干燥,得到比表面积为1735.1m2/g、平均孔径为0.6nm的微孔型残渣基载体。
2、采用步骤1的残渣基载体,按照实施例1的步骤2制备残渣基载体负载α-FeOOH催化剂。
实施例3
1、将6g煤油共炼残渣、3g KOH混合球磨均匀后,在N2保护下于管式炉中550℃碳化1.5h,然后升温至900℃活化2h;所得产物用质量浓度为8%的盐酸洗涤后,用去离子水洗涤至中性,过滤干燥,得到比表面积为500.35m2/g、平均孔径为0.6nm的微孔型残渣基载体。
2、采用步骤1的残渣基载体,按照实施例1的步骤2制备残渣基载体负载α-FeOOH催化剂。
对比例
将6g煤油共炼残渣直接在N2保护下于管式炉中550℃碳化1.5h,然后升温至900℃活化2h,得到残渣基载体。经低温N2吸附测定,其比表面积仅为2.08m2/g,而实施例1~3中经过KOH活化热解处理之后,比表面积有了大幅度的提高,为后续残渣基载体的应用奠定了良好的基础。
为了明确残渣基载体负载煤油共炼催化剂活性组分的重复使用性能,采用长庆FCC油浆(240g)、陕北横山魏强煤矿(60g)为原料,在1.8L高温高压反应釜反应,以实施例3制备的残渣基载体负载α-FeOOH催化剂(加入量为煤和油浆总质量的1%),硫化剂,机械搅拌,455℃下反应1h,氢气初压为9MPa。试验结果显示,煤转化率63.08%、沥青质转化率35.55%、液体收率75.28%。
Claims (9)
1.一种煤油共炼残渣资源化利用工艺,其特征在于包括以下步骤:
(1)将煤油共炼残渣与活化剂混合均匀后,在惰性气体保护下炭化后,升温活化,所得产物酸洗后水洗至中性,过滤干燥,得到残渣基载体;
(2)以步骤(1)得到的残渣基载体,负载煤油共炼催化剂活性组分,制备煤油共炼催化剂。
2.根据权利要求1所述的煤油共炼残渣资源化利用工艺,其特征在于:步骤(1)中,所述活化剂为KOH。
3.根据权利要求2所述的煤油共炼残渣资源化利用工艺,其特征在于:所述煤油共炼残渣与活化剂的质量比为1:0.5~2。
4.根据权利要求1所述的煤油共炼残渣资源化利用工艺,其特征在于:步骤(1)中,所述炭化的温度为500~600℃,时间为1~2小时。
5.根据权利要求1所述的煤油共炼残渣资源化利用工艺,其特征在于:步骤(1)中,所述活化的温度为850~950℃,时间为1~4小时。
6.根据权利要求1所述的煤油共炼残渣资源化利用工艺,其特征在于:步骤(1)中,所得产物用稀盐酸洗涤后,水洗至中性。
7.根据权利要求1所述的煤油共炼残渣资源化利用工艺,其特征在于:步骤(2)中,所述催化剂活性组分为α-FeOOH。
8.根据权利要求7所述的煤油共炼残渣资源化利用工艺,其特征在于:步骤(2)中,将FeSO4·7H2O固体粉末溶于水中,向其中加入残渣基载体,鼓泡,加入氨水控制溶液的pH值为6~7,搅拌反应2~12小时,过滤、干燥,得到残渣基载体负载α-FeOOH催化剂,即煤油共炼催化剂。
9.根据权利要求7或8所述的煤油共炼残渣资源化利用工艺,其特征在于:以催化剂的质量为100%计,α-FeOOH的负载量为5%~15%。
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