CN105776270B - The preparation method of nano-aluminum hydroxide in a kind of pelite - Google Patents
The preparation method of nano-aluminum hydroxide in a kind of pelite Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002386 leaching Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000012535 impurity Substances 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract 4
- 238000005406 washing Methods 0.000 claims abstract 4
- 238000006243 chemical reaction Methods 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 5
- 229910001679 gibbsite Inorganic materials 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 2
- FLTRNWIFKITPIO-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe] FLTRNWIFKITPIO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims 2
- 238000000605 extraction Methods 0.000 claims 2
- 229910001388 sodium aluminate Inorganic materials 0.000 claims 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims 1
- 239000000920 calcium hydroxide Substances 0.000 claims 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims 1
- 239000000347 magnesium hydroxide Substances 0.000 claims 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000006396 nitration reaction Methods 0.000 claims 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims 1
- 239000011435 rock Substances 0.000 abstract description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 abstract description 10
- 238000000746 purification Methods 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 description 9
- 239000011707 mineral Substances 0.000 description 9
- 239000011575 calcium Substances 0.000 description 7
- 229910018626 Al(OH) Inorganic materials 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910019440 Mg(OH) Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 229910001648 diaspore Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000007785 strong electrolyte Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/24—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with nitric acid or nitrogen oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明公开了一种铝质岩中纳米氢氧化铝的制备方法，将铝质岩磨细至74um以下，再烘干后与一定浓度的盐酸与硝酸按一定比例混合，置于水浴锅中机械搅拌浸出，控制浸出时间、温度，浸出液冷却后过滤，所得滤液缓慢加入氢氧化钠溶液调节pH除杂，分步过滤后得到纯的铝盐，再通入CO2后得到氢氧化铝沉淀，再过滤洗涤干燥得到纳米氢氧化铝制品。本发明的制备方法制备效率高，浸出彻底，产量和利用率高，纯度高，通过本发明的方法用盐酸和硝酸混合液浸出铝质岩，经过除杂，净化，提纯等工序，可获得质量较好纳米氢氧化铝粉体，既能获得较好的经济效益，同时又使铝质岩资源得到综合利用。
The invention discloses a method for preparing nano-aluminum hydroxide in aluminum rocks. The aluminum rocks are ground to a fineness below 74um, dried, mixed with certain concentrations of hydrochloric acid and nitric acid in a certain proportion, placed in a water bath, and mechanically prepared. Stir leaching, control the leaching time and temperature, filter the leaching liquid after cooling, slowly add sodium hydroxide solution to the obtained filtrate to adjust the pH to remove impurities, obtain pure aluminum salt after step-by-step filtration, and then pass in CO2 to obtain aluminum hydroxide precipitation, and then filter Washing and drying to obtain nano aluminum hydroxide products. The preparation method of the present invention has high preparation efficiency, thorough leaching, high yield and utilization rate, and high purity. Through the method of the present invention, the aluminum rock is leached with a mixed solution of hydrochloric acid and nitric acid, and after impurity removal, purification, purification and other processes, quality can be obtained. High-quality nano-aluminum hydroxide powder can not only obtain good economic benefits, but also make comprehensive utilization of aluminum rock resources.
Description
技术领域technical field
本发明属于铝质岩中纳米氢氧化铝粉体制备技术领域，涉及一种铝质岩中纳米氢氧化铝的制备方法。The invention belongs to the technical field of preparing nanometer aluminum hydroxide powder in aluminous rocks, and relates to a method for preparing nanometer aluminum hydroxide in aluminous rocks.
背景技术Background technique
铝质岩是含铝的氢氧化物，我国铝质岩主要含一水硬铝石和粘土矿物共生，另外还含有硅质和锐钛矿等。而随着资源匮乏加剧和人们环保意识的加强，铝质岩综合利用越来越受到广泛的关注。铝质岩中主要矿物是一水硬铝石和粘土矿物，含有较高是Al2O3，利用铝质岩与混酸浸出后再除杂可得到纳米氢氧化铝粉体，所得纳米氢氧化铝粉体可广泛用于各种阻燃剂和无机填充剂等。Aluminous rocks are hydroxides containing aluminum. In my country, aluminous rocks mainly contain diaspore and clay minerals, and also contain siliceous and anatase. With the increasing scarcity of resources and the strengthening of people's awareness of environmental protection, the comprehensive utilization of alumina rock has attracted more and more attention. The main minerals in the alumina rock are diaspore and clay minerals, and the content is relatively high. Body can be widely used in various flame retardants and inorganic fillers.
纳米氢氧化铝目前主要采用固相法、气相法和液相法来制备，但是固相法需要很高的温度，因此设备要求高，设备购买成本贵；液相法是常用的制备纳米氢氧化铝粉体的方法，但是液相法容易引入新杂质，导致制备的纳米氢氧化铝纯度不高；而气相法，在收集时难以搜集和产率低。At present, nano-aluminum hydroxide is mainly prepared by solid-phase method, gas-phase method and liquid-phase method, but the solid-phase method requires high temperature, so the equipment requirements are high, and the equipment purchase cost is expensive; the liquid-phase method is commonly used to prepare nano-hydroxide The method of aluminum powder, but the liquid phase method is easy to introduce new impurities, resulting in low purity of the prepared nano aluminum hydroxide; and the gas phase method is difficult to collect and the yield is low when collecting.
发明内容Contents of the invention
本发明要解决的技术问题是：提供一种铝质岩中纳米氢氧化铝的制备方法，制备效率高，浸出彻底，产量和利用率高，纯度高，制备简单，制备成本低，以解决现有技术中存在的问题。The technical problem to be solved by the present invention is to provide a method for preparing nano-aluminum hydroxide in aluminum rock, which has high preparation efficiency, thorough leaching, high yield and utilization rate, high purity, simple preparation, and low preparation cost, so as to solve the current There are problems in the technology.
本发明采取的技术方案为：The technical scheme that the present invention takes is:
一种铝质岩中纳米氢氧化铝的制备方法，该方法包括以下步骤：A method for preparing nanometer aluminum hydroxide in aluminum rock, the method comprising the following steps:
（1）以铝质岩为原料，将其用颚式破碎机破碎后，再用球磨机将破碎的矿粉碎粒磨制粒度74um以下；(1) Use alumina rock as raw material, crush it with a jaw crusher, and then use a ball mill to grind the crushed ore to a particle size below 74um;
（2）将步骤（1）中磨制的矿粉样品烘干后，将盐酸和硝酸的混合溶液与烘干的矿粉按比例置于水浴锅中搅拌，浸出所涉及的化学反应有：(2) After drying the mineral powder sample ground in step (1), put the mixed solution of hydrochloric acid and nitric acid and the dried mineral powder in proportion to the water bath and stir. The chemical reactions involved in leaching are as follows:
Al2O3+6HCl=2AlCl3+3H2OAl 2 O 3 +6HCl=2AlCl 3 +3H 2 O
Al2O3+6HNO3=2Al(NO3)3+3H2OAl 2 O 3 +6HNO 3 =2Al(NO 3 ) 3 +3H 2 O
Fe2O3+6HCl=2FeCl3+3H2OFe 2 O 3 +6HCl=2FeCl 3 +3H 2 O
Fe2O3+6HNO3=2Fe(NO3)3+3H2O；Fe 2 O 3 +6HNO 3 =2Fe(NO 3 ) 3 +3H 2 O;
（3）将所得浸出液过滤、洗涤，滤液加入氢氧化钠溶液调节pH除杂，除杂所涉及的化学反应有：(3) Filter and wash the resulting leachate, add sodium hydroxide solution to the filtrate to adjust the pH to remove impurities, and the chemical reactions involved in the removal of impurities are:
3OH-+Fe3+=Fe(OH)3↓ Mg2++3OH-=Mg（OH）2↓3OH - +Fe 3+ =Fe(OH)3↓ Mg 2+ +3OH - =Mg(OH) 2 ↓
Ca2++OH-=Ca(OH)2↓ Al(OH)3+NaOH(过量)=NaAlO2+H2O；Ca 2+ +OH - =Ca(OH) 2 ↓ Al(OH) 3 +NaOH (excess)=NaAlO 2 +H 2 O;
（4）除杂后所得滤液中通入CO2得到氢氧化铝沉淀，所涉及的化学反应有：(4) Pass CO into the obtained filtrate after removing impurities to obtain aluminum hydroxide precipitation. The chemical reactions involved are:
NaAlO2 + CO2 + 2 H2O = Al(OH)3 ↓+ NaHCO3；NaAlO 2 + CO 2 + 2 H 2 O = Al(OH) 3 ↓ + NaHCO 3 ;
（5）所得Al(OH)3沉淀浓缩过滤得到纳米氢氧化铝制品。(5) The resulting Al(OH) 3 precipitate is concentrated and filtered to obtain nano-aluminum hydroxide products.
上述铝质岩中Al2O3含量为30%。The content of Al 2 O 3 in the above alumina rock is 30%.
上述步骤（2）中浸出时所用混合液是体积分数20%浓盐酸和20%浓硝酸，液固比即混酸体积与矿粉质量比为4：1。The mixed solution used for leaching in the above step (2) is 20% concentrated hydrochloric acid and 20% concentrated nitric acid by volume fraction, and the liquid-solid ratio, that is, the mass ratio of mixed acid volume to mineral powder is 4:1.
上述步骤（2）中的浸出时间2h，浸出温度80℃。The leaching time in the above step (2) is 2 hours, and the leaching temperature is 80°C.
上述步骤（3）中氢氧化钠溶液pH为13，缓慢加入氢氧化钠溶液调节pH为4.5时过滤洗涤，再向滤液中缓慢加入氢氧化钠溶液调节pH为13时过滤洗涤。The pH of the sodium hydroxide solution in the above step (3) is 13, slowly add sodium hydroxide solution to adjust the pH to 4.5, filter and wash, then slowly add sodium hydroxide solution to the filtrate to adjust the pH to 13, filter and wash.
本发明的有益效果：与现有技术相比，本发明效果如下：Beneficial effects of the present invention: compared with the prior art, the present invention has the following effects:
（1）铝质岩磨细后增大比表面积使其反应充分彻底，反应更快，效率更高，且有利于铝质岩中Al2O3浸出更彻底，利于提高纳米氢氧化铝的产率，以及杂质（如铁、钙和镁等）的浸出彻底，利于后续杂质的沉淀，让制得的纳米氢氧化铝的纯度更高；(1) After the alumina rock is ground, the specific surface area is increased to make the reaction fully and completely, the reaction is faster and the efficiency is higher, and it is conducive to the more thorough leaching of Al 2 O 3 in the alumina rock, which is conducive to improving the production of nano-aluminum hydroxide The efficiency, and the leaching of impurities (such as iron, calcium and magnesium, etc.) are thorough, which is conducive to the precipitation of subsequent impurities, so that the purity of the prepared nano-aluminum hydroxide is higher;
（2）所用盐酸和硝酸混合溶液为强电解质，采用体积分数为20%浓盐酸和20%浓硝酸，液固比即混合溶液体积与矿粉质量比为4：1的配比下，能更好的浸出一水铝石中的Al2O3以及杂质；(2) The mixed solution of hydrochloric acid and nitric acid used is a strong electrolyte, and the volume fraction is 20% concentrated hydrochloric acid and 20% concentrated nitric acid. The liquid-solid ratio, that is, the ratio of the volume of the mixed solution to the mass ratio of the mineral powder is 4:1. Good leaching of Al 2 O 3 and impurities in gibbsite;
（3）所用硝酸溶液为强氧化剂，能直接将铝质岩中部分二价铁氧化成三价铁，免去了后续氧化的工序，使其减少后期氧化步骤，缩短了制备时间，效率更高，也提高了除杂的效果；(3) The nitric acid solution used is a strong oxidant, which can directly oxidize part of the divalent iron in the alumina rock to ferric iron, eliminating the need for subsequent oxidation processes, reducing the post-oxidation steps, shortening the preparation time, and improving efficiency , also improves the effect of impurity removal;
（4）温度在80℃时，离子迁移速度加快，使其化学反应速率快，使其浸出加快和彻底，大大提高浸出效率；(4) When the temperature is 80°C, the ion migration speed is accelerated, making the chemical reaction rate fast, making the leaching speed up and thorough, and greatly improving the leaching efficiency;
（5）时间2小时使其浸出彻底；(5) Time 2 hours to make it leaching thoroughly;
（6）浸出后用pH为13的氢氧化钠溶液除杂，调节pH为4.5时过滤洗涤除铁，再向滤液中缓慢加入氢氧化钠溶液调节pH为13时过滤洗涤除钙、镁，除杂完全，让制得的纳米氢氧化铝更纯；(6) After leaching, use a sodium hydroxide solution with a pH of 13 to remove impurities. When the pH is adjusted to 4.5, filter and wash to remove iron, and then slowly add sodium hydroxide solution to the filtrate to adjust the pH to 13. When the pH is 13, filter and wash to remove calcium and magnesium. The impurity is complete, so that the prepared nano-aluminum hydroxide is more pure;
综上所述：通过本发明的方法用盐酸和硝酸混合液浸出铝质岩，经过除杂，净化，提纯等工序，可获得质量较好纳米氢氧化铝粉体，既能获得较好的经济效益，同时又使铝质岩资源得到综合利用，另外无需购买高端的设备就可实现制备，设备购买成本更低。To sum up: the aluminum rock is leached with the mixed solution of hydrochloric acid and nitric acid through the method of the present invention, and through the processes of impurity removal, purification and purification, nano aluminum hydroxide powder with better quality can be obtained, which can obtain better economical At the same time, the aluminous rock resources can be comprehensively utilized. In addition, the preparation can be realized without purchasing high-end equipment, and the equipment purchase cost is lower.
附图说明Description of drawings
图1为本发明的制备工艺流程示意图。Figure 1 is a schematic diagram of the preparation process of the present invention.
具体实施方式Detailed ways
下面结合附图及具体的实施例对本发明进行进一步介绍。The present invention will be further introduced below in conjunction with the accompanying drawings and specific embodiments.
实施例1：一种铝质岩中纳米氢氧化铝的制备方法，该方法包括以下步骤：Embodiment 1: a kind of preparation method of nanometer aluminum hydroxide in aluminum rock, this method comprises the following steps:
（1）以铝质岩为原料，Al2O3含量为30%，将其用颚式破碎机破碎后，再用球磨机将破碎的矿粉碎粒磨制粒度74um以下，铝质岩磨细后增大比表面积使其反应充分彻底，反应更快，效率更高，且有利于铝质岩中Al2O3浸出更彻底；(1) Use alumina rock as raw material, with Al 2 O 3 content of 30%, crush it with a jaw crusher, and then use a ball mill to grind the crushed ore to a particle size below 74um. After the alumina rock is ground Increase the specific surface area to make the reaction fully and completely, the reaction is faster, the efficiency is higher, and it is conducive to the more thorough leaching of Al 2 O 3 in the alumina rock;
（2）将步骤（1）中磨制的矿粉样品烘干后，将盐酸和硝酸的混合溶液与烘干的矿粉按比例置于水浴锅中搅拌，所用混合液是体积分数20%浓盐酸和20%浓硝酸，液固比即混酸体积与矿粉质量比为4：1，浸出时间2h，浸出温度80℃，采用体积分数为20%浓盐酸和20%浓硝酸，液固比即混合溶液体积与矿粉质量比为4：1的配比下，能更好的浸出一水铝石中的Al2O3，温度在80℃时，离子迁移速度加快，使其化学反应速率快，使其浸出加快和彻底，大大提高浸出效率；(2) After drying the mineral powder sample ground in step (1), put the mixed solution of hydrochloric acid and nitric acid and the dried mineral powder in a water bath in proportion to stir, and the mixed solution used is 20% concentrated by volume fraction Hydrochloric acid and 20% concentrated nitric acid, the liquid-solid ratio, that is, the mass ratio of the mixed acid volume to the mineral powder, is 4:1, the leaching time is 2 hours, and the leaching temperature is 80°C. The volume fraction is 20% concentrated hydrochloric acid and 20% concentrated nitric acid. The liquid-solid ratio is When the ratio of the volume of the mixed solution to the mass of the mineral powder is 4:1, the Al 2 O 3 in the gibbsite can be better leached. When the temperature is 80°C, the ion migration speed is accelerated, making the chemical reaction rate fast , so that the leaching is accelerated and thorough, and the leaching efficiency is greatly improved;
步骤（2）中浸出所涉及的化学反应有：The chemical reactions involved in leaching in step (2) are:
Al2O3+6HCl=2AlCl3+3H2OAl 2 O 3 +6HCl=2AlCl 3 +3H 2 O
Al2O3+6HNO3=2Al(NO3)3+3H2OAl 2 O 3 +6HNO 3 =2Al(NO 3 ) 3 +3H 2 O
Fe2O3+6HCl=2FeCl3+3H2OFe 2 O 3 +6HCl=2FeCl 3 +3H 2 O
Fe2O3+6HNO3=2Fe(NO3)3+3H2O；Fe 2 O 3 +6HNO 3 =2Fe(NO 3 ) 3 +3H 2 O;
（3）将所得浸出液过滤、洗涤，滤液加入氢氧化钠溶液调节pH除杂，氢氧化钠溶液pH为13，缓慢加入氢氧化钠溶液调节pH为4.5时过滤洗涤除铁，再向滤液中缓慢加入氢氧化钠溶液调节pH为13时过滤洗涤除钙、镁；(3) Filter and wash the obtained leaching solution, add sodium hydroxide solution to the filtrate to adjust the pH to remove impurities, the pH of the sodium hydroxide solution is 13, slowly add sodium hydroxide solution to adjust the pH to 4.5, filter and wash to remove iron, and then slowly add to the filtrate Add sodium hydroxide solution to adjust the pH to 13, filter and wash to remove calcium and magnesium;
步骤（3）中除杂所涉及的化学反应有：The chemical reactions involved in the removal of impurities in step (3) are:
3OH-+Fe3+=Fe(OH)3↓ Mg2++3OH-=Mg（OH）2↓3OH - +Fe 3+ =Fe(OH) 3 ↓ Mg 2+ +3OH - =Mg(OH) 2 ↓
Ca2++OH-=Ca(OH)2↓ Al(OH)3+NaOH(过量)=NaAlO2+H2O；Ca 2+ +OH - =Ca(OH) 2 ↓ Al(OH) 3 +NaOH (excess)=NaAlO 2 +H 2 O;
（4）除杂后所得滤液中通入CO2得到氢氧化铝沉淀；(4) CO2 is introduced into the filtrate obtained after removing impurities to obtain aluminum hydroxide precipitation;
步骤（4）中所涉及的化学反应有：The chemical reactions involved in step (4) are:
NaAlO2 + CO2 + 2 H2O = Al(OH)3 ↓+ NaHCO3 ；NaAlO 2 + CO 2 + 2 H 2 O = Al(OH) 3 ↓ + NaHCO 3 ;
（5）所得Al(OH)3沉淀浓缩过滤得到纳米氢氧化铝制品。(5) The resulting Al(OH) 3 precipitate is concentrated and filtered to obtain nano-aluminum hydroxide products.
综上所述：通过本发明的方法用盐酸和硝酸混合液浸出铝质岩，经过除杂，净化，提纯等工序，可获得质量较好纳米氢氧化铝粉体，既能获得较好的经济效益，同时又使铝质岩资源得到综合利用，另外无需购买高端的设备就可实现制备，设备购买成本更低。To sum up: the aluminum rock is leached with the mixed solution of hydrochloric acid and nitric acid through the method of the present invention, and through the processes of impurity removal, purification and purification, nano aluminum hydroxide powder with better quality can be obtained, which can obtain better economical At the same time, the aluminous rock resources can be comprehensively utilized. In addition, the preparation can be realized without purchasing high-end equipment, and the equipment purchase cost is lower.
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内，因此，本发明的保护范围应以所述权利要求的保护范围为准。The above is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Anyone skilled in the art can easily think of changes or substitutions within the technical scope disclosed in the present invention. Should be covered within the protection scope of the present invention, therefore, the protection scope of the present invention should be based on the protection scope of the claims.
Claims (2)
- A kind of 1. preparation method of nano-aluminum hydroxide in pelite, it is characterised in that：This method comprises the following steps：（1）Using pelite as raw material, after it is used into jaw crushing crusher machine, then with ball mill broken miberal powder particle is ground into grain Less than 74 μm of degree；（2）By step（1）In grind miberal powder sample drying after, by the mixed solution of hydrochloric acid and nitric acid with drying miberal powder press than Example, which is placed in water-bath, to be stirred, and leaching involved chemical reaction has：Al2O3+6HCl=2AlCl3+3H2OAl2O3+6HNO3=2Al(NO3)3+3H2OFe2O3+6HCl=2FeCl3+3H2OFe2O3+6HNO3=2Fe(NO3)3+3H2O；Step（2）Mixed liquor used is the concentrated hydrochloric acid of volume fraction 20% and 20% concentrated nitric acid during middle leaching, and liquid-solid ratio is nitration mixture volume It is 4 with powdered ore quality ratio：1；Step（2）In extraction time 2h, 80 DEG C of extraction temperature；（3）By the filtering of gained leachate, washing, filtrate adds sodium hydroxide solution regulation pH removal of impurities, and clean involved chemistry Reaction has：3OH-+Fe3+=Fe(OH)3↓ Mg2++3OH-=Mg（OH）2↓Ca2++OH-=Ca(OH)2↓ Al(OH)3+NaOH=NaAlO2+H2O,Wherein Al (OH)3When being reacted with NaOH, NaOH dosages are excessive；Step（3）Middle sodium hydroxide solution pH is 13, is slowly added to filtration washing when sodium hydroxide solution regulation pH is 4.5, then Filtration washing when sodium hydroxide solution regulation pH is 13 is slowly added into filtrate；（4）After removal of impurities CO is passed through in gained filtrate2Aluminum hydroxide precipitation is obtained, involved chemical reaction has：NaAlO2 + CO2 + 2 H2O = Al(OH)3 ↓+ NaHCO3；（5）Gained Al (OH)3Precipitation concentration is filtrated to get nano-aluminum hydroxide product.
- 2. the preparation method of nano-aluminum hydroxide in a kind of pelite according to claim 1, it is characterised in that：Pelite Middle Al2O3Content is 30%.
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