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Article(id=1240631880559686622, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631872800215183, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2025.01.019, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1722441600000, receivedDateStr=2024-08-01, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773719290151, onlineDateStr=2026-03-17, pubDate=1738339200000, pubDateStr=2025-02-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773719290151, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773719290151, creator=13701087609, updateTime=1773719290151, updator=13701087609, issue=Issue{id=1240631872800215183, tenantId=1146029695717560320, journalId=1235980550691926019, year='2025', volume='45', issue='1', pageStart='1', pageEnd='187', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773719288300, creator=13701087609, updateTime=1773724138257, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1240652215052989235, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631872800215183, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1240652215052989236, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631872800215183, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=103, endPage=108, ext={EN=ArticleExt(id=1240631881541153777, articleId=1240631880559686622, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Thermodynamic and Kinetic Analysis for Phase Transition of Vanadium Slag by Calcified Roasting, columnId=1236276106727321817, journalTitle=Mining and Metallurgical Engineering, columnName=METALLURGY, runingTitle=null, highlight=null, articleAbstract=

Vanadium slag, as raw material, went through calcified roasting processes in the study, and the thermodynamics and kinetic analysis were conducted for verifying the roasting mechanism. The results show that calcified roasting process mainly includes iron oxidation, oxidative decomposition of olivine and spinel, as well as calcification. Based on theoretical and data analysis, calcium-containing phases are formed in the following sequence: CaV2O6, Ca2V2O7, Ca3V2O8, CaSiO3. At a high temperature, excess CaO reacts with vanadium to generate Ca3V2O8 and CaSiO3. The oxidation and calcification processes of vanadium spinel are controlled by a third-order reaction, and the apparent activation energy is 282.45 kJ/mol. In the leaching experiment, the leaching rate reaches the maximum after roasting at 860 ℃ for 120 min, which is consistent with the results obtained from theoretical analysis of calcified roasting process.

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对钒渣原料及钙化焙烧过程进行研究，并采用反应热力学和动力学对其焙烧机理进行理论论证。结果表明：钙化焙烧主要包括铁氧化、橄榄石氧化分解、尖晶石氧化分解及钙化反应；经理论和数据分析，含钙相的形成顺序依次为CaV2O6、Ca2V2O7、Ca3V2O8、CaSiO3。高温情况下，过量的CaO会与钒反应生成Ca3V2O8、CaSiO3。钒尖晶石的氧化钙化过程受三级反应控制，表观活化能为282.45 kJ/mol。浸出实验中，焙烧温度860 ℃、焙烧时间120 min所得焙烧渣的钒浸出率较高，与钙化焙烧理论分析结果一致。

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贺永东（1965—），男，湖北黄冈人，博士，教授，主要研究方向为有色金属及材料化学。E-mail：
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邵甲骥（1997—），男，安徽宿州人，硕士，主要研究方向为材料与化工。E-mail：

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邵甲骥（1997—），男，安徽宿州人，硕士，主要研究方向为材料与化工。E-mail：

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邵甲骥（1997—），男，安徽宿州人，硕士，主要研究方向为材料与化工。E-mail：

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caption=Microstructure of vanadium slag, figureFileSmall=RfCl5rzOp30qkzD/MH6gDQ==, figureFileBig=rWiukgSNSpu9s/lvB8s1pg==, tableContent=null), ArticleFig(id=1240651373096792840, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=图1, caption=钒渣微观形貌, figureFileSmall=RfCl5rzOp30qkzD/MH6gDQ==, figureFileBig=rWiukgSNSpu9s/lvB8s1pg==, tableContent=null), ArticleFig(id=1240651373205844748, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=EN, label=Fig.2, caption=XRD patterns of vanadium slag before and after roasting at different temperatures, figureFileSmall=51xx4yqgwTKmd5apvv7NrA==, figureFileBig=1nHUXGKv08irV6Rpbcn0fw==, tableContent=null), ArticleFig(id=1240651373302313743, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=图2, caption=钒渣原料及不同焙烧温度下所得焙烧料的XRD图谱, figureFileSmall=51xx4yqgwTKmd5apvv7NrA==, figureFileBig=1nHUXGKv08irV6Rpbcn0fw==, tableContent=null), ArticleFig(id=1240651373373616915, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=EN, label=Fig.3, caption=Infrared spectra of vanadium slag before and after roasting at different temperatures, figureFileSmall=/I+0hrno/uUenXfPOQyiKQ==, figureFileBig=prtInnyC+9zpB4maX0SLzA==, tableContent=null), ArticleFig(id=1240651373444920087, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=图3, caption=钒渣原料及不同焙烧温度下所得焙烧料的红外光谱, figureFileSmall=/I+0hrno/uUenXfPOQyiKQ==, figureFileBig=prtInnyC+9zpB4maX0SLzA==, tableContent=null), ArticleFig(id=1240651373533000475, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=EN, label=Fig.4, caption=Microstructure of vanadium slag before and after roasting at different temperatures, figureFileSmall=z7n3MHIEX6/WLBJ5E0x7ZA==, figureFileBig=xtgbWqSTn+GkPcAZmqGckw==, tableContent=null), ArticleFig(id=1240651373629469472, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=图4, caption=钒渣原料及不同焙烧温度所得焙烧料的微观形貌

（a）钒渣原料；（b）600 ℃焙烧料；（c）800 ℃焙烧料；（d）900 ℃焙烧料

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Main chemical composition of vanadium slag

, figureFileSmall=null, figureFileBig=null, tableContent=
FeVMnSiCaOCrTiAlMg
27.639.246.628.832.3136.702.243.801.141.49
), ArticleFig(id=1240651376422875985, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=表1, caption=

钒渣主要化学成分（质量分数）

, figureFileSmall=null, figureFileBig=null, tableContent=
FeVMnSiCaOCrTiAlMg
27.639.246.628.832.3136.702.243.801.141.49
), ArticleFig(id=1240651376506762067, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=EN, label=Table 2, caption=

Energy spectrum analysis of vanadium slag

, figureFileSmall=null, figureFileBig=null, tableContent=
点OFeSiCaVMnTiAlCrMg
130.1446.9711.881.380.497.700.510.590.070.26
29.9365.660.650.166.582.1010.444.170.290.02
), ArticleFig(id=1240651376624202583, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=表2, caption=

钒渣能谱分析结果（质量分数）

, figureFileSmall=null, figureFileBig=null, tableContent=
点OFeSiCaVMnTiAlCrMg
130.1446.9711.881.380.497.700.510.590.070.26
29.9365.660.650.166.582.1010.444.170.290.02
), ArticleFig(id=1240651376741643097, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=EN, label=Table 3, caption=

EDS analysis results of vanadium slag before and after roasting at different temperatures

, figureFileSmall=null, figureFileBig=null, tableContent=
序号元素（原子分数）/%
OFeSiCaVMnTiAlCrMg
a131.4250.6111.110.370.373.840.420.100.121.65
a226.4923.6925.5111.410.692.331.867.65—0.40
a325.5644.050.260.0610.631.6310.851.310.570.17
b128.5141.520.211.4514.032.308.850.472.560.10
b233.1849.057.131.850.466.950.430.230.120.59
b337.4014.0818.3819.390.292.461.915.950.050.10
c111.7074.770.630.491.104.784.860.390.630.64
c221.5971.350.400.430.512.902.020.260.090.46
c321.6866.380.130.240.474.553.460.372.040.69
d110.1875.680.330.841.504.874.420.301.200.68
d227.5818.631.4518.6326.604.282.310.260.100.36
d325.0059.520.801.481.694.195.440.331.000.54
), ArticleFig(id=1240651376812946268, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=表3, caption=

钒渣原料及不同焙烧温度下所得钒渣EDS分析结果

, figureFileSmall=null, figureFileBig=null, tableContent=
序号元素（原子分数）/%
OFeSiCaVMnTiAlCrMg
a131.4250.6111.110.370.373.840.420.100.121.65
a226.4923.6925.5111.410.692.331.867.65—0.40
a325.5644.050.260.0610.631.6310.851.310.570.17
b128.5141.520.211.4514.032.308.850.472.560.10
b233.1849.057.131.850.466.950.430.230.120.59
b337.4014.0818.3819.390.292.461.915.950.050.10
c111.7074.770.630.491.104.784.860.390.630.64
c221.5971.350.400.430.512.902.020.260.090.46
c321.6866.380.130.240.474.553.460.372.040.69
d110.1875.680.330.841.504.874.420.301.200.68
d227.5818.631.4518.6326.604.282.310.260.100.36
d325.0059.520.801.481.694.195.440.331.000.54
), ArticleFig(id=1240651376884249437, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=EN, label=Table 4, caption=

Main chemical reaction equations of calcified roasting of vanadium slag

, figureFileSmall=null, figureFileBig=null, tableContent=
反应方程式编号
（1）
（2）
（3）
（4）
（5）
（6）
（7）
（8）
（9）
（10）
), ArticleFig(id=1240651376959746910, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=表4, caption=

钒渣钙化焙烧主要化学反应方程式

, figureFileSmall=null, figureFileBig=null, tableContent=
反应方程式编号
（1）
（2）
（3）
（4）
（5）
（6）
（7）
（8）
（9）
（10）
), ArticleFig(id=1240651377039438687, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=EN, label=Table 5, caption=

Linear coefficients R2 corresponding to different reaction orders n

, figureFileSmall=null, figureFileBig=null, tableContent=
反应级数n相关系数R2
10.960
20.983
30.999
), ArticleFig(id=1240651377098158945, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631880559686622, language=CN, label=表5, caption=

不同反应级数对应的线性相关系数R2

, figureFileSmall=null, figureFileBig=null, tableContent=
反应级数n相关系数R2
10.960
20.983
30.999
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钒渣钙化焙烧物相变化及热力学动力学分析
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邵甲骥 1 , 孙小涵 2 , 贺永东 1 , 赵亿坤 3 , 陈守俊 4 , 梁飞龙 5
矿冶工程杂志 | 冶金 2025,45(1): 103-108
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矿冶工程杂志 | 冶金 2025, 45(1): 103-108
钒渣钙化焙烧物相变化及热力学动力学分析
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邵甲骥1 , 孙小涵2, 贺永东1 , 赵亿坤3, 陈守俊4, 梁飞龙5
作者信息
  • 1.新疆大学　材料科学与工程学院，新疆　乌鲁木齐　830046
  • 2.山东能源数字科技有限公司，山东　济南　250000
  • 3.新疆大学　物理科学与技术学院，新疆　乌鲁木齐　830046
  • 4.新疆盛安新材料科技有限公司，新疆　哈密　839000
  • 5.新疆湘润新材料科技有限公司，新疆　哈密　839000

    • 邵甲骥（1997—），男，安徽宿州人，硕士，主要研究方向为材料与化工。E-mail：

通讯作者:

贺永东（1965—），男，湖北黄冈人，博士，教授，主要研究方向为有色金属及材料化学。E-mail：
Thermodynamic and Kinetic Analysis for Phase Transition of Vanadium Slag by Calcified Roasting
Jiaji SHAO1 , Xiaohan SUN2, Yongdong HE1 , Yikun ZHAO3, Shoujun CHEN4, Feilong LIANG5
Affiliations
  • 1.School of Materials Science and Engineering, Xinjiang University, Urumqi 830046, Xinjiang, China
  • 2.Shandong Energy Digital Technology Co., Ltd., Jinan 250000, Shandong, China
  • 3.School of Physical Science and Technology, Xinjiang University, Urumqi 830046, Xinjiang, China
  • 4.Xinjiang Sheng'an New Material Technology Co., Ltd., Hami 839000, Xinjiang, China
  • 5.Xinjiang Xiangrun New Material Technology Co., Ltd., Hami 839000, Xinjiang, China
出版时间: 2025-02-01 doi: 10.3969/j.issn.0253-6099.2025.01.019
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摘要
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对钒渣原料及钙化焙烧过程进行研究，并采用反应热力学和动力学对其焙烧机理进行理论论证。结果表明：钙化焙烧主要包括铁氧化、橄榄石氧化分解、尖晶石氧化分解及钙化反应；经理论和数据分析，含钙相的形成顺序依次为CaV2O6、Ca2V2O7、Ca3V2O8、CaSiO3。高温情况下，过量的CaO会与钒反应生成Ca3V2O8、CaSiO3。钒尖晶石的氧化钙化过程受三级反应控制，表观活化能为282.45 kJ/mol。浸出实验中，焙烧温度860 ℃、焙烧时间120 min所得焙烧渣的钒浸出率较高，与钙化焙烧理论分析结果一致。

钒渣  /  钙化焙烧  /  相变过程  /  热力学  /  动力学  /  提钒

Vanadium slag, as raw material, went through calcified roasting processes in the study, and the thermodynamics and kinetic analysis were conducted for verifying the roasting mechanism. The results show that calcified roasting process mainly includes iron oxidation, oxidative decomposition of olivine and spinel, as well as calcification. Based on theoretical and data analysis, calcium-containing phases are formed in the following sequence: CaV2O6, Ca2V2O7, Ca3V2O8, CaSiO3. At a high temperature, excess CaO reacts with vanadium to generate Ca3V2O8 and CaSiO3. The oxidation and calcification processes of vanadium spinel are controlled by a third-order reaction, and the apparent activation energy is 282.45 kJ/mol. In the leaching experiment, the leaching rate reaches the maximum after roasting at 860 ℃ for 120 min, which is consistent with the results obtained from theoretical analysis of calcified roasting process.

vanadium slag  /  calcified roasting  /  phase transition  /  thermodynamics  /  kinetics  /  vanadium extraction
邵甲骥, 孙小涵, 贺永东, 赵亿坤, 陈守俊, 梁飞龙. 钒渣钙化焙烧物相变化及热力学动力学分析. 矿冶工程杂志, 2025 , 45 (1) : 103 -108 . DOI: 10.3969/j.issn.0253-6099.2025.01.019
Jiaji SHAO, Xiaohan SUN, Yongdong HE, Yikun ZHAO, Shoujun CHEN, Feilong LIANG. Thermodynamic and Kinetic Analysis for Phase Transition of Vanadium Slag by Calcified Roasting[J]. Mining and Metallurgical Engineering, 2025 , 45 (1) : 103 -108 . DOI: 10.3969/j.issn.0253-6099.2025.01.019
正文
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钒作为重要战略性资源，被称为“现代工业味精”，广泛应用于钢铁、化工、航天航空、新能源等领域[1-2]。由钒渣制备V2O5的主要工艺是钠化焙烧[3]和钙化焙烧[4]，近年又出现了亚熔盐焙烧法、加压酸浸法、微波焙烧和微生物法提钒工艺[5-6]。钠化焙烧对原料适用性强、工艺成熟，但存在焙烧过程分解有毒气体污染环境、尾渣综合回收利用难等问题[7]。钙化焙烧具有焙烧过程无污染、焙烧成本低、尾渣利用率高等优势。但钒渣成分随高炉炉料变化而变化，焙烧过程中钒渣的物相结构、组成变化大，工艺过程难以精准控制，且钙化焙烧过程钒渣各物相与钙添加剂的反应产物也会影响钒回收率的进一步提高。本文研究钒渣物相组成及其微观形貌特征，分析不同焙烧温度条件下钒渣的物相变化及微观形貌变化，通过反应热力学和动力学对钒渣钙化焙烧相变机理进行深入研究，并探讨焙烧温度、焙烧时间对后续钒浸出率的影响。
1　实验
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1.1　实验材料
钒渣取自新疆盛安新材料科技有限公司。钒渣原料主要呈块状，通体呈黑色，表面有银亮色金属光泽。其主要化学成分如表1所示，主要含有Fe、O、Si、V、Mn等几种元素。钒渣微观形貌见图1。图1中相区点1为橄榄石相，呈深灰色，相区点2为钒尖晶石相，呈浅灰色，对应的能谱分析结果见表2。能谱分析结果与化学成分分析结果一致。
1.2　实验方案
采用X射线衍射仪（XRD）、扫描电镜（SEM）、红外光谱（IR）、X射线能谱分析仪（EDS）对焙烧前、后钒渣进行物相、微观形貌、矿物微区成分分析。
研磨筛分粒度小于0.075 mm的钒渣，按钙、钒物质的量比2∶1将钒渣与CaO均匀混合；将混料平铺于刚玉坩埚中，置入马弗炉，在空气氛围中以升温速率10 ℃/min进行氧化焙烧。钒冶金过程中因为产能及效益问题，焙烧温度一般不会超过1 000 ℃，因此焙烧温度范围选取400～900 ℃。
根据相应固液比量取去离子水，配制一定浓度碳酸根溶液置于三颈烧瓶中，在恒温水浴锅中加热，达到相应温度后加入焙烧料，搅拌一定时间后停止反应，进行液固分离，检测滤渣中钒元素含量，计算浸出率。
2　结果与讨论
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2.1　不同焙烧温度下焙烧料物相变化
图2为钒渣原料及不同焙烧温度下保温2 h所得焙烧料的XRD图谱。与钒渣原料对比，焙烧温度500 ℃时出现了CrVO3特征峰；焙烧温度400 ℃时钒渣没有发生氧化反应，500 ℃时有钒尖晶石开始参与反应，500 ℃保温2 h的焙烧渣中依然存在Fe2SiO4特征峰，说明橄榄石相并未完全氧化。焙烧温度600 ℃时，Fe2SiO4特征峰消失，出现Fe2O3和SiO2特征峰，说明Fe2SiO4在600 ℃之前发生了氧化分解反应、生成了Fe2O3和SiO2并在600 ℃反应完全。焙烧温度600 ℃时出现了4价钒酸盐（FeV2O4）的特征峰，此后再升温，4价钒酸盐特征峰消失，说明4价钒完全氧化为5价钒。随着温度升高，CaO开始参与反应。焙烧温度700 ℃时，出现了可溶性钒酸盐CaV2O6的特征峰，说明V3+和V4+在空气中氧化为V5+并与Ca2+结合形成5价钒酸盐。焙烧温度800 ℃时，物相无变化。焙烧温度900 ℃时，出现硅酸钙CaSiO3，说明SiO2与CaO在较高温度下才能发生反应。根据钒渣氧化物酸碱性定义，CaO与钒渣中氧化物的结合能力顺序为：V2O5>SiO2。CaO的衍射峰在400～800 ℃一直存在，900 ℃消失，说明CaO一直参与反应，900 ℃反应趋于完全。此外，出现了Ca2V2O7和Ca3V2O8特征峰，CaV2O6特征峰消失，证明在CaO过量情况下CaV2O6会转化为Ca2V2O7、Ca3V2O8，焙烧温度达到900 ℃，钒尖晶石的钙化焙烧氧化产物为Ca2V2O7、Ca3V2O8，但Ca3V2O8不能直接生成，需由CaV2O6、Ca2V2O7与CaO反应而得。
图3为钒渣原料及不同焙烧温度下保温2 h所得焙烧料的红外光谱。图3中，3 653 cm-1处为CaO的特征吸收峰，500 ℃以上时CaO特征峰开始减弱，900 ℃时CaO特征峰消失，这与XRD分析结果一致。
几乎所有的特征吸收带都在红外光谱的指纹区内（400～1300 cm-1）。随着焙烧温度升高，1处（468 cm-1）和2处（564 cm-1）尖晶石中的M—O伸缩吸收峰开始变宽变弱，并逐渐向低频偏移，结合图2可知，这是尖晶石相发生氧化分解所致。橄榄石相[SiO4]四面体的振动峰在3处（874 cm-1）和4处（947 cm-1）存在；随着温度升高，特征峰逐渐变弱且向低频率方向转变，并在600 ℃消失，说明600 ℃之前橄榄石已完全分解，与图2中橄榄石的分解温度一致。900 ℃时V—O消失，表明钒酸钙发生了转变。
2.2　不同焙烧温度下焙烧料形貌变化及元素迁移
图4为钒渣原料及不同焙烧温度下保温2 h所得焙烧料的微观形貌，对应的EDS分析结果见表3。从图4及表3可以确定温度升高对钒渣物相微观形貌及成分变化的影响。钒渣原料渣粒表面光滑致密，点a1和a2为橄榄石相，a3为尖晶石相。焙烧温度600 ℃时，尖晶石周围深灰色区域b3含Si相（18.38%），且整体结构完整，说明硅酸盐相并未完全氧化分解，但该处Ca含量增加，说明CaO开始与钒酸盐反应，结合图2可知，此时尖晶石相已经开始氧化并进行物相重构。焙烧温度升至800 ℃时，渣粒表面出现密集浑圆小颗粒，这些小颗粒充满整个试样，此时钒渣中的含钒尖晶石相及其嵌合硅酸盐相被完全破坏，结合表3可知，粒渣表面小颗粒主要为Fe2O3和Mn2O3的金属氧化物相，此时V质量分数急剧减小，从a3的10.63%降至0.47%，说明含钒尖晶石氧化分解，V元素已经迁移出渣粒内部。焙烧温度升到900 ℃时，焙烧矿微观形貌离散程度更高，结合表3可知，点d2为钒酸钙相，此时钒元素已迁移至渣粒外部并与Ca结合生成钒酸钙相，其V质量分数为26.60%、Ca质量分数为18.63%。这也印证了图2的结果。
图5为900 ℃焙烧渣BSE形貌及元素分布图。由图5可以看出，除了少部分Ca、V留存在渣粒晶间内部，大部分Ca、V元素都不断迁移，呈不规则环状聚集在渣粒外部；其中Si元素呈斑点状分散在渣粒中，与Fe、Ca、V元素相混杂，说明焙烧温度900 ℃时出现了硅酸盐相夹杂钒酸钙中，不利于下一步钒的浸出。
2.3　温度对钒渣物相影响的机理分析
2.3.1　热力学分析
表4为钒渣钙化焙烧主要化学反应方程式，图6为其标准吉布斯自由能变化与温度的关系，图7为理想钙钒二元反应DTA热值曲线图，图8为实验钒渣钙化反应DTA热值曲线图。
由图6可知，在反应温度范围内，除反应（7）外，其他反应ΔG均为负值，说明从热力学角度而言，钙化焙烧各个阶段均可进行。随着温度升高，部分反应吉布斯自由能增加，说明热力学因素不是主要控制因素。反应（1）、（2）、（3）的吉布斯自由能图表明，先是氧化亚铁的氧化，后是铁橄榄石和钒尖晶石的氧化分解。铁橄榄石先分解形成SiO2，分散包覆在尖晶石相周围的铁橄榄石先分解形成SiO2，尖晶石才得以被氧化。700 ℃后，反应生成钒酸钙和硅酸钙的顺序为：Ca2V2O7、CaV2O6、CaSiO3，说明CaO更容易与钒结合生成钒酸钙。700 ℃以下，反应（5）的ΔG比反应（6）和反应（7）的ΔG更负，说明钒酸钙的生成顺序为：CaV2O6、Ca2V2O7、Ca3V2O8。且Ca3V2O8在500 ℃后后ΔG>0，反应无法自发进行，焦钒酸钙只能通过已氧化的钒与过量氧化钙直接反应生成。由图7～8可见，383～384 ℃出现了吸热峰，该吸热峰归因于混合物中吸附的结晶水消失。图7中623和755.5 ℃处共检测到2个尖锐的吸热峰，结合热力学分析可知，这是生成了钒酸钙。图8中671 ℃有一处不明显的波峰，应是生成了钒酸钙。
2.3.2　动力学分析
设计实验升温速度10 ℃/min，从室温到1 000 ℃范围内进行动态升温实验，空气流量200 mL/min，钒渣钙、钒物质的量比2∶1，所得TG曲线如图9所示。
钒渣的氧化钙化过程是一种非等温非均相气固反应。在气固反应中，当反应速率受A物质控制时，反应速率符合方程：
式中：α为反应物在t时刻向产物转化的百分数（表示在非均相体系中反应进展的程度）；n为反应级数；T为开尔文温度；E为表观活化能；R为摩尔气体常数；A为指前因子。对于等速升温条件，升温速率β为常数。
对式（11）两边取对数：
一般来说，，，所以式（12）和（13）右端第一项为常数，用或对作图，可得斜率为的直线。
运用动力学方程对升温速率10 ℃/min的TG数据进行拟合确定反应级数n，结果如表5所示。
由线性相关系数R2可知，本实验条件下钒渣氧化过程受三级化学反应控制，拟合得到表观活化能为282.45 kJ/mol。
2.4　焙烧条件对浸出结果的影响
通过分析焙烧过程中的物相可知，CaV2O6会在800 ℃之前出现，Ca2V2O7和Ca3V2O8在900 ℃生成，不同的焙烧温度会对钒渣的物相变化造成影响，从而影响钒的浸出，其中CaV2O6是理想状态下的实验产物。
浸出实验保持浸出时间120 min、浸出温度90 ℃、Na2CO3浸出剂质量浓度100 g/L、固液比1∶10，对浸出渣中的钒含量进行检测，计算钒浸出率。
2.4.1　焙烧温度对浸出结果的影响
为找到适宜的焙烧温度，提高钒浸出率，在800～900 ℃之间每隔20 ℃设置一个温度节点，焙烧时间2 h，焙烧温度对钒浸出率的影响见图10。由图10可知，800 ℃时钒浸出率低于80%，说明此时可与Na2CO3发生复分解反应的钒酸盐还未反应完全，与XRD分析中800 ℃出现CaV2O6相印证。随着焙烧温度升高，钒浸出率上升，800～860 ℃上升幅度很大，860 ℃时浸出率达到91.5%；860～900 ℃时钒浸出率趋于平稳。结合XRD分析结果可知，800～900 ℃，CaV2O6已反应完全，但温度过高时，CaV2O6会二次反应生成Ca3V2O8及CaSiO3。CaSiO3会形成胶体裹络钒酸盐，使其既不溶于水也不溶于碱。
结合焙烧过程物相变化和浸出率变化分析，焙烧温度860 ℃左右，钙化焙烧渣物相更有利于浸出反应的进行，与钙化焙烧过程物相变化分析结果一致。
2.4.2　焙烧时间对浸出结果的影响
钒渣中各元素的氧化程度取决于焙烧时间的长短，焙烧时间对钒渣氧化焙烧效果有一定影响。将钒渣置于马弗炉中，随炉升温至860 ℃，焙烧时间对钒浸出率的影响见图11。由图11可知，焙烧时间从60 min增至120 min，钒浸出率随之升高，且增幅相对较大。焙烧时间过短，钒渣在高温环境中的驻留时间短，低价钒不能充分氧化成高价钒，即可溶钒酸盐无法反应完全；焙烧时间增至150 min后，钒浸出率基本保持不变，说明120 min时钒已基本氧化完全，继续增加焙烧时间会增大能耗及成本。综合考虑，焙烧时间120 min为宜。
3　结论
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1）钒渣中的钒以尖晶石方式存在，并被橄榄石为主的相包裹，钙化焙烧过程中，600 ℃时橄榄石会氧化分解为Fe2O3和SiO2。600 ℃以上，钒尖晶石分解氧化后与CaO初步结合生成CaV2O6。焙烧温度达到900 ℃，钒尖晶石的钙化焙烧氧化产物为Ca2V2O7、Ca3V2O8。900 ℃时过量的CaO会与SiO2反应生成硅酸钙CaSiO3。
2）热力学分析结果表明，钒酸钙的生成顺序为：CaV2O6、Ca2V2O7、Ca3V2O8。Ca3V2O8生成反应在500 ℃后ΔG>0，反应无法自发进行，Ca3V2O8不能直接生成，需由CaV2O6、Ca2V2O7与CaO反应而来。
3）钙化焙烧过程钒渣中尖晶石氧化钙化受三级反应控制，反应表观活化能为282.45 kJ/mol。
4）焙烧温度860 ℃、焙烧时间120 min时，钒渣钙化焙烧所得物相更有利于浸出反应的进行。
基金
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  • 国家自然科学基金(51861033)
  • 新疆维吾尔自治区科技厅重点研发专项(2020B02007)
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2025年第45卷第1期
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doi: 10.3969/j.issn.0253-6099.2025.01.019
  • 接收时间：2024-08-01
  • 首发时间：2026-03-17
  • 出版时间：2025-02-01
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  • 收稿日期：2024-08-01
基金
国家自然科学基金(51861033)
新疆维吾尔自治区科技厅重点研发专项(2020B02007)
作者信息
    1.新疆大学　材料科学与工程学院，新疆　乌鲁木齐　830046
    2.山东能源数字科技有限公司，山东　济南　250000
    3.新疆大学　物理科学与技术学院，新疆　乌鲁木齐　830046
    4.新疆盛安新材料科技有限公司，新疆　哈密　839000
    5.新疆湘润新材料科技有限公司，新疆　哈密　839000

通讯作者:

贺永东（1965—），男，湖北黄冈人，博士，教授，主要研究方向为有色金属及材料化学。E-mail：
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2种不同金属材料的力学参数
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total species (%)		 属
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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