CN1263675C - Inert thick salt medium method for preparing nanometer powder - Google Patents

Inert thick salt medium method for preparing nanometer powder Download PDF

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CN1263675C
CN1263675C CN 200410060779 CN200410060779A CN1263675C CN 1263675 C CN1263675 C CN 1263675C CN 200410060779 CN200410060779 CN 200410060779 CN 200410060779 A CN200410060779 A CN 200410060779A CN 1263675 C CN1263675 C CN 1263675C
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易求实
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湖北教育学院
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Abstract

惰性浓盐介质法制备纳米粉体的方法,涉及一种用沉淀法制备纳米粉体的方法。 Concentrated salt thereof as an inert medium prepared nanopowder relates to a method for precipitation Nanoparticles Prepared by. 是先将要进行反应的物质分别溶解在一种或几种惰性的高浓度盐组成的溶液中,然后在搅拌下进行混合反应,将反应产生的产品沉淀物经过滤,用含有分散剂的洗涤剂洗尽惰性浓盐,经干燥得到纳米粉体材料;或将反应产生的产品前驱体沉淀物,经过滤后进行干燥、粉碎、热分解,然后经冷却、洗涤、过滤、干燥得纳米粉体材料。 Is a substance to be reacted are first dissolved in a high concentration solution of salt of one or more inert the composition, and then mixing with stirring, the reaction products resulting precipitate was filtered, washed with a detergent containing a dispersing agent inert concentrated salt washed away, and dried to obtain nano-powder; or the reaction product of a precursor precipitate was filtered and dried, pulverized, thermal decomposition, then cooled, washed, filtered and dried to obtain nano-powder . 惰性浓盐中的盐是指在制备条件下不与反应物、前驱体沉淀物、产物及溶剂发生反应,并能稳定存在的盐。 Concentrated hydrochloric salt in an inert means that no reactant, precursor precipitate, the solvent and reacting the product under production conditions, and stable salts present. 本方法能简便有效的抑制沉淀的生长速率和防止沉淀的二次凝聚。 This simple method can effectively inhibit the growth rate of precipitation and the precipitation preventing secondary aggregation. 本方法可适用于金属氧化物、金属氢氧化物、难溶性金属盐、非金属氧化物等纳米粉体的制备。 The present method is applicable Preparation of Nano metal oxides, metal hydroxides, metal salts poorly soluble, non-metal oxide and the like in.

Description

惰性浓盐介质法制备纳米粉体的方法 Nanometer inert powder concentrated salt media SYSTEM method

技术领域 FIELD

本发明涉及一种用沉淀法制备纳米粉体的方法。 The present invention relates to a method for use of nano powder prepared by precipitation.

背景技术 Background technique

液相沉淀法是制备纳米粉体中较为常用的一种方法,其优点是无需苛刻的物理条件,就可能得到性能较优异的纳米粉体。 Precipitation method Preparation of Nano is more commonly used in a method, the advantage without harsh physical conditions, it is possible to obtain relatively excellent performance nanopowder. 它是在溶液状态下将不同化学成分的物质混合产生沉淀,以制取纳米粒子产品或前驱体沉淀物。 It is a substance in a solution state with different chemical compositions mixing a precipitate, in the preparation of nanoparticles or a precursor product precipitates. 产品沉淀物用含分散剂的洗涤剂进行洗涤,然后过滤、干燥得纳米粉体材料;前驱体沉淀物,过滤后进行干燥、粉碎、热分解,然后冷却、用含分散剂的洗涤剂进行洗涤、过滤、干燥得纳米粉体材料。 Product-containing detergent precipitate was washed with a dispersant, then filtered and dried to obtain nano-powder; precursor precipitate filtered and dried, pulverized, thermal decomposition, followed by cooling, with a detergent containing washing dispersant , filtered, and dried to obtain nano-powder.

沉淀法按其特点又可分为直接沉淀法、间接沉淀法、水解沉淀法等。 Precipitation their features can be divided into direct precipitation method, precipitation method indirect hydrolysis precipitation method.

直接沉淀法是在一定的条件下,在包含一种或多种离子的可溶性盐溶液中加入沉淀剂和分散剂,直接生成沉淀,从溶液中析出,将杂质离子除去,沉淀物经干燥、热分解等操作制得纳米粉体。 Direct precipitation under certain conditions, comprising adding one or more soluble ionic salt solution precipitating and dispersing agents, to directly generate precipitate out of solution, the impurity ions are removed, the precipitate was dried, heat decomposition operation had nanopowders. 由于加入的沉淀剂不可能在瞬间分散于整个溶液中,导致成核、长大、沉淀的过程难以控制,易发生不均匀成核,而使制得的粉体粒度不均匀。 Due to the addition of the precipitating agent can not instantaneously dispersed throughout the solution, leading to nucleation, growth, difficult to control the precipitation process, nonuniform nucleation easily occurs, unevenness of the obtained powder particle size.

间接沉淀法也叫均匀沉淀法,是利用某一化学反应使溶液中的构晶离子从含有分散剂的溶液中缓慢地、均匀地释放出来,其他的步骤与直接沉淀法相同。 Indirect precipitation method is also called homogeneous precipitation method, a chemical reaction is the use of the crystal structure of the ions in the solution slowly and uniformly released from the solution containing the dispersing agent, other steps are the same as direct precipitation method. 在反应过程中,加入的沉淀剂不是立刻与被沉淀组分发生反应,而是通过化学反应使沉淀剂在整个溶液中缓慢析出,使得构晶离子在整个溶液中分布比较均匀,所以沉淀物的颗粒均匀而致密,便于过滤和洗涤,产品粒度小、分布窄、团聚小。 During the reaction, the addition of precipitating agent is not immediately precipitated with the components of the reaction, but by chemical reaction slowly precipitated in the precipitating agent throughout the solution, the crystal structure so that the ion is more evenly distributed throughout the solution, the precipitate particles uniformly and dense, easy filtration and washing, the product of small particle size, narrow distribution, small agglomerates.

水解沉淀法是利用醇盐在水中能快速发生水解,形成氢氧化物沉淀,再经过滤、干燥、焙烧等过程来制备纳米粉体。 Hydrolysis precipitation method using an alkoxide hydrolyzable occurs rapidly in water to form a hydroxide precipitate, to prepare nano powder after filtration and drying, roasting process. 目前已经开发研制的可水解的金属醇盐已有30多种元素。 Metal alkoxide already developed hydrolyzable over 30 different elements. 该法的突出优点是反应条件温和,操作简单。 The advantage of this method is that the protruding mild reaction conditions, easy to operate. 但原料成本较高,其应用受到一定限制。 However, higher raw material costs, its application is limited.

以上三种沉淀法的关键是如何促进沉淀的生成速率,抑制沉淀的生长速率,防止沉淀的二次凝聚,人们已经总结出许多有效的成功的经验,并在继续探索新的方法,如《一种沉淀法连续制备超细纳米粉体工艺》(专利号申请号03113326),是将物料经计量加料装置按一定比例和速度同时向反应釜加料,在一定的温度、搅拌速率下,混合均匀发生成核后,迅速进入晶核成长管,在物料混合装置作用下向前推进,最终在晶核成长管的管端出口收集悬浮液经适当干燥后得超细纳米粉体。 These three key precipitation is how to promote the formation of precipitation rate, inhibit the growth rate of sedimentation, prevent the precipitation of secondary aggregation, many people have concluded that effective successful experiences, and continue to explore new approaches, such as "a precipitants continuous preparation of ultrafine nanometer powder technology "(Patent application No. 03113326), the material is metered feeding device by a certain percentage and velocity simultaneously fed to the kettle, at a constant temperature, stirring rate, the occurrence of mixed after nucleation, the nuclei grow rapidly into the tube, pushed forward under the action of the material mixing apparatus, the final ultrafine nano powder collected suspension was properly dried nuclei grow at the tube end of the outlet tube. 通过分别调整反应釜和晶核成长管的温度、反应物料的配比、加料速度、搅拌速率等控制因素来实现对晶粒大小的控制。 To achieve control of the grain size of the reactor and by adjusting the temperature of the growth factors controlling nucleation tube, the ratio of the reaction mass feed rate, stirring rate. 该发明可使沉淀反应连续进行,将沉淀反应中的成核过程和生长过程分开,成核、生长在相对稳定的环境下形成,生成的颗粒粒径可以得到调控,颗粒的单分散性好,分布窄,形貌差异小。 The invention allows continuous precipitation reaction, the precipitate nucleation and growth processes in separate reaction, nucleation, growth is formed in a relatively stable environment, the resulting particle size can be regulated, good monodisperse particles, narrow distribution, small differences in morphology. 《一种制备纳米粉体的技术》(专利号申请号01142821),采用如下步骤:将两种反应物通过加压后形成高速的流体,两种高速流体通过一定的角度进行瞬间混合,在混合过程中进行反应,生成固体料浆,将反应生成的固体料浆与反应物料分开,保持反应过程中反应物料的浓度一致,进而控制生成颗粒的粒径。 "A process for preparing nano powder technology" (Patent Application No. 01142821), the following steps: a high-speed fluid is formed by two reactants pressurized, instantaneous mixing of two high velocity fluid through a certain angle, the mixing during the course of the reaction slurry to form a solid, the reaction slurry and the resulting solid was separated from the reaction mass, keeping the concentration of the reaction mass during the reaction, and then control the particle size of the particles generated. 将反应得到的固体物质进行干燥后得到纳米粉体、或将干燥后的粉体进行焙烧得到纳米粉体。 After reaction solid material obtained was dried to obtain nano powder, or the powder after calcining the dried powder obtained nanometers. 该技术可适用于金属氧化物、金属氢氧化物、难溶性金属盐、非金属氧化物纳米粉体的制备。 This technique is applicable to metal oxide, metal hydroxide powder preparation, insoluble metal salts, non-metal oxide nanoparticles.

发明内容 SUMMARY

本发明的目的是针对上述现状,旨在提供一种能简便有效的抑制沉淀的生长速率和防止沉淀的二次凝聚的惰性浓盐介质法制备纳米粉体的方法。 Object of the present invention is directed to the above-described situation, it aims to provide a simple and effective to inhibit the growth rate of the precipitation method for preparing nano powder and concentrated hydrochloric medium precipitation method of preventing secondary aggregation inert.

本发明目的的实现方式为,惰性浓盐介质法制备纳米粉体的方法,先将要进行反应的物质分别溶解在一种或几种惰性盐组成的饱和溶液中,然后在搅拌下将反应物混合反应,将反应产生的产品沉淀物经过滤,用含有分散剂的洗涤剂洗尽惰性浓盐,经干燥得到纳米粉体材料或将反应产生的产品前驱体沉淀物,经过滤后进行干燥、粉碎、热分解,然后经冷却、洗涤、过滤、干燥得纳米粉体材料。 Implementation of the object of the present invention, for concentrated salt method for preparing an inert medium in the Preparation of a substance to be reacted are first dissolved in a saturated solution of one or more inert salts, and then the reaction mixture under stirring was the reaction, the reaction product resulting precipitate was filtered, concentrated salt washed away with a detergent containing an inert dispersant, and dried to obtain the nano powder material or a precursor reaction product precipitate was filtered and dried, pulverized thermal decomposition, then cooled, washed, filtered and dried to obtain nano-powder.

惰性浓盐中的盐是指在制备条件下不与反应物、产物以及溶剂发生反应,且在反应中能稳定存在,能溶解在反应进行的溶剂中的一类无机或有机盐中的一种或几种,当生成前驱体沉淀物时,该盐也不与前驱体沉淀物反应。 An inert salt concentration means salt does not react with the reactants, product, and a solvent under manufacturing conditions, and can stably exist in the reaction, one of a class capable of dissolving the organic or inorganic salts in a solvent in the reaction or more, to generate the precursor when the precipitate, the precursor of the salt does not precipitate the reaction.

本方法能简便有效的抑制沉淀的生长速率和防止沉淀的二次凝聚。 This simple method can effectively inhibit the growth rate of precipitation and the precipitation preventing secondary aggregation. 本方法可适用于金属氧化物、金属氢氧化物、难溶性金属盐、非金属氧化物等纳米粉体的制备。 The present method is applicable Preparation of Nano metal oxides, metal hydroxides, metal salts poorly soluble, non-metal oxide and the like in.

具体实施方式 Detailed ways

本发明是将要进行反应的物质分别溶解惰性的高浓度盐组成的溶液中,然后在搅拌下将反应物混合反应,将反应产生的产品沉淀物经过滤,用含有分散剂的洗涤剂洗尽惰性浓盐,经干燥得到纳米粉体材料,或将反应产生的产品前驱体沉淀物,经过滤后进行干燥、粉碎、热分解,然后经冷却、过滤洗涤、干燥得纳米粉体材料。 The present invention is a solution of the substances to be reacted separately dissolved in a high concentration of an inert salt thereof, followed by stirring the reactants in the reaction mixture, the reaction product resulting precipitate was filtered, washed with a detergent containing an inert dispersant washed away concentrated saline, and dried to obtain nano-powder, or the precursor reaction product precipitate was filtered and dried, pulverized, thermal decomposition, and then cooled, filtered, washed, and dried to obtain nano-powder.

本发明沉淀的生成方式,包括直接沉淀法、间接沉淀法、水解沉淀法。 Generating a precipitate of the present invention, including direct precipitation, indirect precipitation method, a hydrolysis precipitation.

惰性浓盐中的盐是指在制备条件下不与反应物、产物以及溶剂发生反应,且在反应中能稳定存在,能溶解在反应进行的溶剂中的一类无机或有机盐中的一种或几种。 An inert salt concentration means salt does not react with the reactants, product, and a solvent under manufacturing conditions, and can stably exist in the reaction, one of a class capable of dissolving the organic or inorganic salts in a solvent in the reaction or more.

在生成前驱体沉淀物的反应中,惰性浓盐中的盐是指在制备条件下不与反应物、前驱体沉淀物、产物以及溶剂发生反应,且在反应中能稳定存在,能溶解在反应进行的溶剂中的一类无机或有机盐中的一种或几种。 In the reaction precursor precipitate in an inert concentrated salt salt means that no reactant, precursor precipitate the product and solvent reacts under production conditions, and can stably exist in the reaction, it can be dissolved in the reaction a class of one or more organic or inorganic salt in a solvent.

上述的惰性浓盐中的盐为NaCl和KCl,也就是说以NaCl和KCl为首选。 The aforementioned salt concentration of an inert salt is NaCl and KCl, NaCl and KCl that is to say the first choice.

用本发明方法获得的产品包括金属氧化物、金属氢氧化物、难溶性金属盐、非金属氧化物等。 Product obtained by the method of the present invention include metal oxides, metal hydroxides, metal salts poorly soluble, non-metal oxide and the like.

下面举出本发明的实施例: Embodiments of the invention include the following:

例1:纳米碱式硫酸铜的制备:取50gCuSO4·5H2O溶于100ml水中,室温条件下逐步加入固体NaCl直至饱和,计消耗144gNaCl。 Example 1: Preparation of Nano basic copper sulfate: Take 50gCuSO4 · 5H2O was dissolved in 100ml of water at room temperature was gradually added solid NaCl until saturated, the consumed 144gNaCl. 另取8gNaOH溶于100ml水中,冷却至室温后也逐步加入固体NaCl直至饱和,计消耗35gNaCl。 Another 8gNaOH After dissolved in 100ml of water, cooled to room temperature gradually added solid NaCl until saturated, the consumed 35gNaCl. 充分搅拌下将NaOH溶液加入到CuSO4溶液中,加至反应计量时,得到蓝绿色碱式硫酸铜纳米浆。 When stirring sufficiently NaOH solution was added to a solution of CuSO4, was added to the reaction measurement, basic copper sulfate to give a blue-green slurry nanometers. 真空抽滤,滤饼用浓度为0.3%多聚磷酸钠的水溶液洗涤3~4次,得到碱式硫酸铜为主体的纳米浆,碱式硫酸铜粒径约40nm。 Vacuum filtration, the filter cake was washed with an aqueous solution of 0.3% concentration of sodium tripolyphosphate 3 to 4 times to obtain basic copper sulfate pulp as the main nanometers, basic copper sulfate particle diameter of about 40nm. 如滤饼最后用无水乙醇洗涤2次,于50℃下真空干燥3小时,则得到碱式硫酸铜纳米粉体。 The final filter cake was washed with absolute ethanol twice, and dried in vacuo at 50 ℃ 3 hours, to obtain basic copper sulfate nano powder.

例2纳米氧化锌的制备:取无水21.2gNa2CO3,加蒸馏水100ml搅拌溶解后,逐步加入26.5g固体氯化钠使其溶解,制成30℃时的饱和溶液,称取27.2gZnCl2,加水100ml溶解,逐步加入58g固体氯化钠制成30℃时的饱和溶液。 Nano zinc oxide prepared in Example 2: anhydrous 21.2gNa2CO3, after adding 100ml distilled water and dissolved with stirring, solid sodium chloride was gradually added to dissolve 26.5g, prepared saturated solution at 30 ℃, weighed 27.2gZnCl2, dissolved water 100ml , when a saturated solution of sodium chloride was gradually added 58g of solid formed 30 ℃. 剧烈搅拌下将Na2CO3溶液加入到ZnCl2溶液中,反应完毕后过滤,前驱体于105℃下干燥,烘干后粉碎,置入马弗炉中,于300℃温度下灼烧3小时,取出用浓度为0.3%多聚磷酸钠的水溶液浸泡并洗涤3~4遍,溶解去除氯化钠,最后用无水乙醇洗涤2遍,沉淀物于50℃下真空干燥3小时,即得到疏松的纳米ZnO粉体,含量98.5%,粒度15~20nm。 Na2CO3 solution under vigorous stirring to the ZnCl2 solution was added. After completion of the reaction was filtered, the precursor was dried at 105 ℃, dried and pulverized, placed in a muffle furnace at a temperature of burning 300 ℃ 3 hours, removed by concentration soaking an aqueous solution of 0.3% sodium polyphosphate and washed 3 to 4 times, dissolve and remove sodium chloride, and finally washed with absolute ethanol 2 times, the precipitate was vacuum dried for 3 hours at 50 deg.] C under obtain nano ZnO loose powder body content of 98.5%, particle size of 15 ~ 20nm.

例3纳米Sb2O3粉体的制备:室温下配制NaCl的饱和溶液1500ml备用,另配制3‰的三聚磷酸钠分散液备用。 Example 3 Preparation of Sb2O3 powder: Alternate preparation 1500ml NaCl saturated solution at room temperature, another formulation of sodium tripolyphosphate 3 ‰ dispersion liquid reserve.

称取106g硫酸亚锑置于2000ml的烧杯中,搅拌下缓缓加入饱和氯化钠溶液直至1500ml,继续搅拌30分钟,使之水解完全。 Weigh 106g of antimony sulfite 2000ml beaker and stirred slowly adding saturated sodium chloride solution until 1500ml, stirring was continued for 30 minutes to complete the hydrolysis. 离心分离,沉淀转入2000ml烧杯中,加入3‰的三聚磷酸钠分散剂约300ml,升温至沸腾,分次加入30%的氨水142ml,并保温至Sb2O3生成完全。 Centrifugation, precipitated into 2000ml beaker, 3 ‰ tripolyphosphate dispersants about 300ml, was heated to boiling, was added in 142ml of 30% aqueous ammonia, and incubated to generate a full Sb2O3. 离心沉降,用浓度为0.3%多聚磷酸钠的水溶液洗涤沉淀3~4次。 Centrifugal sedimentation, and washed with an aqueous solution of a concentration of 0.3% sodium polyphosphate precipitate was 3 to 4 times. 最后用甲醇洗涤2次,在50-60℃温度范围内真空干燥即得到Sb2O3纳米晶,粒径20~30nm。 Finally washed twice with methanol, and dried in vacuo to obtain nanocrystals Sb2O3 at a temperature in the range of 50-60 deg.] C, particle diameter of 20 ~ 30nm.

例4纳米Mg(OH)2粉体的制备:称取101.6gMgCl2·6H2O于1000mL烧杯中,加入去离子水500mL,搅拌下添加氯化钠至饱和备用,计消耗氯化钠180g。 Example 4 Preparation of nano-Mg (OH) 2 powder: Weigh 101.6gMgCl2 · 6H2O in 1000mL beaker, was added 500 mL of deionized water, was added under stirring to a saturated aqueous sodium chloride standby, the consumed sodium chloride 180g. 量取17mol/L的浓氨水76mL于2000mL烧杯中,稀释至300mL,添加氯化钠至饱和,计消耗氯化钠114g,将变速搅拌机搅拌桨插入并调整好高度和搅拌速度,升温到60℃左右,在强烈搅拌下将氯化镁溶液徐徐转入氨水中,转移完毕后强烈搅拌60min,然后继续在此温度下搅拌1小时。 Amount of 17mol / L of concentrated aqueous ammonia in 76mL 2000mL beaker, diluted to 300 mL, was added sodium chloride to saturation, the consumed sodium chloride 114g, the shift paddle stirrer is inserted and adjust the height and the stirring speed was raised to 60 deg.] C left, under vigorous stirring slowly transferred into aqueous ammonia chloride solution, after the transfer is complete vigorous stirring 60min, and then stirring was continued at this temperature for 1 hour. 提高并保持温度至90℃缓慢搅拌2小时,高速离心分离,并以含0.3%硬脂酸、pH值为11的稀氨水搅拌洗涤并离心分离,如此重复3次。 And maintaining the temperature increase to 90 deg.] C was slowly stirred for 2 hours, high-speed centrifugation, and containing 0.3% stearic acid, pH = 11 with dilute aqueous ammonia was stirred and centrifuged and washed, so repeated 3 times. 最后用无水乙醇洗涤2次,转入蒸发皿中,置于真空干燥箱中于50℃下真空干燥3小时,得到疏松的白色Mg(OH)2纳米粉体,粒径约30nm。 Finally washed with absolute ethanol twice, transferred to an evaporating dish and placed in a vacuum oven and dried in vacuum for 3 h at 50 deg.] C, the resulting loose white Mg (OH) 2 nano powder, particle size of about 30nm.

Claims (4)

1.惰性浓盐介质法制备纳米粉体的方法,其特征在于先将要进行反应的物质分别溶解在一种或几种惰性盐组成的饱和溶液中,然后在搅拌下将反应物混合反应,将反应产生的产品沉淀物经过滤,用含有分散剂的洗涤剂洗尽惰性浓盐,经干燥得到纳米粉体材料或将反应产生的产品前驱体沉淀物,经过滤后进行干燥、粉碎、热分解,然后经冷却、洗涤、过滤、干燥得纳米粉体材料,惰性浓盐中的盐是指在制备条件下不与反应物、产物以及溶剂发生反应,且在反应中能稳定存在,能溶解在反应进行的溶剂中的一类无机或有机盐中的一种或几种,当生成前驱体沉淀物时,该盐也不与前驱体沉淀物反应。 1. A method inert medium salt concentration Nanoparticles Prepared characterized in that the material to be reacted are first dissolved in a saturated solution of one or more inert salts, and then the reaction was stirred under mixing of the reaction, the reaction product resulting precipitate was filtered, washed out with a detergent containing a dispersant concentration of an inert salt, and dried to obtain the nano powder material or a precursor reaction product precipitate was filtered and dried, pulverized, thermal decomposition then cooled, washed, filtered and dried to obtain nano-powder, salt concentration of an inert salt means does not react with the reactants, product, and a solvent under manufacturing conditions, and can stably exist in the reaction, it can be dissolved in reaction solvent in a class of one or more inorganic or organic salts, when generating precursor precipitate the salt does not precipitate the reaction with the precursor.
2.根据权利要求1所述的惰性浓盐介质法制备纳米粉体的方法,其特征在于沉淀的生成方式包括直接沉淀法、间接沉淀法和水解沉淀法。 2. The method of Nanoparticles Prepared concentrated hydrochloric SYSTEM inert medium according to claim 1, characterized in that the formation of a precipitate which include direct precipitation method, precipitation method and the indirect hydrolysis precipitation.
3.根据权利要求1所述的惰性浓盐介质法制备纳米粉体的方法,其特征在于惰性浓盐中的盐为NaCl和KCl。 3. The method of Nanoparticles Prepared concentrated hydrochloric SYSTEM inert medium according to claim 1, characterized in that an inert salt is in concentrated hydrochloric NaCl and KCl.
4.根据权利要求1所述的惰性浓盐介质法制备纳米粉体的方法,其特征在于产品包括金属氧化物、金属氢氧化物、难溶性金属盐和非金属氧化物。 4. The method of Nanoparticles Prepared concentrated hydrochloric SYSTEM inert medium according to claim 1, characterized in that the product comprises metal oxides, metal hydroxides, metal and non-metal oxides insoluble.
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