石煤提钒工艺研究及关键设备设计
|
摘要
钒是工业生产中的一种重要金属元素,由于它的一些优良的特性,如今得到了愈来愈广泛的应用。钒资源主要存在于石煤中,因此从石煤中提钒成为我国利用钒资源的一个重要发展方向。传统的石煤提钒方法存在钒的回收率较低、浪费资源,有害气体排放量大、严重污染环境的问题,因此研究一种新工艺代替传统工艺,减少污染,提高资源利用率具有重要意义。
本文采用湿法工艺提取石煤中的五氧化二钒,设计正交试验考察了操作压力、硫酸浓度、保温时间对石煤中五氧化二钒浸出率的影响,确定最佳操作条件;以压力容器设计的相关标准和规范为基准,设计了一套石煤提钒的反应装置;在反应器的上方安装安全阀,防止由于压力过大而发生爆炸,设计基于单片机的石煤提钒设备的控制系统。
研究结果表明,硫酸浓度为25%(质量浓度),液固比为0.8:1(体积比),在1.5MPa的饱和水蒸汽压力环境下保温2.5h,钒的浸出率在78%左右。反应器的设计压力为1.7MPa,设计温度为205℃,反应器的主要壁厚为9mm,材料为16MnR;反应器的温度控制系统反应灵敏、控制稳定。该工艺不产生有害气体和烟尘,钒的回收率高,反应装置和温度控制系统运行情况良好,为该工艺的工业化提供了理论基础。
Vanadium is an important metal of industry. With these excellent characteristics, vanadium has been used extensively. In China, Vanadium resource mainly exists in stone coal. It's an very important development direction to extract vanadium in stone coal. The traditional methods emit a large quantity of harmful gases, serious pollution of the environment, while vanadium recovery rate of less. Reseach a new technology to replace the traditional process, improve the utilization rate of resources and reduce pollution is of great significance.
Vanadium pentoxide was leached from stone coal with H_2SO_4 and FeSO_4, inthis paper. The orthogonal experiment have been designed to investigate the effect of processing pressure, sulfuric acid concentration and hold time to leaching rate of vanadium pentoxide, selecting the optimal condition. Referring to the pressure vessel relevant standards and norms as a benchmark, a set of stone coal extracting vanadium installation was designed. The safety valve is installed on the top of reactor which can prevent explosion of reek. The system of temperature detecting uses the single board microcomputer.
The results show that the mass ratio of 25% of H_2SO_4, the ratio of liquid-solid is 0.8:1 and keeping saturation reek press in 1.5MPa for 2.5 hours, vanadium leaching rate is 70%. The design pressure is 1.7MPa. The design temperature is 205℃. The pressure vessel of the main wall thickness is 9mm. The process has advantages of less harmful gases, high leaching ratio. A set of installation and control system has been designed, creating a good condition to industrialization.
本文采用湿法工艺提取石煤中的五氧化二钒,设计正交试验考察了操作压力、硫酸浓度、保温时间对石煤中五氧化二钒浸出率的影响,确定最佳操作条件;以压力容器设计的相关标准和规范为基准,设计了一套石煤提钒的反应装置;在反应器的上方安装安全阀,防止由于压力过大而发生爆炸,设计基于单片机的石煤提钒设备的控制系统。
研究结果表明,硫酸浓度为25%(质量浓度),液固比为0.8:1(体积比),在1.5MPa的饱和水蒸汽压力环境下保温2.5h,钒的浸出率在78%左右。反应器的设计压力为1.7MPa,设计温度为205℃,反应器的主要壁厚为9mm,材料为16MnR;反应器的温度控制系统反应灵敏、控制稳定。该工艺不产生有害气体和烟尘,钒的回收率高,反应装置和温度控制系统运行情况良好,为该工艺的工业化提供了理论基础。
Vanadium is an important metal of industry. With these excellent characteristics, vanadium has been used extensively. In China, Vanadium resource mainly exists in stone coal. It's an very important development direction to extract vanadium in stone coal. The traditional methods emit a large quantity of harmful gases, serious pollution of the environment, while vanadium recovery rate of less. Reseach a new technology to replace the traditional process, improve the utilization rate of resources and reduce pollution is of great significance.
Vanadium pentoxide was leached from stone coal with H_2SO_4 and FeSO_4, inthis paper. The orthogonal experiment have been designed to investigate the effect of processing pressure, sulfuric acid concentration and hold time to leaching rate of vanadium pentoxide, selecting the optimal condition. Referring to the pressure vessel relevant standards and norms as a benchmark, a set of stone coal extracting vanadium installation was designed. The safety valve is installed on the top of reactor which can prevent explosion of reek. The system of temperature detecting uses the single board microcomputer.
The results show that the mass ratio of 25% of H_2SO_4, the ratio of liquid-solid is 0.8:1 and keeping saturation reek press in 1.5MPa for 2.5 hours, vanadium leaching rate is 70%. The design pressure is 1.7MPa. The design temperature is 205℃. The pressure vessel of the main wall thickness is 9mm. The process has advantages of less harmful gases, high leaching ratio. A set of installation and control system has been designed, creating a good condition to industrialization.
引文
1.陈鉴,何晋秋,林京,李国良,符迈群.钒及钒冶金[M].攀枝花资源综合利用领导小组办公室,1983,2-3
2.马胜芳.粘土钒矿提钒新工艺研究及钒催化剂的制备与评价.[硕士学位论文],武汉:武汉理工大学,2007
3.郑祥明.石煤提钒新工艺研究.[硕士学位论文],湖南:湘潭大学,2003
4.漆明鉴.从石煤中提钒现状及前景[J].湿法冶金,1999,72(4):1-10
5.董建华,杨芝兰,冯冀燕.石煤钒矿提精五氧化二钒的研究.西安冶金建筑学院学报,1993,
6.蔡晋强.石煤提钒在湖南的发展[J].稀有金属与硬质合金,2001,(01)
7.席歆,姚谦,胡克俊.国外含钒石油渣提钒生产技术现状[J].有色金属,2001,(5):30-40
8.朱保仓.高碳石煤提钒新工艺研究.[硕士学位论文],西安:西安建筑科技大学,2007
9.邴桔.从石煤中提取五氧化二钒的工艺研究.[硕士学位论文],湖南:中南大学,2007
10.杨雨浓.国外钒生产及钒资源再生处理技术[J].稀有金属与硬质合金,1989,(99):49-52
11.中国科技情报所重庆分所二室冶金组.国外钒钛工业及钒钛磁铁矿的利用情况[J].国外钒钛,1980,(08):3-4
12.马士强,刘世森.石煤提钒工艺评述[J].湖南有色金属,1998,14(04):21-24
13.宾智勇.石煤提钒研究进展与五氧化二钒的市场状况[J].湖南有色金属,2006,22(1):16-20
14.李静,李朝建,吴雪文,仲晓玲,王海华,刘素琴,黄可龙.石煤提钒焙烧工艺及机理探讨[J].湖南有色金属,2007,23(6):7-10
15.向小艳,王明玉,肖连生,高泽斌.石煤酸浸提钒工艺研究[J].稀有金属与硬质合金,2007,35(3):10-13
16.张萍,蒋馥华.苛化泥为焙烧添加剂从石煤提取五氧化二钒[J].稀有金属,2000
17.李晓健.酸浸-萃取工艺在石煤提钒工业中的设计与应用[J].湖南有色金属,2000,16(3):21-23 五氧化二钒的方法[P].CN200610031913.5
19.潘勇,于吉顺,吴红丹.石煤提钒的工艺评价[J].矿业快报,2007,456(4):10-13
20.彭声谦,侯兰杰,刘福生,蔡世明.四川广旺石煤提钒焙烧过程中钒价态的变化[J].中国矿业,1999,8(1):69-72
21.林海玲,范必威,庾化龙,张云.石煤中影响钒转浸率的主要因素研究[J].成都理工学院学报,1999,26(3):317-320
22.梁建龙,刘惠娟,史文革,胡鄂明,李熙琪,彭军.湿法冶金提钒浸出新工艺[J].中国矿业,2006,15(7):64-66
23.李静,李朝建,吴雪文,仲晓玲,王海华,刘素琴,黄可龙.石煤提钒焙烧工艺及机理探讨[J].湖南有色金属,2007,23(6):7-10
24.张辉.利用正交试验确定钒渣焙烧的最佳工艺条件[J].无机盐工业,2003,35(3):29-31
25.韩露.山西典型煤种制备超级活性炭的正交试验研究.[硕士学位论文],山西:太原理工大学,2008
26.王万中.试验的设计与分析[M].北京:高等教育出版社,2004
27.苏均和.试验设计[M].上海:上海财经大学出版社,2005
28.赵选民.试验设计方法[M].北京:科学出版社,2006
29.压力容器安全技术监督规程[M].国家质量技术监督局,1999
30.郭朋鸥,尹振海,王培铣,赵渊.压力容器技术基础[M].西安:西北大学出版社,1991
31.丁伯民,黄正林.化工设备设计全书-高压容器[M].北京:化学工业出版社2003
32.丁伯民,蔡仁良.压力容器设计原理及工程应用[M].北京:中国石化出版社,1992
33.王心明.工程压力容器设计与计算[M].北京:国防工业出版社,1986
34.郑津洋,董起伍,桑芝富.过程设备设计[M].北京:化学工业出版社,2005
35.杨武.浅谈压力容器的设计[J].湖南农机,2007,(11):170-171
36.侯佐岗,陆楞严.压力容器与传热设备[M].大连:大连理工大学出版社,1994
37.李志义,喻健良,刘志军.过程机械[M].北京:化学工业出版社,2008
38.刘湘秋.常用压力容器手册[M].北京:机械工业出版社,2005
39.董大勤,袁凤隐.压力容器设计手册[M].北京:化学工业出版社,2005
40.王心明.工程压力容器设计及计算[M].国防工业出版社,1986
41.王志文.化工容器设计[M].化学工业出版社,1998
42.Ernest E.Ludwig.化工装置实用工艺设计[M].北京:化学工业出版社,2006
43.徐煜明.单片机原理及接口技术[M].电子工业出版社,2004
44.AT89S52单片机功能特性[EB/OL].http://www.atmel.com,pdfprodoct/DSP/8051architecture/search-AT89S52/AT89S52,2006-2-1
45.陈京培.AT89S52单片机实验系统的开发与应用.[硕士学位论文],无锡:江南大学
46.李敏,孟臣.单片K型热电偶放大与数字转换器MAX6675[J].单片机与嵌入式系统应用,2003,09
47.李希胜,王绍纯.热电偶特性数字线性化新方案[J].仪表技术与传感器,2000,09
48.高瑞丽.基于CAN总线的智能温度变送器.[硕士学位论文],山东:山东科技大学
49.宋龙,田红兵,詹天军.K型热电偶数字转换器MAX6675及其在铝液液位温度测量仪中的应用[J].甘肃科技,2004,06
50.黄燕辉.高温无屑成型摩擦钻孔研究.[硕士学位论文],吉林:吉林大学
51.虞致国,徐健健.MAX6675的原理及应用[J].国外电子元器件,2002,12
52.路明礼,付春仙,陈玉仙.基于K型热电偶变换器MAX6675的巡检式数字温度监控仪[J].洛阳工业高等专科学校学报
53.李平,李亚荣.基于MAX6675的温度控制器设计[J].仪表技术与传感器,2004,07
54.陈慧明,杨灿军,陈鹰.利用MAX6675组建测温网络[J].工业仪表与自动化仪,2004,01
55.张向丰.锅炉的单片机控制系统.[硕士学位论文],山东:山东大学
56.谭浩强.C语言程序设计[M].北京清华大学出版社,1999
57.Dongsheng He,Qiming Feng,Guofan Zhang,Leming Ou,Yiping Lu.An environmentally-friendly technology of vanadium extraction from stone coal[J].Minerals Engineering,2007,20:1184-1186
58.N.Panichev,K.Mandiwana,D.Moema,R.Molatlhegi,P.Ngobeni.Distribution of vanadium species between soil and plants in the vicinity of vanadium mine[J].Journal of Hazardous Materials,2006,A137:649-653
59.Wang Mingyu,Xiang Xiaoyan,Zhang Liping,Xiao Liansheng.Effect of vanadium occurrence state on the choice of extracting vanadium technology from stone coal[J].Rare Metals,2008,27(2):112-115
60.R.R Moskalyk,A.M.Alfantazi.Processing of vanadium:a review[J].Minerals Engineering, 2003,16:793-805
61. Justyna Poledniok, Franciszek Buhl, Speciation of vanadium in soil [J]. Talanta, 2003, 59:1-8
62. R. Navarro, J. Guzman, I. Saucedo, J. Revilla, E. Guibal. Vanadium recovery from oil fly ash by leaching, precipitation and solvent extraction processes [J]. Waste Management, 2007, 27:425-438
63. Sandra Vitolo, Maurizia Seggiani, Sara Filippi, Cristina Brocchini. Recovery of vanadium from heavy oil and Orimulsion fly ashes [J]. Hydrometallurgy, 2000, 57:141-149
2.马胜芳.粘土钒矿提钒新工艺研究及钒催化剂的制备与评价.[硕士学位论文],武汉:武汉理工大学,2007
3.郑祥明.石煤提钒新工艺研究.[硕士学位论文],湖南:湘潭大学,2003
4.漆明鉴.从石煤中提钒现状及前景[J].湿法冶金,1999,72(4):1-10
5.董建华,杨芝兰,冯冀燕.石煤钒矿提精五氧化二钒的研究.西安冶金建筑学院学报,1993,
6.蔡晋强.石煤提钒在湖南的发展[J].稀有金属与硬质合金,2001,(01)
7.席歆,姚谦,胡克俊.国外含钒石油渣提钒生产技术现状[J].有色金属,2001,(5):30-40
8.朱保仓.高碳石煤提钒新工艺研究.[硕士学位论文],西安:西安建筑科技大学,2007
9.邴桔.从石煤中提取五氧化二钒的工艺研究.[硕士学位论文],湖南:中南大学,2007
10.杨雨浓.国外钒生产及钒资源再生处理技术[J].稀有金属与硬质合金,1989,(99):49-52
11.中国科技情报所重庆分所二室冶金组.国外钒钛工业及钒钛磁铁矿的利用情况[J].国外钒钛,1980,(08):3-4
12.马士强,刘世森.石煤提钒工艺评述[J].湖南有色金属,1998,14(04):21-24
13.宾智勇.石煤提钒研究进展与五氧化二钒的市场状况[J].湖南有色金属,2006,22(1):16-20
14.李静,李朝建,吴雪文,仲晓玲,王海华,刘素琴,黄可龙.石煤提钒焙烧工艺及机理探讨[J].湖南有色金属,2007,23(6):7-10
15.向小艳,王明玉,肖连生,高泽斌.石煤酸浸提钒工艺研究[J].稀有金属与硬质合金,2007,35(3):10-13
16.张萍,蒋馥华.苛化泥为焙烧添加剂从石煤提取五氧化二钒[J].稀有金属,2000
17.李晓健.酸浸-萃取工艺在石煤提钒工业中的设计与应用[J].湖南有色金属,2000,16(3):21-23 五氧化二钒的方法[P].CN200610031913.5
19.潘勇,于吉顺,吴红丹.石煤提钒的工艺评价[J].矿业快报,2007,456(4):10-13
20.彭声谦,侯兰杰,刘福生,蔡世明.四川广旺石煤提钒焙烧过程中钒价态的变化[J].中国矿业,1999,8(1):69-72
21.林海玲,范必威,庾化龙,张云.石煤中影响钒转浸率的主要因素研究[J].成都理工学院学报,1999,26(3):317-320
22.梁建龙,刘惠娟,史文革,胡鄂明,李熙琪,彭军.湿法冶金提钒浸出新工艺[J].中国矿业,2006,15(7):64-66
23.李静,李朝建,吴雪文,仲晓玲,王海华,刘素琴,黄可龙.石煤提钒焙烧工艺及机理探讨[J].湖南有色金属,2007,23(6):7-10
24.张辉.利用正交试验确定钒渣焙烧的最佳工艺条件[J].无机盐工业,2003,35(3):29-31
25.韩露.山西典型煤种制备超级活性炭的正交试验研究.[硕士学位论文],山西:太原理工大学,2008
26.王万中.试验的设计与分析[M].北京:高等教育出版社,2004
27.苏均和.试验设计[M].上海:上海财经大学出版社,2005
28.赵选民.试验设计方法[M].北京:科学出版社,2006
29.压力容器安全技术监督规程[M].国家质量技术监督局,1999
30.郭朋鸥,尹振海,王培铣,赵渊.压力容器技术基础[M].西安:西北大学出版社,1991
31.丁伯民,黄正林.化工设备设计全书-高压容器[M].北京:化学工业出版社2003
32.丁伯民,蔡仁良.压力容器设计原理及工程应用[M].北京:中国石化出版社,1992
33.王心明.工程压力容器设计与计算[M].北京:国防工业出版社,1986
34.郑津洋,董起伍,桑芝富.过程设备设计[M].北京:化学工业出版社,2005
35.杨武.浅谈压力容器的设计[J].湖南农机,2007,(11):170-171
36.侯佐岗,陆楞严.压力容器与传热设备[M].大连:大连理工大学出版社,1994
37.李志义,喻健良,刘志军.过程机械[M].北京:化学工业出版社,2008
38.刘湘秋.常用压力容器手册[M].北京:机械工业出版社,2005
39.董大勤,袁凤隐.压力容器设计手册[M].北京:化学工业出版社,2005
40.王心明.工程压力容器设计及计算[M].国防工业出版社,1986
41.王志文.化工容器设计[M].化学工业出版社,1998
42.Ernest E.Ludwig.化工装置实用工艺设计[M].北京:化学工业出版社,2006
43.徐煜明.单片机原理及接口技术[M].电子工业出版社,2004
44.AT89S52单片机功能特性[EB/OL].http://www.atmel.com,pdfprodoct/DSP/8051architecture/search-AT89S52/AT89S52,2006-2-1
45.陈京培.AT89S52单片机实验系统的开发与应用.[硕士学位论文],无锡:江南大学
46.李敏,孟臣.单片K型热电偶放大与数字转换器MAX6675[J].单片机与嵌入式系统应用,2003,09
47.李希胜,王绍纯.热电偶特性数字线性化新方案[J].仪表技术与传感器,2000,09
48.高瑞丽.基于CAN总线的智能温度变送器.[硕士学位论文],山东:山东科技大学
49.宋龙,田红兵,詹天军.K型热电偶数字转换器MAX6675及其在铝液液位温度测量仪中的应用[J].甘肃科技,2004,06
50.黄燕辉.高温无屑成型摩擦钻孔研究.[硕士学位论文],吉林:吉林大学
51.虞致国,徐健健.MAX6675的原理及应用[J].国外电子元器件,2002,12
52.路明礼,付春仙,陈玉仙.基于K型热电偶变换器MAX6675的巡检式数字温度监控仪[J].洛阳工业高等专科学校学报
53.李平,李亚荣.基于MAX6675的温度控制器设计[J].仪表技术与传感器,2004,07
54.陈慧明,杨灿军,陈鹰.利用MAX6675组建测温网络[J].工业仪表与自动化仪,2004,01
55.张向丰.锅炉的单片机控制系统.[硕士学位论文],山东:山东大学
56.谭浩强.C语言程序设计[M].北京清华大学出版社,1999
57.Dongsheng He,Qiming Feng,Guofan Zhang,Leming Ou,Yiping Lu.An environmentally-friendly technology of vanadium extraction from stone coal[J].Minerals Engineering,2007,20:1184-1186
58.N.Panichev,K.Mandiwana,D.Moema,R.Molatlhegi,P.Ngobeni.Distribution of vanadium species between soil and plants in the vicinity of vanadium mine[J].Journal of Hazardous Materials,2006,A137:649-653
59.Wang Mingyu,Xiang Xiaoyan,Zhang Liping,Xiao Liansheng.Effect of vanadium occurrence state on the choice of extracting vanadium technology from stone coal[J].Rare Metals,2008,27(2):112-115
60.R.R Moskalyk,A.M.Alfantazi.Processing of vanadium:a review[J].Minerals Engineering, 2003,16:793-805
61. Justyna Poledniok, Franciszek Buhl, Speciation of vanadium in soil [J]. Talanta, 2003, 59:1-8
62. R. Navarro, J. Guzman, I. Saucedo, J. Revilla, E. Guibal. Vanadium recovery from oil fly ash by leaching, precipitation and solvent extraction processes [J]. Waste Management, 2007, 27:425-438
63. Sandra Vitolo, Maurizia Seggiani, Sara Filippi, Cristina Brocchini. Recovery of vanadium from heavy oil and Orimulsion fly ashes [J]. Hydrometallurgy, 2000, 57:141-149