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Article(id=1241321991119098478, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.02.025, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1697731200000, receivedDateStr=2023-10-20, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773883825330, onlineDateStr=2026-03-19, pubDate=1711900800000, pubDateStr=2024-04-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773883825330, onlineIssueDateStr=2026-03-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773883825330, creator=13701087609, updateTime=1773883825330, updator=13701087609, issue=Issue{id=1241321979433767757, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='2', pageStart='1', pageEnd='191', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773883822544, creator=13701087609, updateTime=1773884556149, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241325056454881881, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241325056454881882, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=100, endPage=105, ext={EN=ArticleExt(id=1241321991924404917, articleId=1241321991119098478, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Experimental Study on Preparation of High Purity Sodium Aluminate with Sodium Aluminate Solution, columnId=1236276106727321817, journalTitle=Mining and Metallurgical Engineering, columnName=METALLURGY, runingTitle=null, highlight=null, articleAbstract=

High purity sodium aluminate was prepared with sodium aluminate solution by adopting a process consisting of evaporation, cooling crystallization, and dewatering for purification. The effects of additives on caustic ratio and crystallization products, as well as the function and behavior of sodium aluminate solution during evaporation and crystallization were studied. The results show that with NaOH as an additive, the caustic ratio of the solution system can be increased, and the product from evaporation and crystallization can be converted to NaAlO2. By using NaAlO2 as seed crystal and adjusting the caustic ratio of system to 1.36 with NaOH, the product of NaAlO2 with purity of 88.1% can be obtained after evaporation at 100 ℃ for 2 h with stirring rate of 300 r/min. Then, after 1 h dewatering at 200 ℃ and 1 h purification with alcohol at 100 ℃, a kind of solid NaAlO2 can be obtained with purity of 93.8% and crystal particles of 5-25 μm.

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以铝酸钠水溶液为原料，通过蒸发-冷却析晶-脱水提纯工艺制备高纯固体铝酸钠，研究了添加剂对体系苛性比及析晶产物的影响以及铝酸钠溶液蒸发结晶过程的作用及行为。结果表明，以NaOH为添加剂能增加溶液体系苛性比，使蒸发结晶产物转变为NaAlO2；添加NaAlO2晶种、以NaOH为添加剂调节体系苛性比至1.36，蒸发温度100 ℃、结晶时间2 h、搅拌速率300 r/min条件下，可获得纯度88.1%的铝酸钠产品；在脱水温度200 ℃、脱水时间1 h、乙醇100 ℃提纯1 h条件下，可得到纯度93.8%、晶体粒度5～25 μm的固体高纯铝酸钠。

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焦芬（1983—），女，山西运城人，博士，教授，主要研究方向为再生资源高效清洁利用。E-mail：
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刘世阳（1999—），男，河南南阳人，硕士研究生，主要研究方向为铝渣无害化处理。E-mail：

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刘世阳（1999—），男，河南南阳人，硕士研究生，主要研究方向为铝渣无害化处理。E-mail：

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刘世阳（1999—），男，河南南阳人，硕士研究生，主要研究方向为铝渣无害化处理。E-mail：

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Journal of Molecular Liquids, 2016, 223: 955-959., articleTitle=Kinetics investigation on the decomposition process of supersaturated sodium aluminate solution using UV spectroscopy, refAbstract=null), Reference(id=1241327514606433063, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241321991119098478, doi=null, pmid=null, pmcid=null, year=2018, volume=176, issue=null, pageStart=253, pageEnd=259, url=null, language=null, rfNumber=[12], rfOrder=11, authorNames=LIU G, WU G, CHEN W, journalName=Hydrometallurgy, refType=null, unstructuredReference=LIU G, WU G, CHEN W, et al. Increasing precipitation rate from sodium aluminate solution by adding active seed and ammonia[J]. 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（a）30 ℃下不同αk值的蒸发结晶产物；（b）不同温度下的蒸发结晶产物

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（a）NaAlO2；（b）NaAlO2+NaOH；（c）NaAlO2+Al（OH）3；（d）NaAlO2+Na2CO3

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铝酸钠溶液中主要化学成分及含量

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铝酸钠溶液制备固体高纯铝酸钠实验研究
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刘世阳 1, 2 , 焦芬 1, 2 , 刘维 1, 2 , 李琛 1, 2 , 董良民 1, 2 , 王焕龙 1, 2 , 覃文庆 1, 2
矿冶工程杂志 | 冶金 2024,44(2): 100-105
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矿冶工程杂志 | 冶金 2024, 44(2): 100-105
铝酸钠溶液制备固体高纯铝酸钠实验研究
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刘世阳1, 2 , 焦芬1, 2 , 刘维1, 2, 李琛1, 2, 董良民1, 2, 王焕龙1, 2, 覃文庆1, 2
作者信息
  • 1.中南大学　资源加工与生物工程学院，湖南　长沙　410083
  • 2.中南大学　战略含钙矿物资源清洁高效利用湖南省重点实验室，湖南　长沙　410083

    • 刘世阳（1999—），男，河南南阳人，硕士研究生，主要研究方向为铝渣无害化处理。E-mail：

通讯作者:

焦芬（1983—），女，山西运城人，博士，教授，主要研究方向为再生资源高效清洁利用。E-mail：
Experimental Study on Preparation of High Purity Sodium Aluminate with Sodium Aluminate Solution
Shiyang LIU1, 2 , Fen JIAO1, 2 , Wei LIU1, 2, Chen LI1, 2, Liangmin DONG1, 2, Huanlong WANG1, 2, Wenqing QIN1, 2
Affiliations
  • 1.School of Minerals Processing and Bioengineering, Central South University, Changsha 410083, Hunan, China
  • 2.Hunan Provincial Key Laboratory of Clean and Efficient Utilization of Strategic Calcium-Containing Mineral Resources, Central South University, Changsha 410083, Hunan, China
出版时间: 2024-04-01 doi: 10.3969/j.issn.0253-6099.2024.02.025
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摘要
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以铝酸钠水溶液为原料，通过蒸发-冷却析晶-脱水提纯工艺制备高纯固体铝酸钠，研究了添加剂对体系苛性比及析晶产物的影响以及铝酸钠溶液蒸发结晶过程的作用及行为。结果表明，以NaOH为添加剂能增加溶液体系苛性比，使蒸发结晶产物转变为NaAlO2；添加NaAlO2晶种、以NaOH为添加剂调节体系苛性比至1.36，蒸发温度100 ℃、结晶时间2 h、搅拌速率300 r/min条件下，可获得纯度88.1%的铝酸钠产品；在脱水温度200 ℃、脱水时间1 h、乙醇100 ℃提纯1 h条件下，可得到纯度93.8%、晶体粒度5～25 μm的固体高纯铝酸钠。

高纯铝酸钠  /  蒸发结晶  /  苛性比  /  提纯

High purity sodium aluminate was prepared with sodium aluminate solution by adopting a process consisting of evaporation, cooling crystallization, and dewatering for purification. The effects of additives on caustic ratio and crystallization products, as well as the function and behavior of sodium aluminate solution during evaporation and crystallization were studied. The results show that with NaOH as an additive, the caustic ratio of the solution system can be increased, and the product from evaporation and crystallization can be converted to NaAlO2. By using NaAlO2 as seed crystal and adjusting the caustic ratio of system to 1.36 with NaOH, the product of NaAlO2 with purity of 88.1% can be obtained after evaporation at 100 ℃ for 2 h with stirring rate of 300 r/min. Then, after 1 h dewatering at 200 ℃ and 1 h purification with alcohol at 100 ℃, a kind of solid NaAlO2 can be obtained with purity of 93.8% and crystal particles of 5-25 μm.

high purity sodium aluminate  /  evaporation and crystallization  /  caustic ratio  /  purification
刘世阳, 焦芬, 刘维, 李琛, 董良民, 王焕龙, 覃文庆. 铝酸钠溶液制备固体高纯铝酸钠实验研究. 矿冶工程杂志, 2024 , 44 (2) : 100 -105 . DOI: 10.3969/j.issn.0253-6099.2024.02.025
Shiyang LIU, Fen JIAO, Wei LIU, Chen LI, Liangmin DONG, Huanlong WANG, Wenqing QIN. Experimental Study on Preparation of High Purity Sodium Aluminate with Sodium Aluminate Solution[J]. Mining and Metallurgical Engineering, 2024 , 44 (2) : 100 -105 . DOI: 10.3969/j.issn.0253-6099.2024.02.025
正文
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铝酸钠是一种重要的无机化工产品，被广泛应用于造纸工业、水处理及土木建材领域[1-4]。铝酸钠的制备工艺分为火法工艺和湿法工艺。火法工艺是将工业Al（OH）3或Al2O3添加物质的量比1∶1的Na2CO3，磨细混匀后在1 000～1 100 ℃下灼烧，生成不含结晶水的NaAlO2。火法工艺流程简单，且产物为不含结晶水的NaAlO2，但火法工艺原料成本高、过程能耗高，不适合大规模工业生产[5]。湿法工艺主要以碱溶法为主，是将金属铝或工业氢氧化铝溶解于氢氧化钠溶液中，并将溶液中苛性碱浓度调至300 g/L以上，在较高苛性比下蒸发结晶析出铝酸钠晶体[6]。湿法工艺操作简单、浸出效率高，但制备成本较高、制备条件苛刻。
目前国内外针对铝酸钠溶液制备固体铝酸钠的研究较少[7-8]，对于铝酸钠溶液中铝酸钠晶体蒸发结晶过程的析出行为尚不明晰。本文以二次铝渣碱性焙烧脱硅水浸液为研究对象，研究溶液体系中铝酸钠晶体蒸发结晶的析出行为，并通过脱水提纯工艺制备固体高纯铝酸钠。
1　实验原料及实验方法
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1.1　实验原料
实验原料为铝渣碱性焙烧水浸后脱硅的铝酸钠溶液，其主要化学成分及含量如表1所示。溶液中Al浓度为20.460 g/L，Na2O浓度为38.241 g/L，硅量指数为635.57，溶液初始苛性比（αk）为0.982。
1.2　实验方法
向浸出液中添加一定质量添加剂调节苛性比，然后在一定温度下蒸发至一定体积，冷却至20 ℃结晶；对冷却结晶后的液固体系进行过滤分离，得到带有结晶水的铝酸钠；将带有结晶水的铝酸钠置于马弗炉中在一定温度下脱水，最后用乙醇提纯得到固体铝酸钠产品。实验所用氢氧化钠、碳酸钠、氢氧化铝、乙醇均为分析纯，购自国药集团化学试剂有限公司。
脱硅溶液蒸发结晶过程中，采用式（1）计算初始苛性比αk，采用式（2）计算铝酸钠纯度θ，采用式（3）计算结晶率η。
式中n（Na2O）和n（Al2O3）分别为铝酸钠溶液中苛性碱和氧化铝物质的量，mol；c（Na2O）和c（Al2O3）分别为铝酸钠溶液中苛性碱和氧化铝的浓度，mol/L；ω（Al2O3）和ω（Na2O）分别为产品中Al2O3和Na2O的质量分数，%；R（Al2O3）和R（Na2O）分别为Al2O3和Na2O的相对分子质量；m（NaAlO2）为蒸发结晶出的铝酸钠质量，g；m（NaAlO2）0为蒸发结晶母液中铝酸钠质量，g；m（Al2O3）为蒸发结晶出的氧化铝质量，g；m（Al2O3）0为蒸发结晶母液中氧化铝质量，g。
采用X射线荧光分析仪表征蒸发结晶产物结晶率和纯度，采用X射线衍射分析仪表征蒸发结晶产物晶型，采用扫描电子显微镜表征产物微观形貌。
2　结果与讨论
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2.1　蒸发结晶产物分析
图1为Na2O-Al2O3-H2O体系拜耳法循环图。分析图1，铝酸钠溶液蒸发结晶产物主要为Al（OH）3和NaAlO2。体系中Na2O浓度逐渐增大时，Al2O3溶解度呈先增后减的趋势，B点处Al2O3溶解度达到最大。因此推测，1 mol NaAlO2晶体溶解于纯水，使体系αk值为1，在80 ℃下蒸发至一定体积后冷却至常温结晶，过滤分离得到的晶体为Al（OH）3；加入1 mol NaAlO2晶体和2 mol NaOH晶体溶解于纯水，使体系αk值为3，相同条件下得到的晶体为NaAlO2；加入1 mol NaAlO2晶体和1 mol Al（OH）3晶体溶解于纯水，使体系αk值为0.5，相同条件下得到的晶体为Al（OH）3[9-11]。
为验证体系αk值对蒸发产物的影响，选择Na2CO3、NaOH、Al（OH）3为添加剂，以0.1 mol/L NaAlO2溶液为实验体，在蒸发温度80 ℃下蒸发溶液至一定体积后冷却至室温结晶，过滤分离结晶产物并进行XRD分析，结果见图2。由图2可知，0.1 mol/L NaAlO2溶液蒸发结晶产物为Al（OH）3；0.1 mol/L NaAlO2+NaOH溶液的蒸发结晶产物由Al（OH）3转变为NaAlO2·1.25H2O；0.1 mol/L NaAlO2+Al（OH）3溶液的蒸发结晶产物仍为Al（OH）3；0.1 mol/L NaAlO2+Na2CO3溶液的蒸发结晶产物为NaAlO2·1.25H2O和Na2CO3，这是由于碳酸钠在强碱性溶液中水解程度较小，蒸发后随铝酸钠一同析出，导致铝酸钠中含有杂质。以下以NaOH为添加剂调节体系αk值。
2.2　蒸发结晶单因素实验
体系初始αk值2、结晶时间2 h、搅拌速率300 r/min条件下，蒸发温度对蒸发结晶率的影响见图3。由图3可知，随着蒸发温度提高，铝酸钠结晶率呈上升趋势，其中60～80 ℃时铝酸钠结晶率提高较明显，80～100 ℃时铝酸钠结晶率逐渐趋于平滑，100 ℃时铝酸钠结晶率为73.77%。温度升高，铝酸钠溶解度的不饱和区域增大，铝酸钠溶解度增大，因此降低温度时可以析出更多的结晶。此外，提高蒸发温度对晶体生长有促进作用。适宜的蒸发温度为100 ℃。
体系初始αk值2、蒸发温度100 ℃、搅拌速率300 r/min条件下，结晶时间及晶种添加对蒸发结晶率的影响如图4所示。由图4可知，随着结晶时间延长，铝酸钠结晶率逐渐增加，其中结晶的前2 h铝酸钠结晶率增长速率较快，结晶时间超过2 h后铝酸钠晶体的析出逐渐趋于平衡。添加NaAlO2晶种对铝酸钠结晶率有促进作用。添加NaAlO2晶种为溶液中铝酸钠晶体生长提供了作用位点[12-13]，有助于铝酸钠晶体的生长，促进了铝酸钠晶体的析出，且原生晶核的生长速率比次生晶核生产速率慢，添加晶种加快了结晶的速率。适宜条件为添加晶种、结晶时间2 h。
蒸发温度100 ℃、结晶时间2 h、搅拌速率300 r/min条件下，体系初始αk值对蒸发结晶率的影响。如图5所示。由图5可知，随着αk值增大，铝酸钠结晶率逐渐降低，铝酸钠纯度先增高后降低，αk=1.18时，结晶率达到了93.3%，αk=1.55时，纯度达到了97.1%。随着初始αk值增大，加入NaOH的量增加，溶液中NaOH浓度上升，使得NaOH先于NaAlO2析出，铝酸钠纯度降低的同时铝酸钠结晶率也在降低。适宜的初始αk值为1.36。
初始αk值1.36、蒸发温度100 ℃、结晶时间2 h条件下，冷却结晶搅拌速率对铝酸钠结晶率的影响如图6所示。由图6可知，提高搅拌速率对铝酸钠结晶率有促进作用，特别是在100～300 r/min范围内，增大搅拌速率，铝酸钠结晶率提高较大，搅拌速率300 r/min时铝酸钠结晶率为88.7%。提高搅拌速率对铝酸钠晶体生长过程中的二次成核有促进作用，晶体在外力机械力作用下“被迫”析出。适宜的搅拌速率为300 r/min。
综上所述，蒸发结晶适宜的工艺条件为：体系初始αk值1.36、蒸发温度100 ℃、结晶时间2 h、搅拌转速300 r/min，该条件下所得产物为结晶率88.1%、纯度88.7%的铝酸钠。
2.3　结晶产品脱水提纯及表征
在优化条件下制得了结晶率88.1%、纯度88.7%铝酸钠产物，该蒸发结晶产物呈黏稠状，其XRD图谱见图7。由图7可知，蒸发产物主要物相为NaAlO2和NaAlO2·1.25H2O，推测产物黏稠是结晶水的缘故，后续拟进行脱水试验。
对蒸发结晶产物进行了热重分析，结果见图8。结果表明，样品在125.9 ℃和170.4 ℃有明显失重，说明该温度下可以实现结合水的脱除。
脱水温度和脱水时间对结晶产物脱水率的影响如图9所示。由图9可知，随着脱水温度升高，结晶产物脱水率不断升高，脱水速率也有所上升，120～140 ℃间脱水率出现了大幅度提升，160 ℃脱水4 h脱水率可达99.5%，200 ℃脱水1 h脱水率可达99.98%。
160 ℃/4 h脱水产物XRD图谱见图10。由图10可知，160 ℃即可实现蒸发产物结晶水的完全脱除，验证结合水的脱除大部分在125.9 ℃下发生。综合考虑，适宜的脱水条件为200 ℃脱水1 h。
脱水后铝酸钠纯度仅88.7%。这是由于蒸发结晶过程中少量NaOH一同析出。拟进行乙醇提纯试验，提纯温度和提纯时间对脱水产物提纯效果的影响如图11所示。由图11可知，20～60 ℃条件下产品纯度无明显变化，80 ℃和100 ℃条件下产品纯度有提升。这是因为氢氧化钠与乙醇在常温下不发生反应，乙醇沸点为78.3 ℃，乙醇沸腾时，反应较为剧烈，氢氧化钠可与乙醇反应生成乙醇钠，达到提纯铝酸钠的效果。适宜的提纯条件为：温度100 ℃，时间60 min。
200 ℃脱水1 h、100 ℃提纯60 min所得铝酸钠产品XRD和SEM-EDS结果分别见图12和图13。从图12～13可知，产物铝酸钠纯度较高，与标准卡片中的表征峰均吻合，脱水后产物铝酸钠纯度为93.8%，其中杂质主要为蒸发结晶过程中一同析出的NaOH；铝酸钠产品粒度5～25 μm，其中散落的细小颗粒推测为搅拌过程中机械力作用导致颗粒间碰撞所致。
3　结论
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1）提高蒸发温度和延长结晶时间均可提高铝酸钠结晶率；添加NaAlO2晶种可提高铝酸钠结晶率；随着体系初始αk值增加，铝酸钠结晶率逐渐降低，铝酸钠纯度先增加后降低；随着冷却结晶搅拌速率提高，结晶率逐渐提高。在蒸发温度100 ℃、结晶时间2 h、体系初始αk值1.36、搅拌速率300 r/min条件下可得到结晶率88.1%、纯度88.7%的黏稠状铝酸钠产品。
2）提高脱水温度、延长脱水时间，铝酸钠晶体脱水率逐渐增加，且提高脱水温度可提高脱水速率。在脱水温度200 ℃、脱水时间1 h、添加乙醇、100 ℃下提纯60 min，可得到纯度93.8%的固体铝酸钠晶体。铝酸钠晶体颗粒呈不规则块状，大小5～25 μm。
基金
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  • 国家重点研发计划(2020YFC1909203; 2018YFC1902505)
  • 国家自然科学基金面上项目(51874356)
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2024年第44卷第2期
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doi: 10.3969/j.issn.0253-6099.2024.02.025
  • 接收时间：2023-10-20
  • 首发时间：2026-03-19
  • 出版时间：2024-04-01
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  • 收稿日期：2023-10-20
基金
国家重点研发计划(2020YFC1909203; 2018YFC1902505)
国家自然科学基金面上项目(51874356)
作者信息
    1.中南大学　资源加工与生物工程学院，湖南　长沙　410083
    2.中南大学　战略含钙矿物资源清洁高效利用湖南省重点实验室，湖南　长沙　410083

通讯作者:

焦芬（1983—），女，山西运城人，博士，教授，主要研究方向为再生资源高效清洁利用。E-mail：
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
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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