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Article(id=1241321981044380509, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241321979433767757, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.02.031, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1698163200000, receivedDateStr=2023-10-25, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773883822927, onlineDateStr=2026-03-19, pubDate=1711900800000, pubDateStr=2024-04-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773883822927, onlineIssueDateStr=2026-03-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773883822927, creator=13701087609, updateTime=1773883822927, 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=135, endPage=140, ext={EN=ArticleExt(id=1241321981296038759, articleId=1241321981044380509, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Preparation of Pseudo-boehmite with Large Pore Size and High Specific Surface Area by Using High Aluminum Pickling Sludge, columnId=1236276108207902848, journalTitle=Mining and Metallurgical Engineering, columnName=MATERIALS, runingTitle=null, highlight=null, articleAbstract=

Aluminum sulfate, sodium hydroxide, and high-aluminum pickling sludge were used as raw materials to prepare pseudo-boehmite by adopting a dual aluminum source method. The effects of pH value, reaction temperature, and urea addition on the formation and structure of pseudo-boehmite, as well as the effects of synthesis conditions on the phase and structural properties of pseudo-boehmite were investigated. The results show that as the reaction temperature increases, the specific surface area and pore volume of pseudo-boehmite increase, and the crystallinity also increases. With pH value between 6.5 and 9.5, a clear pseudo-boehmite phase can be obtained; with pH value up to 10.5, a trihydrate alumina phase will be formed. The addition of urea can significantly increase the specific surface area and pore size of pseudo-boehmite.

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以硫酸铝、氢氧化钠及高纯铝酸洗废渣为原料，采用双铝法制备拟薄水铝石，研究了pH值、反应温度及尿素添加量对拟薄水铝石的形成及结构的影响与合成条件对拟薄水铝石形成时的物相及结构性能的影响。结果表明，随着反应温度升高，拟薄水铝石比表面积和孔容增大，结晶度提高。pH值6.5～9.5时，可以得到明显的拟薄水铝石物相；pH值达到10.5时，会产生三水铝石相。添加尿素能显著增加拟薄水铝石的比表面积和孔径。

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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、材料化学。E-mail：
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袁辉（1997—），男，安徽六安人，硕士，主要研究方向为材料化学。E-mail：

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袁辉（1997—），男，安徽六安人，硕士，主要研究方向为材料化学。E-mail：

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袁辉（1997—），男，安徽六安人，硕士，主要研究方向为材料化学。E-mail：

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（a）0；（b）2%；（c）4%；（d）8%；（e）16%

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PB-7.5-80243.10.286.18
PB-8.5-80381.60.8610.31
PB-9.5-80337.40.323.64
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利用高纯铝酸洗废渣制备大孔高比表面积拟薄水铝石研究
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袁辉 1 , 贺永东 1 , 赵亿坤 1 , 孙小涵 2 , 刘小龙 3 , 杜玉峰 4 , 白万全 5 , 陈守俊 6
矿冶工程杂志 | 材料 2024,44(2): 135-140
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矿冶工程杂志 | 材料 2024, 44(2): 135-140
利用高纯铝酸洗废渣制备大孔高比表面积拟薄水铝石研究
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袁辉1 , 贺永东1 , 赵亿坤1, 孙小涵2, 刘小龙3, 杜玉峰4, 白万全5, 陈守俊6
作者信息
  • 1.新疆大学　物理科学与技术学院，新疆　乌鲁木齐　830046
  • 2.山东能源集团，山东　济南　250100
  • 3.新疆天龙矿业股份有限公司，新疆　阜康　831500
  • 4.新疆农六师铝业有限公司，新疆　五家渠　831300
  • 5.天山铝业有限公司，新疆　石河子　832061
  • 6.新疆盛安新材料股份有限公司，新疆　哈密　839000

    • 袁辉（1997—），男，安徽六安人，硕士，主要研究方向为材料化学。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、材料化学。E-mail：
Preparation of Pseudo-boehmite with Large Pore Size and High Specific Surface Area by Using High Aluminum Pickling Sludge
Hui YUAN1 , Yongdong HE1 , Yikun ZHAO1, Xiaohan SUN2, Xiaolong LIU3, Yufeng DU4, Wanquan BAI5, Shoujun CHEN6
Affiliations
  • 1.School of Physical Science and Technology, Xinjiang University, Urumqi 830046, Xinjiang, China
  • 2.Shandong Energy Group, Jinan 250100, Shandong, China
  • 3.Xinjiang Tianlong Mining Co Ltd, Fukang 831500, Xinjiang, China
  • 4.Xinjiang Nongliushi Aluminum Co Ltd, Wujiaqu 831300, Xinjiang, China
  • 5.Tianshan Aluminum Co Ltd, Shihezi 832061, Xinjiang, China
  • 6.Xinjiang Sheng'an New Materials Co Ltd, Hami 839000, Xinjiang, China
出版时间: 2024-04-01 doi: 10.3969/j.issn.0253-6099.2024.02.031
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摘要
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以硫酸铝、氢氧化钠及高纯铝酸洗废渣为原料，采用双铝法制备拟薄水铝石，研究了pH值、反应温度及尿素添加量对拟薄水铝石的形成及结构的影响与合成条件对拟薄水铝石形成时的物相及结构性能的影响。结果表明，随着反应温度升高，拟薄水铝石比表面积和孔容增大，结晶度提高。pH值6.5～9.5时，可以得到明显的拟薄水铝石物相；pH值达到10.5时，会产生三水铝石相。添加尿素能显著增加拟薄水铝石的比表面积和孔径。

双铝法  /  拟薄水铝石  /  尿素  /  孔径  /  孔容  /  比表面积

Aluminum sulfate, sodium hydroxide, and high-aluminum pickling sludge were used as raw materials to prepare pseudo-boehmite by adopting a dual aluminum source method. The effects of pH value, reaction temperature, and urea addition on the formation and structure of pseudo-boehmite, as well as the effects of synthesis conditions on the phase and structural properties of pseudo-boehmite were investigated. The results show that as the reaction temperature increases, the specific surface area and pore volume of pseudo-boehmite increase, and the crystallinity also increases. With pH value between 6.5 and 9.5, a clear pseudo-boehmite phase can be obtained; with pH value up to 10.5, a trihydrate alumina phase will be formed. The addition of urea can significantly increase the specific surface area and pore size of pseudo-boehmite.

dual aluminum source method  /  pseudo-boehmite  /  urea  /  aperture  /  pore volume  /  specific surface area
袁辉, 贺永东, 赵亿坤, 孙小涵, 刘小龙, 杜玉峰, 白万全, 陈守俊. 利用高纯铝酸洗废渣制备大孔高比表面积拟薄水铝石研究. 矿冶工程杂志, 2024 , 44 (2) : 135 -140 . DOI: 10.3969/j.issn.0253-6099.2024.02.031
Hui YUAN, Yongdong HE, Yikun ZHAO, Xiaohan SUN, Xiaolong LIU, Yufeng DU, Wanquan BAI, Shoujun CHEN. Preparation of Pseudo-boehmite with Large Pore Size and High Specific Surface Area by Using High Aluminum Pickling Sludge[J]. Mining and Metallurgical Engineering, 2024 , 44 (2) : 135 -140 . DOI: 10.3969/j.issn.0253-6099.2024.02.031
正文
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拟薄水铝石（Al2O3·nH2O，n=1.4～2.0）又名假一水软铝石，是一种结晶不完全、从无序到有序、从弱晶态到晶态的产物，是制备活性氧化铝的重要前驱体，具有高比表面积和大孔容孔径[1]，主要用作催化剂及催化剂载体原料、吸附剂、干燥剂等，被广泛应用于石油化工、环境保护、陶瓷、涂层等行业[2-5]。目前我国在石油化工领域中不仅要求拟薄水铝石具有较大的孔容、孔径，还要求其具有较低的生产成本[6]。因此，需要开发大孔容和大孔径拟薄水铝石的低成本制备方法。
拟薄水铝石的制备方法主要为中和法和有机醇铝法[7-8]。有机醇铝法制备的拟薄水铝石纯度高、结晶度好，但制备工艺复杂、原料成本较高，不易大规模生产[9-10]。目前，我国主要使用碳化中和法[11]与双铝中和法[12]制备拟薄水铝石，采用铝土矿溶出精炼后的NaAlO2溶液作为原料。碳化中和法是将CO2气体通入NaAlO2溶液水解得到结晶度较高的拟薄水铝石产品，由于是气液两相反应，反应过程不易控制，产物孔径不均匀，孔结构性能较差。双铝中和法是利用铝盐与NaAlO2溶液发生中和反应得到结晶度不高但孔容、孔径较好的拟薄水铝石，此方法工艺简单且成本低廉。
本文采用高纯铝酸洗废渣作为原料，以双铝中和法制备拟薄水铝石，通过调控pH值与水解温度探究拟薄水铝石相和孔结构性能，选择适宜的制备工艺。以尿素为扩孔剂，对双铝中和法进行优化，探究适宜的尿素含量，从而制备具有高质量、大孔容、大孔径的拟薄水铝石产品。
1　实验
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1.1　实验材料
实验原料为高纯铝酸洗废渣（新疆众和股份有限公司）；实验用水为去离子水；实验试剂包括NaOH（分析纯）、Al2（SO4）3（分析纯）和尿素（分析纯）。
原料呈白色颗粒状，粒度在0.147 mm以下，主要含有O、Al、H、N、Na等元素，主要元素含量如表1所示。由元素含量可推测原料的主要物相为Al（OH）3、NaNO3、Na2O等。对原料进行水洗除杂，原料、原料处理后废液及固渣XRD分析结果如图1所示。由图1可知，未处理原料的主要特征衍射峰为NaNO3，并无其他特征衍射峰，经多次水洗后的废渣样品无明显特征峰，原料处理后留下的废液（干燥成粉末后检测）则以NaNO3形式呈现。由此可见，水洗可以有效去除NaNO3，实现物相分离。
将原料放入烧杯，在60 ℃下水洗搅拌5 h，之后将水洗后的废渣过滤放入干燥箱中烘干。称取39 g烘干废渣，配置500 mL NaOH溶液（4%），将废渣加入NaOH溶液中，90 ℃下恒温水浴搅拌1 h，利用离心机过滤得NaAlO2溶液，其XRD图谱如图2所示。图中主要衍射峰为NaAlO2，并伴随少量NaNO3，其为洗涤后原料中的部分残留物。
1.2　实验方案
配制Al2（SO4）3溶液（10%），将NaAlO2和Al2（SO4）3溶液以流速4 mL/min流至装有200 mL去离子水的三颈烧瓶中，利用pH计观察滴定过程中溶液的pH值变化，恒温水浴搅拌1 h，搅拌速率为1 000 r/min，滴加适量的尿素，继续搅拌时效1 h，将时效后的溶液放入抽滤瓶中进行抽滤，抽成滤饼后，反复洗涤过滤，最终将滤饼放入80 ℃干燥箱中，干燥后破碎研磨成粉末，得到拟薄水铝石样品，工艺流程如图3所示。以（U）PB-X-Y-Z命名样品：U表示尿素，PB表示拟薄水铝石，X表示pH值，Y表示温度，Z表示尿素掺杂量。例如，UPB-8.5-80-8%是指在80 ℃、pH值8.5、使用质量分数8%的尿素制备的拟薄水铝石。
1.3　表征
使用X射线衍射仪（D8 advance）表征拟薄水铝石的物相。采用表面积分析仪（TriStarⅡ3020）进行N2吸附脱附，测试温度-195.8 ℃；测试前，在300 ℃下对样品脱气处理5 h。分别使用Brunauer-Emmett-Teller（BET）和Barrett-Joyner-Halenda（BJH）方法检测拟薄水铝石的比表面积和孔容孔径。采用场发射电子扫描电镜（SU8010）表征拟薄水铝石的形貌。采用傅里叶红外光谱仪（VERTEX 70 RAMI）对实验样品的官能团进行红外光谱表征。
2　结果与讨论
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2.1　pH值对拟薄水铝石的影响
水解温度80 ℃，不同pH值条件下制备的拟薄水铝石XRD图谱如图4所示。由图4可知，pH值6.5～9.5时，可制得具有拟薄水铝石相的氧化铝样品；pH值达到10.5时，样品中开始出现三水铝石衍射峰；pH值升至12时，衍射峰发生变化，拟薄水铝石相大多转化为三水铝石相。
水解pH值较低时，由于特定层错及正常层的旋转与位移，衍射峰朝右偏移[13]；pH值超过10.5时，可以发现18.5°处存在三水铝石相的衍射峰。在NaAlO2与Al2（SO4）3的反应体系中，二者并流时会发生式（1）所示的反应，形成无定形的Al（OH）3沉淀。随着pH值升高，溶液中残留的NaAlO2会水解形成三水铝石，如式（2）所示。
不同pH值条件下拟薄水铝石的N2吸附-脱附等温线及孔径分布曲线见图5。由图5可知，等温线均为典型Ⅳ型，伴随迟滞回线出现，表明有孔结构的存在[14-15]。同时，这些迟滞回线属于H2型和H3型复合物，表明样品与墨水瓶状孔隙具有一定的孔连通性。pH值6.5～9.5范围内制备的样品环闭合点较高，表明孔隙较大，孔径分布范围很宽[16]。随着pH值升高，拟薄水铝石样品的迟滞回线升至较高的相对压力范围，表明孔容、孔径增大。除了pH值8.5时制备的拟薄水铝石孔径分布比较宽泛，其余pH值条件下制备的拟薄水铝石孔径基本分布在2～7 nm之间。
不同pH值条件下制备的拟薄水铝石孔结构物理特性数据如表2所示。由表2可知，pH值从6.5升至8.5时，样品比表面积从155.2 m2/g升至381.6 m2/g；pH值超过8.5后，拟薄水铝石样品结构发生变化，导致平均孔径、孔容变小。pH值较高时，样品中存在可溶性负电荷物质[AlnOm（OH）p]（p+2m-3n）-，其会进入勃姆石晶格并促进晶粒生长[17-18]。在高pH值环境中，β1-Al（OH）3大晶粒的溶解和再沉淀会降低拟薄水铝石样品的比表面积。
2.2　温度对拟薄水铝石的影响
pH=8.5，不同温度下制备的拟薄水铝石的XRD图谱见图6。从图6可以看出，样品的物相均为拟薄水铝石。随着温度升高，样品衍射峰强度逐渐增强，表明温度越高，样品结晶度越高，晶粒尺寸越大。温度低于50 ℃时，拟薄水铝石样品结晶度较差。较高的反应温度有利于促进胶体成核，使样品具有较好的结晶度[16]。同时伴随着温度升高，样品衍射峰没有发生明显偏移，说明温度变化对样品晶体结构并无影响。
pH=8.5，不同温度下拟薄水铝石的N2吸附-脱附等温线及孔径分布曲线如图7所示。由图7可知，所有样品的等温线均为典型Ⅳ型，表明这些样品本质上是介孔材料。在相对压力0.4～0.8的中压区发生了毛细凝聚现象，出现迟滞回线，其介于H2型和H3型之间，说明这些样品与通道状孔隙具有较好的连通性。样品PB-8.5-70和PB-8.5-80具有宽孔径分布，样品PB-8.5-40和PB-8.5-50孔径主要分布于5～20 nm之间，其余样品的孔径基本分布在2～5 nm之间。
不同温度下拟薄水铝石孔结构物理特性见表3。由表3可知，随着温度升高，拟薄水铝石样品比表面积、孔容和孔径整体呈先增大后减小的趋势，其中在80 ℃下制备的样品比表面积、孔容分别为381.6 m2/g、0.86 cm3/g。由此可得，拟薄水铝石可以在不同温度下制备，且在一定温度范围内随着温度升高，其比表面积和孔容增大。
2.3　尿素添加量对拟薄水铝石的影响
80 ℃、pH=8.5时，缓慢加入不同含量的尿素，对样品进行水解，不同尿素添加量下制备的拟薄水铝石XRD图谱见图8。由图8可知，掺杂后的样品中均存在拟薄水铝石相，随着尿素添加量增加，样品衍射峰强度增大，半高宽减小；尿素添加量达到16%时，样品特征衍射峰强度开始减小，说明尿素掺杂过量时，可能会阻碍晶粒的生长。
图9为不同尿素添加量下拟薄水铝石的红外光谱分析图。由图9可知，3 000～3 750 cm-1范围内存在明显的吸收峰，其与1 639 cm-1处的吸收峰均为拟薄水铝石表面吸附水的弯曲振动。482 cm-1与613 cm-1处的吸收峰属于Al—O—Al的伸缩振动；1 076 cm-1与3 093 cm-1处的吸收峰属于拟薄水铝石羟基的弯曲振动；756 cm-1处的吸收峰属于拟薄水铝石羟基的面外弯曲振动。对比不同样品的红外光谱可以发现样品均为拟薄水铝石。尿素添加量16%时制备的样品在3 093 cm-1及1 076 cm-1处的吸收峰不明显，说明此时样品结晶度不高，尿素添加量2%～8%范围内的吸收峰则较明显。
图10为不同尿素添加量下拟薄水铝石的N2吸附-脱附等温曲线和孔径分布曲线。由图10可知，所有样品等温线均为典型Ⅳ型，均存在中孔，与未掺杂尿素的拟薄水铝石（PB-8.5-80）相似。通过尿素改性后的样品迟滞回线为H3型，存在较宽的孔隙。与未掺杂尿素的样品相比，改性后的拟薄水铝石具有宽孔径分布，孔隙宽度明显增大，其中UPB-8.5-80-4%和UPB-8.5-80-8%样品孔径主要集中于15.2 nm左右，未添加尿素的样品孔径主要集中在7.4 nm。由此可得，尿素能有效提高拟薄水铝石的孔径宽度。
图11为不同尿素添加量下拟薄水铝石的SEM图。由图11可知，拟薄水铝石样品形貌均为片状。加入尿素后的拟薄水铝石中出现了明显的大孔结构；尿素添加量8%时，样品中形成了较大的孔径，但当掺杂的尿素超过一定量时，孔径变小。可见添加尿素可以调整样品孔径大小、改变样品形态，达到扩孔的效果，但掺杂过多时，样品孔径会减小。
不同尿素添加量掺杂后拟薄水铝石孔结构物理特性如表4所示。由表4可知，随着尿素添加量增加，拟薄水铝石样品比表面积增大，但当尿素添加量超过8%后，比表面积随着尿素添加量增加而减小。通常比表面积越大，孔径越小，但在本实验中，添加8%尿素制备得到了具有高比表面积和大孔结构的拟薄水铝石，其性能超过了传统工艺制备的拟薄水铝石。然而，尿素添加过量时，改性后样品比表面积可能会小于未掺杂尿素的样品。
3　结论
收起
1）在不同pH值下合成拟薄水铝石，随着pH值升高，样品物相发生变化，pH=10.5时开始形成三水铝石相；pH=8.5时拟薄水铝石具有较好的吸附能力。
2）在不同温度下制备的样品均为拟薄水铝石，随着温度升高，拟薄水铝石相结晶度有所提高且样品孔结构大小呈先升高后降低的趋势，80 ℃时拟薄水铝石具有大孔径和高比表面积。
3）为了进一步提高拟薄水铝石性能，在pH=8.5、温度80 ℃时掺杂尿素，随着尿素添加量增加，样品比表面积、孔容、平均孔径均有所增加，尿素添加量8%时，拟薄水铝石的改性条件适宜。
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项目(2020B02007)
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doi: 10.3969/j.issn.0253-6099.2024.02.031
  • 接收时间：2023-10-25
  • 首发时间：2026-03-19
  • 出版时间：2024-04-01
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  • 收稿日期：2023-10-25
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项目(2020B02007)
作者信息
    1.新疆大学　物理科学与技术学院，新疆　乌鲁木齐　830046
    2.山东能源集团，山东　济南　250100
    3.新疆天龙矿业股份有限公司，新疆　阜康　831500
    4.新疆农六师铝业有限公司，新疆　五家渠　831300
    5.天山铝业有限公司，新疆　石河子　832061
    6.新疆盛安新材料股份有限公司，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、材料化学。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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