KCl-NaOH混合碱熔分解锆英砂工艺研究

采用KCl作为添加剂,研究了KCl-NaOH混合碱熔分解锆英砂过程中KCl与锆英砂摩尔比、反应温度、反应时间对锆英砂分解率的影响。采用X射线衍射仪(XRD)和差热-热重分析仪(DTA-TG)对分解产物的物相组成和反应过程中的热现象进行分析。结果表明:随着KCl与锆英砂摩尔比的增加,锆英砂的分解率先升高后下降,当KCl与锆英砂摩尔比为0.15时,锆英砂的分解率达到最大值,为98.26%。锆英砂的分解率随反应温度的升高和反应时间的延长而增大,当反应温度超过700℃,反应时间超过30min后,锆英砂的分解率不再有明显变化。KCl-NaOH混合碱熔分解锆英砂的最佳工艺条件为:KCl与锆英砂摩尔比为0.15,反应温度为700℃,反应时间为30min。锆英砂碱熔分解后的主要产物为Na2ZrO3,Na_4SiO_4和K2SiO3。KCl-NaOH混合碱熔分解锆英砂体系在温度升高至660℃以后发生放热反应,且反应过程中有水蒸气生成,水蒸气不断逸出体系导致体系出现明显的失重现象。     

CaCl2和NaOH复合分解锆英砂工艺研究

采用CaCl2做添加剂,研究了CaCl2加入量对锆英砂碱熔分解工艺锆转化率的影响。将锆英砂和固体氢氧化钠按质量比1：1．2混合均匀,分别加入0．2％、0．4％、0．6％、0．8％、1％的氯化钙（以锆英砂的百分比计）,然后置于坩埚中,在马弗炉中按设定的温度和时间进行高温烧结。对CaCl2和NaOH复合分解锆英砂产物的物相组成和反应过程中的热变化进行了分析。研究结果表明,当CaCl2加入量为0．8％时,烧结料中可溶性锆含量达到最大值31．04％。锆英砂经CaCl2和NaOH高温烧结后,烧结料中不溶物的物相组成主要为Na2ZrO3。     

Ca（OH）2的加入量对锆英砂碱熔分解过程的影响

在锆英砂与氢氧化钠质量比为1.0∶1.2时,分别选取锆英砂含量0.2%,0.4%,0.6%,0.8%和1.0%的Ca(OH)2作为添加剂,研究Ca(OH)2加入量对锆英砂碱熔分解过程的影响。采用X射线衍射仪和差热-热重分析仪对反应物料的组成和反应体系热量变化进行分析。结果表明:在Ca(OH)2加入量为1.0%时,锆英砂的分解率达到最大值,为96.4%,碱熔过程中在590℃以后发生剧烈的放热反应,锆英砂碱熔分解后的主要产物为Na2ZrO3和Na2SiO3。烧碱和添加剂复合分解锆英砂的适宜工艺条件为:烧结温度为750℃,烧结时间为30 min。     

氧化铝生产中结晶草酸钠的无毒化处理

针对结晶洼除去拜尔液中草酸钠的工艺。用氩氧化钙对结晶出的草酸钠进行无毒化处理，并可回收苛性碱。苛化的最佳工艺条件是：反应温度50℃、氧化钙粒度小于140目、CaO／Na2C2O4（分子比）〉1．2、反应时间1h。在此条件下．苛化效率可以达到99．2％以上。在含有苛性碱的溶液中，Na2O浓度〈3.2g／L时草酸钠可以稳定存在．而在含有碳碱的溶液中，草酸钠的稳定性不是很好。     

固相反应法制备β″-Al_2O_3粉末的热力学研究

以Na2CO3和α-Al2O3为原料,Na2CO3与α-Al2O3的物质的量比为1:6,采用固相合成法制备β″/β-Al2O3粉末。通过热力学计算原料粉末在不同温度下可能发生的化学反应的吉布斯自由能,并结合Na2CO3/α-Al2O3混合粉末的DTA曲线,研究可能发生的化学反应的温度条件。同时,用X射线衍射仪(XRD)对固相合成粉末的物相组成进行分析。结果表明,Na2CO3/α-Al2O3混合粉末在1 150℃左右开始发生反应生成β″/β-Al2O3;最适宜的反应温度为1 250℃,α-Al2O3全部转化为β/β″-Al2O3,并且β″-Al2O3含量最高;当温度升高到1 400℃时,β/β″-Al2O3发生分解,生成α-Al2O3和Na2O,并且随温度升高,更多的β/β″-Al2O3发生分解,而Na2O在高温下挥发会促进β/β″-Al2O3的分解。当煅烧温度超过1 500℃时,β″-Al2O3分解还生成微量的Na Al O2。     

固体酸La2O3-Ga2O3/硅胶的研制及其催化合成丙酸异丁酯

采用自制固体酸La2O3-Ga2O3/硅胶为催化剂催化丙酸与异丁醇进行酯化反应合成了丙酸异丁酯,并采用IR分析对催化剂进行了表征。催化剂的制备条件为La2O3∶Ga2O3∶硅胶=5∶20∶75(质量比),500℃焙烧2 h。考察了催化剂用量、醇酸物质的量比、反应时间、带水剂种类和催化剂的重复使用性等因素对酯化率的影响。结果表明,适宜的反应条件为0.20 mol丙酸,催化剂用量1.00 g、醇酸物质的量比1.8,反应时间90 min,酯化率可达98.2%。     

沉淀法制备微米四氧化三钴试验研究

研究了以氯化钴为钴源,采用碳酸钠、氢氧化钠、碳酸氢铵沉淀体系制备Co_3O_4。以碳酸氢铵为沉淀剂制备前驱体,煅烧后制得四氧化三钴。结果表明,物质的量比是影响前驱体物相的主要因素:碳酸氢铵与氯化钴物质的量比≤3∶1时,前驱体为碱式碳酸钴(Co(CO_3)_(0.5)(OH)·0.11H_2O);碳酸氢铵与氯化钴物质的量比为4.5∶1时,前驱体为碳酸钴(CoCO_3)和复合碱式碳酸钴((NH_4)_2Co_8(CO_3)_6(OH)_6·4H_2O)的混合物。采用该体系,在物质的量比4.5∶1,氯化钴质量浓度13 g/L、反应温度60℃、反应时间10 h条件下,所得Co_3O_4粉体粒度分布均匀且范围窄,D_(50)为9.08μm,形貌为类球形。     

NaPO3 用于粗锑火法精炼过程除铅

针对传统粗锑精炼工艺中除铅的难题,提出用Na PO3作为除铅剂,生成磷酸盐渣浮于锑液表面除去的方法.用热重-差热法和X射线衍射技术研究反应机理并进行粗锑除铅的条件实验.研究发现,Pb O与Na PO3在590℃时即开始吸热反应,在850℃以下主要形成Na Pb4(PO4)3,而在850℃以上主要形成Na Pb PO4,反应彻底.Pb O、Sb2O3和Na PO3混合物的反应表明:在Na PO3量不足时,优先与Pb O反应,只有当Na PO3足量时才会与Sb2O3生成锑的非晶态玻璃.用Na NO3作为氧化剂,在氮气保护下进行了除铅单因素实验,考察反应时间和温度、Na PO3和Na NO3加入量对结果的影响.在最优条件下精锑含铅0.047%,除铅率98.90%.     

含钛磁铁矿精矿氢还原冶炼时碳酸钠对相变的影响

俄罗斯莫斯科市的一冶金研究机构近来进行了这项研究。将含钛磁铁精矿（含Fe2O361．3％，TiO23．0％）与1．5％或2．5％的Na2CO3混合，在氢气流量为18．5cm3／min的条件下加热到700～1000C。这时添加剂Na。CO。可促使还原反应加速，其原因是：Na。C（）s可使主要含铁相在700～IOOOC下分解，并限制在温度＞11O0C时生成铁的固溶相。在反应的后阶段，由于reo、vgo及其它相的分离，St（人生成铝硅酸盐，使Na入）的耗量增加。随着青铜色氧化物（温度＜gOOC）或钛酸钠（温度＞1100C）的形成，剩余的NaD与Ti人结合。在游离MgO出现的过…     

Zr(HPO4)(C6H5PO3)/Cr2O3选择性催化合成苯酚的研究

报道了以Zr(HPO4)(C6H5PO3)／Cr2O3为苯选择性氧化为苯酚的催化剂，对苯氧化制备苯酚的反应条件进行了研究。实验表明：最佳条件为n(C6H6)：n(H2O2)=1：0．75，催化剂用量为反应反应物料总质量的1．0％，反应时间为12h，反应温度为55℃。在上述条件下，苯的转化率可达到45．1％，苯酚的收率可达到42．8％，催化剂Zr(HPO4)(C6H5POH)／Cr2O3的氧化苯制备苯酚的选择性达到94．9％。     

Decomposition Reaction of Mixed Rare Earth Concentrate and Roasted with CaO and NaCl

The reaction of the mixed rare earth concentrate including monazite ( REPO4 ) and bastnaesite ( REFCO3 )decomposed by CaO and NaCl additives at the temperature range from 100 to 1000 ℃ was studied by means of XRD and TG-DTA.The results show that when CaO and NaCl are not added, only REFCO3 can be decomposed at the temperature of 377 ～ 450 ℃.The decomposition products include REOF, RE2O3 and CeO2.However, REFCO3 can not be decomposed.When CaO is added, the decomposition reactions occur at the temperature range from 660 to 750 ℃.CaO has three decomposition functions: ( 1 ) REPO4 can be decomposed by CaO and the decomposition products include RE2O3 and Ca3 (PO4)2; (2) CaO can decompose REOF, and the decomposition products are RE2O3 and CaF2; (3)CaO can decompose REPO4 with CaF2, and the decomposition products are RE2 O3, Ca5 F( PO4 )3.The decomposition ratio of the mixed rare earth concentrate increased obviously, when CaO and NaC1 were added.NaC1 can supply the liquid for the reaction, improve the mass transfer process and accelerate the reaction.At the same time, NaC1 participated in the reaction that REPO4 was decomposed by CaO.     

钨钼混配型杂多酸盐催化剂上酯化反应条件的优化研究

以Na2WO4·2H2O和 Na2MoO4·2H2O为原料,通过硝酸酸化-乙醚萃取法制备了一种钨钼混配型杂多酸盐催化剂（Na4SiMoW12O40·xH2O）.应用X射线荧光光谱对合成的催化剂的元素组成进行了分析;通过红外光谱对其的官能团结构进行了分析;借助热重分析对其的热稳定性进行了研究.并以正丁醇和乙酸为反应物,研究了所制备的钨钼混配型杂多酸盐在催化酯化反应时的活性和稳定性.通过正交试验[L9（3）4]对影响乙酸正丁酯收率的关键影响参数进行了优化,包括催化剂与反应物的质量比、反应时间和温度、以及正丁醇与乙酸的摩尔比.结果表明：当反应时间为120 min,反应温度为90℃,催化剂用量为0.4 g,醇酸摩尔比为2∶1,酯化效果最好,达到93.24 wt%.     

Influence of NaCl-CaCl2 on Decomposing REPO4 with CaO

The influence of NaCl-CaCl2 on thermal decomposition of REPO4（RE： Ce, La, Nd, Th） with CaO was studied. The heat decomposing process of REPO4 was tested with TG-DTA experiments. The results showed that the decomposition temperature of REPO4 with CaO was reduced because of adding NaCl-CaCl2 mixture （NaCl：CaCl2 = 1：1 ）. The influence of the addition of NaCl-CaCl2, roasting temperature and roasting time on decomposition ratio of REPO4 with CaO was studied. The results showed that the decomposition ratio of REPO4with CaO was 79% when the addition percentage of NaCl-CaCl2 was 10%, the roasting temperature was 750℃, and the roasting time was 1 h.     

铅锌混合矿氧气熔融脱硫

随着烧结+鼓风炉工艺处理铅锌混合精矿能耗高和环境污染的问题日益凸显,使用熔池熔炼法替代烧结工艺成为铅锌混合精矿较好的火法冶炼工艺选择。采用静态法和XRD技术研究了O₂流量、温度、入炉炉料成分对铅锌混合矿脱硫的影响以及脱硫渣物相变化。结果表明:与烧结工艺相比,铅锌混合精矿高温熔融脱硫时间短、脱硫率高。O₂流量的增加和温度的提高有利于铅锌混合矿脱硫反应的进行,铅锌混合矿脱硫率随着ω（Fe）/ω（SiO₂）和ω（CaO）/ω（SiO₂）的增加而降低,但在1 400 ℃时ω（CaO）/>ω（SiO₂）的增加有利于脱硫速率的加快和脱硫率的增加。当反应温度为1 250 ℃时,随着熔渣中Fe/SiO₂的增加,熔渣中尖晶石相（Zn_xFe_3-xO_4+y）开始形成并增多。      

Kinetics of mixed rare earths minerals decomposed by CaO with NaCl-CaCl₂ melting salt

For increasing reaction rate and reducing decomposing temperature,TG-DTA,XRD,SEM and Chemical analysis were used to study the kinetics of mixed rar e earths minerals decomposed by CaO with NaCl-CaCl2. The results showed that the reaction rate increased with increasing of NaC-CaCl2 addition,CaO addition,an d decomposition temperature. The kinetics of mixed rare earths minerals decompos ed by CaO conformed to 1-2/3X-(1-X) 2/3=kdt mode. The decomposition reaction rate was controlled by two steps,and the activation energy was decreased with addin g of NaCl-CaCl2 melting salt. The micro-pattern of products was loosening and po rous with NaCl-CaCl2 in decomposition system.     

Determination of optimal conditions for obtaining a mixture of associated dioxides of zirconium and silicon by sintering of ZrSiO4 with MgO

Obtaining dissociated zircon (a mixture of associated dioxides of zirconium and silicon (ZrO₂, SiO₂) by sintering ZrSiO₄ with MgO and the subsequent leaching of the forming pitch by concentrated hydrochloric acid is studied. The mechanism of sintering of the ZrSiO₄ + MgO mixture is established based on laboratory investigations. The optimal parameters of the process (the molar ratio of components and the temperature and duration of heating at the final temperature) for the maximal transformation of zircon into zirconium dioxide are determined.     

Study on Roasting Decomposition of Mixed Rare Earth Concentrate in CaO-NaCl-CaCl2

The decomposed process of bastnaesite, monazite and mixed rare earth concentrate in CaO-CaCl-CaCl2 was studied by means of TG-DTA method. The relationship among decomposition ratio, roasting temperature, and CaO-NaCl addition was studied by the quadratic regression orthogonal analysis, and then the regression equation was obtained. Through analysis, the optimum process conditions of mixed rare earth concentrate decomposed by CaO-CaCl-CaCl2 were obtained as follows: roasting temperature: 700 ℃, CaO addition: 15%, NaCl-CaCl2 addition: 10%, roasting time: 60 min, the decomposition ratio: 91.3%.     

Kinetics of mixed rare earths minerals decomposed by CaO with NaCl-CaCl2 melting salt

For increasing reaction rate and reducing decomposing temperature, TG-DTA, XRD, SEM and Chemical analysis were used to study the kinetics of mixed rare earths minerals decomposed by CaO with NaCl-CaCl₂. The results showed that the reaction rate increased with increasing of NaC-CaCl₂ addition, CaO addition, and decomposition temperature. The kinetics of mixed rare earths minerals decomposed by CaO conformed to 1-2/3X-(1-X)^2/3=k_dt mode. The decomposition reaction rate was controlled by two steps, and the activation energy was decreased with adding of NaCl-CaCl₂ melting salt. The micro-pattern of products was loosening and porous with NaCl-CaCl₂ in decomposition system.     

煤焦还原分解烧结烟气脱硫石膏的试验

 针对烟气脱硫石膏综合利用问题,提出了利用煤焦还原分解石膏制备CaO和SO2的新方法。采用FactSage 6.1计算了煤焦与脱硫石膏的高温反应特性,并利用热重分析仪在理论上分析了煤焦还原分解石膏行为的可行性。通过管式电阻炉试验进一步研究了温度、煤焦添加量、保温时间对石膏分解率和固态产物影响以及气体SO2释放规律。试验结果表明,升高温度、增加煤焦添加量和保温时间均能提高石膏的分解率;煤焦质量分数从5%增加到20%,CaO和SO2的质量分数先升高后下降,而CaS的质量分数一直增大;在煤焦量为11%时,CaO和SO2的质量分数达到最大值,CaO和SO2成分的变化规律主要受CaS和CaSO4相对含量的影响。采用煤焦还原分解石膏的方法,可为石膏综合利用提供理论指导。