常压稀硝酸自循环氧化氰化提金工艺试验研究
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摘要
本论文通过对云南镇沅老王寨金矿的提金工艺现状进行分析研究后，在近半年的时间内反复摸索、试验，最终确立了硝酸预氧化—脱硫—氰化工艺。试验在NITROX法和ARSENO法的基础上，通过改进氧化装置和采用不同的脱硫试剂，减少了硝酸的用量，提高了硝酸的利用率。同时验证了不同的脱硫试剂在该工艺中的不同影响。试剂A的脱硫效果虽然不如试剂B，但试剂A的特性使它可以通过改变操作方式实现边氧化边脱硫，而试剂B虽然只能对氧化后的矿渣进行脱硫，但脱硫效果彻底，进而更能提高氰化浸出率，对于象老王寨这样的金精矿来说，浸出率每提高一个百分点都意味着效益的增加。两种试剂都具有操作简便、可以重复使用的特点。整个试验所完成的一些具体工作如下：
1、对老王寨金矿的提金工艺现状进行了综述，分析了当前所存在的问题。即传统的焙烧法产生了大量的烟气，收尘压力大，工艺中还增加了细磨、碱洗工艺，工艺复杂。固硫焙烧法则产生了水溶性的硫酸钙，不利于氰化浸出。生物氧化法虽然具有浸出率高和环境友好的优点，但存在氧化时间过长、初期投资高、操作不易控制的缺点。均不是老王寨金矿理想的提金工艺。
2、本论文根据老王寨金精矿的物相分析了难浸的原因，在对传统的硫化矿预氧化提金工艺进行了了解后，以硝酸氧化法的理论为指导，确定了硝酸预氧化—脱硫—氰化工艺。该工艺改进了原有的氧化装置，设计了新体系，通过反应液中的NO2气体直接转化为硝酸以及使用液膜吸收过剩的NO2气体，实现了硝酸在反应器内的循环使用。
3，由于工艺中生成的硫在金的表面形成了二次包裹，导致金的浸出率不高，ARSENO法和NITROX法曾采用了高温中添加石灰石溶解氧化渣中硫的方法，但这样使得流程复杂化，并存在有经济问题，因此本试验在经过分析后，进行了两种试剂对氧化渣脱硫效果的研究，发现了脱硫渣的氰化提金率随脱硫率的不同而改变，脱硫效果佳，则氰化提金率高，反之亦如此。
4、通过两试剂对比试验，分析了不同的试剂适用的提金工艺。并受试剂A脱硫结果的启发，为阳极氧化—脱硫氰化提金工艺提供了一种新的思路。
This thesis passes to the analysis research of extracting gold mine craft of laowangzhai of zhenyuan in Yunnan in the present condition proceeds, and again and again groping and experiment in the half a year, finally establish the craft of the nitric acid pre- Oxidizing ?desulfuration ?cyaniding. Basing on NITROX method and ARSENO method, experiment pass to improve on the device of oxidation and to adopt the different reagent of desulfuration, reduced the dosage of nitric acid, and increase the nitric acid's utilization, at the same time verified different influence of different reagent of desulfuration in the craft. Although result of desulfuration of reagent AN is not as good as reagent B, characteristic of reagent A make it realize to oxidize and to desulfate at the same time through changing the method of operation. Although reagent B only can desulfate for oxidized scoria, the effect of desulfuration is obvious, which can more increase the rate of cyaniding and lixiviating. For laowangzhai gold concentrate, improvement of one percentage point of rate of lixiviating predicates enhance of benefit. Two reagents all have characteristics of simple operation and repeating usage. The accomplished concrete work of whole experiment is following.
1 The thesis summarized the present condition of craft of extracting of laowangzhai, and analyzed the current existed problem. The traditional baking method produced large quantity's smoke, whose pressure of accepting dust is big. The craft still increased craft of fine grinding and alkali washing, which is complicacy. The fixed sulphur baking produce the water-soluble sulfuric acid calcium, which make against the cyaniding lixiviation. Although bio-oxidization method has advantages of high rate of lixiviation and amity environment, it exists disadvantage of long time of oxidization, the high early investment and not easily controlling operation. All is not ideal craft of extracting gold of laowangzhai.
2 The thesis analyzed the reason of the difficult lixiviation according to material photograph of laowangzhai gold concentrate and after understanding traditional extracting gold craft of sulfuration mineral pre-oxidation, it fixed on the craft of the nitric acid pre- Oxidizing ?desulfuration ?cyaniding guided by the theory of the method of nitric acid pre- oxidation. That craft improved on intrinsic equipment of oxidation, designed the new system and realized circular usage of nitric acid in the reactor passing the direct conversion of N02 in the liquid of reaction to nitric acid and the liquid film to absorb the excess' s N02.
3 Because the sulphur produced in craft forms twice package at gold surface, it cause low rate of lixiviation. The ARSENO method with NITROX method once adopted the method of dissolving sulfur in oxidation sediment by adding limestone the under high temperature. But this makes the flow
complicate and have economic problem, therefore the experiment carries through research of desulfurization effect of oxidation sediment about two reagents after analysis. And discover the change of rate of cyaniding extracting gold of desulfurization sediment following the different rate of desulfurization. The effect of desulfurization is good, so the rate of cyaniding extracting gold is high , vice versa .
4 Through contrasting experiment between two reagents, I analyze the different reagents to adapt different craft of extracting gold. And enlightened by the result of desulfurization of reagent A, I offer a new thinking for anode oxidization- desulfurization cyaniding craft of extracting gold.
1、对老王寨金矿的提金工艺现状进行了综述，分析了当前所存在的问题。即传统的焙烧法产生了大量的烟气，收尘压力大，工艺中还增加了细磨、碱洗工艺，工艺复杂。固硫焙烧法则产生了水溶性的硫酸钙，不利于氰化浸出。生物氧化法虽然具有浸出率高和环境友好的优点，但存在氧化时间过长、初期投资高、操作不易控制的缺点。均不是老王寨金矿理想的提金工艺。
2、本论文根据老王寨金精矿的物相分析了难浸的原因，在对传统的硫化矿预氧化提金工艺进行了了解后，以硝酸氧化法的理论为指导，确定了硝酸预氧化—脱硫—氰化工艺。该工艺改进了原有的氧化装置，设计了新体系，通过反应液中的NO2气体直接转化为硝酸以及使用液膜吸收过剩的NO2气体，实现了硝酸在反应器内的循环使用。
3，由于工艺中生成的硫在金的表面形成了二次包裹，导致金的浸出率不高，ARSENO法和NITROX法曾采用了高温中添加石灰石溶解氧化渣中硫的方法，但这样使得流程复杂化，并存在有经济问题，因此本试验在经过分析后，进行了两种试剂对氧化渣脱硫效果的研究，发现了脱硫渣的氰化提金率随脱硫率的不同而改变，脱硫效果佳，则氰化提金率高，反之亦如此。
4、通过两试剂对比试验，分析了不同的试剂适用的提金工艺。并受试剂A脱硫结果的启发，为阳极氧化—脱硫氰化提金工艺提供了一种新的思路。
This thesis passes to the analysis research of extracting gold mine craft of laowangzhai of zhenyuan in Yunnan in the present condition proceeds, and again and again groping and experiment in the half a year, finally establish the craft of the nitric acid pre- Oxidizing ?desulfuration ?cyaniding. Basing on NITROX method and ARSENO method, experiment pass to improve on the device of oxidation and to adopt the different reagent of desulfuration, reduced the dosage of nitric acid, and increase the nitric acid's utilization, at the same time verified different influence of different reagent of desulfuration in the craft. Although result of desulfuration of reagent AN is not as good as reagent B, characteristic of reagent A make it realize to oxidize and to desulfate at the same time through changing the method of operation. Although reagent B only can desulfate for oxidized scoria, the effect of desulfuration is obvious, which can more increase the rate of cyaniding and lixiviating. For laowangzhai gold concentrate, improvement of one percentage point of rate of lixiviating predicates enhance of benefit. Two reagents all have characteristics of simple operation and repeating usage. The accomplished concrete work of whole experiment is following.
1 The thesis summarized the present condition of craft of extracting of laowangzhai, and analyzed the current existed problem. The traditional baking method produced large quantity's smoke, whose pressure of accepting dust is big. The craft still increased craft of fine grinding and alkali washing, which is complicacy. The fixed sulphur baking produce the water-soluble sulfuric acid calcium, which make against the cyaniding lixiviation. Although bio-oxidization method has advantages of high rate of lixiviation and amity environment, it exists disadvantage of long time of oxidization, the high early investment and not easily controlling operation. All is not ideal craft of extracting gold of laowangzhai.
2 The thesis analyzed the reason of the difficult lixiviation according to material photograph of laowangzhai gold concentrate and after understanding traditional extracting gold craft of sulfuration mineral pre-oxidation, it fixed on the craft of the nitric acid pre- Oxidizing ?desulfuration ?cyaniding guided by the theory of the method of nitric acid pre- oxidation. That craft improved on intrinsic equipment of oxidation, designed the new system and realized circular usage of nitric acid in the reactor passing the direct conversion of N02 in the liquid of reaction to nitric acid and the liquid film to absorb the excess' s N02.
3 Because the sulphur produced in craft forms twice package at gold surface, it cause low rate of lixiviation. The ARSENO method with NITROX method once adopted the method of dissolving sulfur in oxidation sediment by adding limestone the under high temperature. But this makes the flow
complicate and have economic problem, therefore the experiment carries through research of desulfurization effect of oxidation sediment about two reagents after analysis. And discover the change of rate of cyaniding extracting gold of desulfurization sediment following the different rate of desulfurization. The effect of desulfurization is good, so the rate of cyaniding extracting gold is high , vice versa .
4 Through contrasting experiment between two reagents, I analyze the different reagents to adapt different craft of extracting gold. And enlightened by the result of desulfurization of reagent A, I offer a new thinking for anode oxidization- desulfurization cyaniding craft of extracting gold.
引文
[1] 中国科学院黄金科技工作领导小组办公室。中国金矿研究新发展第三卷[M]。北京：冶金工业出版社，1996，9
[2] 聂树人，索有瑞。难选冶金矿石浸金[M]。北京：地质出版社，1997，8
[3] 郭长阁。含砷难浸金矿的处理综述[J]。国外金属矿选矿，1995，3：40—41
[4] 郭长阁。含金硫化矿氧化预处理综述[J]。国外金属矿选矿，1996，3：38—40
[5] 王力军，刘春谦。难处理金矿石预处理技术综述[J]。黄金，2000(1)：38—45
[6] G. P. Demopoulos, etc, "Recent advances in refractory gold processing," CIM Bulletin [J]. vol. 82, NO. 931, 1989, 85—91
[7] D. Robert. Weir. etc, "Refractory gold: the role of pressure oxidation," The proceedings of Gold 100[J], sec, vo 275—286
[8] Lane white, "Treating of refractory gold ores," Mining Engineering[J]. 1990, NO. 2 168—174
[9] N.C. Wall etc "Gold Beneficent,"Mining Magazine[J]. May 1987, 393—401
[10] 姜涛。提金化学[M]。湖南科学技术出版社，1998，8
[11] 黄金生产工艺指南编委会。黄金生产工艺指南[M]。北京：地质出版社，2000，1
[12] 黄礼煌。金银提取技术(第二版)[M]。北京：冶金工业出版社，2000，8
[13] H. L. Ehrlich, "Recent advances in microbial processing[J]., May 1988, 58-60
[14] S. R. Hutchins etc., "Microbial pretreatment ores," The 116th Annual AIME Meeting [M]
[15] Richard W. Lawrence etc, "Biological Pre-oxidation of a pyrite gold concentrate," [M]. in Frontier Technology in Mineral processing
[16] H.R. Lawrence etc, "Biological pre-oxidation to enhance gold and Concentrate, "CIM Bulletin[J]. 76, 875, 107-110, 1983
[17] 彭担任。难浸金矿石预处理评述[J]。国外金属矿选矿，1994(11)：40—41
[18] 姜涛，胡熙庚。关于难选金矿石的处理[J]。黄金，199l(5)：26—31
[19] 陶元杰。黄金。1987，N0．3，41—47
[20] 董智虞等译“某些金矿难以氰化的原因及其处理途径，”[J]。矿产综合利用，1998，NO．2，85-93
[21] H. Von. Michaeis, "Innovation in gold and silver recovery" [J]. The
proceedings of 14th international symposium on mineral processing, 1982, 10
[22] J. B. Hiskey, "Thiourea Leaching of Gold and Silver-Technology update and Additional Application" [J]. Minerals and Metallurgical processing, Vol, 1, November 1981, 173-179
[23] R.G. Schulze, "New Aspects in Thiourea Leaching of Precious Metal" [J]. Journal of Metal. Vol. 36, NO. 6 June 1984, 62-65
[24] G. Deschenes, "Leaching of Gold from Chalcopyrite Concentrate by Thiourea" [J]. Hydro-metallurgy, 20(1998)179-202
[25] D. Zipperian etc., "Gold and Silver Extraction by Ammoniacal Thiosulfate Leaching from a Rhyolite ore" [J]. Hydro-metallurgy, 19(1988)361-375
[26] J. B. Hiskey etc., "Dissolution chemistry of Gold and Silver in Different Lixiviants" [J]. Mineral Processing and Extractive Metallurgy Review, 1988, Vol. 4, 95-134
[27] 王康林。难处理金矿石的细菌氧化预处理研究现状[J]。黄金科学技术，2001，(1)：19-24
[28] 张培科。老王寨金矿提金工艺研究[M]。未发表，2002，3
[29] 邓日章，赵天从，钟竹前等。从含硫浸出渣中回收元素硫的研究[J]。中南矿冶学院学报，1992(3)：287～291
[30] 昆明冶金研究院。含砷高硫金精矿焙烧—氰化工艺研究[J]。云南冶金，1999(8)：30-36
[31] 王文潜等。难浸金矿预处理方法评价及新进展[J]。云南冶金，1997(12)：30-34
[32] 海光宝。镇沅金矿固硫焙烧焙砂多硫化物浸出工艺研究[J]。云南冶金，2000(4)：37-39
[33] 童雄等。镇沅浮选金精矿细菌氧化—硫脲浸金的实验研究[J]。国外金属矿选矿，1998，4：37-38
[34] 余忠清等。云南镇沅县载金黄铁矿的生物氧化—氰化浸金研究[J]。昆明理工大学学报，1992，5：18-22
[35] Xia Guan xiang etc. Trans. Noferrous Metals soc china, 1995, 5(2):43
[36] Wei Xiao na and Xia Guang xiang. Trans. Noferrous Metals soc. China, 1993, 3(3): 12
[37] 《化工百科全科全书》编辑委员会。化工百科全书(第10卷)[M]。北京：化学工业出版社，1996
[38] Moeller. T. Inorganic Chemistry (A modern Introduetion), wiley, 1982
[39] 程能林。溶剂手册(第二版)[M]。北京：化学工业出版社，1994，9
[40] 熊大民。高砷金矿预先脱砷及反续工艺试验研究[J]。未发表，2001，3
[41] 朱述民等。有色金属(季刊)，1989，41(1)：61—63
[42] 全宏东。矿物化学处理[M]。北京：冶金工业出版社，1984，6。
[43] 孙晋戈。金银冶金[M]。北京：冶金工业出版社，1985
[44] 黎鼎鑫主编。贵金属提取与精炼[M]。北京：冶金工业出版社，1991
[45] 田广荣等译。金的提取冶金[M]。北京：冶金工业出版社，1992
[46] 邱定藩。矿浆电解[M]。北京：冶金工业出版社，1999，1
[47] 陈寿椿，唐春元等。重要无机化学反应(第三版)[M]。上海：上海科学技术出版社，1994
[48] Chanturiga V A. Electrochemical liberation of refractory gold ore minerals. Gorn Zh. 1997, (10)51～55
[49] 薛传东。镇沅老王寨金矿床的围岩蚀变特征[J]。昆明理工大学学报，1997(4)：1～6．
[2] 聂树人，索有瑞。难选冶金矿石浸金[M]。北京：地质出版社，1997，8
[3] 郭长阁。含砷难浸金矿的处理综述[J]。国外金属矿选矿，1995，3：40—41
[4] 郭长阁。含金硫化矿氧化预处理综述[J]。国外金属矿选矿，1996，3：38—40
[5] 王力军，刘春谦。难处理金矿石预处理技术综述[J]。黄金，2000(1)：38—45
[6] G. P. Demopoulos, etc, "Recent advances in refractory gold processing," CIM Bulletin [J]. vol. 82, NO. 931, 1989, 85—91
[7] D. Robert. Weir. etc, "Refractory gold: the role of pressure oxidation," The proceedings of Gold 100[J], sec, vo 275—286
[8] Lane white, "Treating of refractory gold ores," Mining Engineering[J]. 1990, NO. 2 168—174
[9] N.C. Wall etc "Gold Beneficent,"Mining Magazine[J]. May 1987, 393—401
[10] 姜涛。提金化学[M]。湖南科学技术出版社，1998，8
[11] 黄金生产工艺指南编委会。黄金生产工艺指南[M]。北京：地质出版社，2000，1
[12] 黄礼煌。金银提取技术(第二版)[M]。北京：冶金工业出版社，2000，8
[13] H. L. Ehrlich, "Recent advances in microbial processing[J]., May 1988, 58-60
[14] S. R. Hutchins etc., "Microbial pretreatment ores," The 116th Annual AIME Meeting [M]
[15] Richard W. Lawrence etc, "Biological Pre-oxidation of a pyrite gold concentrate," [M]. in Frontier Technology in Mineral processing
[16] H.R. Lawrence etc, "Biological pre-oxidation to enhance gold and Concentrate, "CIM Bulletin[J]. 76, 875, 107-110, 1983
[17] 彭担任。难浸金矿石预处理评述[J]。国外金属矿选矿，1994(11)：40—41
[18] 姜涛，胡熙庚。关于难选金矿石的处理[J]。黄金，199l(5)：26—31
[19] 陶元杰。黄金。1987，N0．3，41—47
[20] 董智虞等译“某些金矿难以氰化的原因及其处理途径，”[J]。矿产综合利用，1998，NO．2，85-93
[21] H. Von. Michaeis, "Innovation in gold and silver recovery" [J]. The
proceedings of 14th international symposium on mineral processing, 1982, 10
[22] J. B. Hiskey, "Thiourea Leaching of Gold and Silver-Technology update and Additional Application" [J]. Minerals and Metallurgical processing, Vol, 1, November 1981, 173-179
[23] R.G. Schulze, "New Aspects in Thiourea Leaching of Precious Metal" [J]. Journal of Metal. Vol. 36, NO. 6 June 1984, 62-65
[24] G. Deschenes, "Leaching of Gold from Chalcopyrite Concentrate by Thiourea" [J]. Hydro-metallurgy, 20(1998)179-202
[25] D. Zipperian etc., "Gold and Silver Extraction by Ammoniacal Thiosulfate Leaching from a Rhyolite ore" [J]. Hydro-metallurgy, 19(1988)361-375
[26] J. B. Hiskey etc., "Dissolution chemistry of Gold and Silver in Different Lixiviants" [J]. Mineral Processing and Extractive Metallurgy Review, 1988, Vol. 4, 95-134
[27] 王康林。难处理金矿石的细菌氧化预处理研究现状[J]。黄金科学技术，2001，(1)：19-24
[28] 张培科。老王寨金矿提金工艺研究[M]。未发表，2002，3
[29] 邓日章，赵天从，钟竹前等。从含硫浸出渣中回收元素硫的研究[J]。中南矿冶学院学报，1992(3)：287～291
[30] 昆明冶金研究院。含砷高硫金精矿焙烧—氰化工艺研究[J]。云南冶金，1999(8)：30-36
[31] 王文潜等。难浸金矿预处理方法评价及新进展[J]。云南冶金，1997(12)：30-34
[32] 海光宝。镇沅金矿固硫焙烧焙砂多硫化物浸出工艺研究[J]。云南冶金，2000(4)：37-39
[33] 童雄等。镇沅浮选金精矿细菌氧化—硫脲浸金的实验研究[J]。国外金属矿选矿，1998，4：37-38
[34] 余忠清等。云南镇沅县载金黄铁矿的生物氧化—氰化浸金研究[J]。昆明理工大学学报，1992，5：18-22
[35] Xia Guan xiang etc. Trans. Noferrous Metals soc china, 1995, 5(2):43
[36] Wei Xiao na and Xia Guang xiang. Trans. Noferrous Metals soc. China, 1993, 3(3): 12
[37] 《化工百科全科全书》编辑委员会。化工百科全书(第10卷)[M]。北京：化学工业出版社，1996
[38] Moeller. T. Inorganic Chemistry (A modern Introduetion), wiley, 1982
[39] 程能林。溶剂手册(第二版)[M]。北京：化学工业出版社，1994，9
[40] 熊大民。高砷金矿预先脱砷及反续工艺试验研究[J]。未发表，2001，3
[41] 朱述民等。有色金属(季刊)，1989，41(1)：61—63
[42] 全宏东。矿物化学处理[M]。北京：冶金工业出版社，1984，6。
[43] 孙晋戈。金银冶金[M]。北京：冶金工业出版社，1985
[44] 黎鼎鑫主编。贵金属提取与精炼[M]。北京：冶金工业出版社，1991
[45] 田广荣等译。金的提取冶金[M]。北京：冶金工业出版社，1992
[46] 邱定藩。矿浆电解[M]。北京：冶金工业出版社，1999，1
[47] 陈寿椿，唐春元等。重要无机化学反应(第三版)[M]。上海：上海科学技术出版社，1994
[48] Chanturiga V A. Electrochemical liberation of refractory gold ore minerals. Gorn Zh. 1997, (10)51～55
[49] 薛传东。镇沅老王寨金矿床的围岩蚀变特征[J]。昆明理工大学学报，1997(4)：1～6．
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