CN105692673A - Preparation method of potassium alum - Google Patents
Preparation method of potassium alum Download PDFInfo
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- CN105692673A CN105692673A CN201410701042.8A CN201410701042A CN105692673A CN 105692673 A CN105692673 A CN 105692673A CN 201410701042 A CN201410701042 A CN 201410701042A CN 105692673 A CN105692673 A CN 105692673A
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- potassium alum
- potassium
- mother liquor
- crystal
- crystallization mother
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- 229940050271 potassium alum Drugs 0.000 title claims abstract description 37
- 235000011126 aluminium potassium sulphate Nutrition 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 title abstract description 29
- 239000013078 crystal Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims abstract description 8
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 8
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 6
- 229940103272 aluminum potassium sulfate Drugs 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims description 17
- 230000008025 crystallization Effects 0.000 claims description 17
- 239000012452 mother liquor Substances 0.000 claims description 12
- GNHOJBNSNUXZQA-UHFFFAOYSA-J potassium aluminium sulfate dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GNHOJBNSNUXZQA-UHFFFAOYSA-J 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000012141 concentrate Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 229910052934 alunite Inorganic materials 0.000 description 3
- 239000010424 alunite Substances 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- KPZTWMNLAFDTGF-UHFFFAOYSA-D trialuminum;potassium;hexahydroxide;disulfate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KPZTWMNLAFDTGF-UHFFFAOYSA-D 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 229910002566 KAl(SO4)2·12H2O Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000008395 clarifying agent Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052600 sulfate mineral Inorganic materials 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明具体涉及一种钾明矾的制备方法。其技术方案是：先将硫酸铝、硫酸钾和水在80~100℃条件下混合、反应，再蒸发浓缩，然后加晶种、冷却降温结晶，制得钾明矾晶体。本发明生产的钾明矾晶体具有粒度分布均匀、平均粒径大的特点。The invention specifically relates to a preparation method of potassium alum. The technical scheme is as follows: first mix and react aluminum sulfate, potassium sulfate and water at 80-100°C, then evaporate and concentrate, then add crystal seeds, cool down and crystallize to obtain potassium alum crystals. The potassium alum crystal produced by the invention has the characteristics of uniform particle size distribution and large average particle size.
Description
技术领域 technical field
本发明属于工业结晶技术领域，具体涉及一种钾明矾的制备方法。 The invention belongs to the technical field of industrial crystallization, and in particular relates to a preparation method of potassium alum.
背景技术 Background technique
钾明矾，KAl(SO4)2 ·12H2O，俗称明矾，十二水硫酸铝钾等。钾明矾是含有结晶水的硫酸钾和硫酸铝的复盐，无色立方晶体，溶于水，不溶于乙醇。钾明矾有抗菌、收敛作用等，可用做中药；还可用于制备铝盐、发酵粉、油漆、澄清剂、媒染剂、造纸、防水剂等。日常生活中，钾明矾还可用于净水以及食用膨胀剂。 Potassium alum, KAl(SO 4 ) 2 · 12H 2 O, commonly known as alum, potassium aluminum sulfate dodecahydrate, etc. Potassium alum is a double salt of potassium sulfate and aluminum sulfate containing crystal water, colorless cubic crystal, soluble in water, insoluble in ethanol. Potassium alum has antibacterial and astringent effects, and can be used as traditional Chinese medicine; it can also be used to prepare aluminum salts, baking powder, paints, clarifying agents, mordants, papermaking, waterproofing agents, etc. In daily life, potassium alum can also be used for water purification and food expansion agent.
钾明矾的工业生产常采用明矾石法和重结晶法。明矾石是非水溶性的钾铝硫酸盐矿物，先要对其进行碎粉、焙烧(脱水、热解或还原热解)，再通过湿法浸取(酸法、碱法或酸碱联合法)，最后通过结晶技术制备钾明矾。明矾石法制备钾明矾具有工艺路线复杂、生产周期长、能耗高、三废产量大、产品质量低、矿石资源利用率低等缺点。重结晶法是以工业钾明矾或含有K+、Al3+以及SO4 2-的物料为原料，通过重结晶制备高纯度钾明矾。 The industrial production of potassium alum often adopts the alunite method and recrystallization method. Alunite is a water-insoluble potassium-aluminum sulfate mineral. It must first be pulverized and roasted (dehydration, pyrolysis or reduction pyrolysis), and then wet leached (acid method, alkali method or acid-base combined method) , and finally potassium alum was prepared by crystallization technique. The preparation of potassium alum by the alunite method has the disadvantages of complex process route, long production cycle, high energy consumption, large output of three wastes, low product quality, and low utilization rate of ore resources. The recrystallization method uses industrial potassium alum or materials containing K + , Al 3+ and SO 4 2- as raw materials to prepare high-purity potassium alum through recrystallization.
发明内容 Contents of the invention
本发明旨在提供一种产品平均粒度大的钾明矾制备方法。 The invention aims to provide a method for preparing potassium alum with a large product average particle size.
为实现上述目的，本发明采用的技术方案的具体步骤是： In order to achieve the above object, the concrete steps of the technical solution adopted in the present invention are:
步骤一、先将硫酸铝、硫酸钾和水按下述配比进行配料，其中：硫酸铝为20~25wt%，硫酸钾为10~13wt%，其余为水；再在常压、80~100℃和150～500r/min的转速条件下搅拌1~2h制得钾明矾结晶母液Ⅰ； Step 1, first mix aluminum sulfate, potassium sulfate and water according to the following ratio, wherein: aluminum sulfate is 20~25wt%, potassium sulfate is 10~13wt%, and the rest is water; ℃ and 150-500r/min rotating speed conditions, stirring for 1-2h to prepare potassium alum crystallization mother liquor Ⅰ;
步骤二、在常压或在真空度为0.02~0.05MPa的条件下，将步骤一制得的钾明矾结晶母液Ⅰ蒸发浓缩至溶液密度为1.25~1.35g/mL，制得钾明矾结晶母液Ⅱ； Step 2. Under normal pressure or under the condition that the degree of vacuum is 0.02~0.05MPa, the potassium alum crystallization mother liquor I prepared in step 1 is evaporated and concentrated to a solution density of 1.25~1.35g/mL, and the potassium alum crystallization mother liquor II is obtained. ;
步骤三、在常压、80~100℃和150～500r/min的转速条件下，向步骤二制得的钾明矾结晶母液Ⅱ中加入晶种，保温搅拌0.5~1h，制得悬浊晶浆； Step 3: Under the conditions of normal pressure, 80-100°C and 150-500r/min, add crystal seeds to the potassium alum crystallization mother liquor II prepared in step 2, keep stirring for 0.5-1h, and prepare a suspended crystal slurry ;
步骤四、在常压和150～500r/min的转速条件下，将步骤三制得的悬浊晶浆以1～10℃/h的速率降温至25~35℃，然后过滤，洗涤，干燥；制得平均粒径大的钾明矾晶体，滤液以及洗涤水返回步骤一循环套用。 Step 4. Under normal pressure and a rotational speed of 150-500r/min, cool the suspended magma prepared in Step 3 to 25-35°C at a rate of 1-10°C/h, then filter, wash and dry; Obtain potassium alum crystals with a large average particle size, and the filtrate and washing water are returned to step 1 for recycling.
所述的晶种是十二水硫酸铝钾晶体，晶种加入量为钾明矾结晶产品总质量的0.1～5wt%。 The seed crystals are potassium aluminum sulfate dodecahydrate crystals, and the seed crystals are added in an amount of 0.1-5 wt% of the total mass of potassium alum crystallization products.
具体实施方式 detailed description
下面结合具体实施方式对本发明作进一步的描述，并非对其保护范围的限制。 The present invention will be further described below in combination with specific embodiments, which are not intended to limit the scope of protection thereof.
实施例 Example
一种钾明矾的制备方法，其具体步骤是： A kind of preparation method of potassium alum, its concrete steps are:
步骤一、先将硫酸铝、硫酸钾和水按下述配比进行配料，其中：硫酸铝为20~25wt%，硫酸钾为10~13wt%，其余为水；再在常压、80~100℃和150～500r/min的转速条件下搅拌1~2h制得钾明矾结晶母液Ⅰ； Step 1, first mix aluminum sulfate, potassium sulfate and water according to the following ratio, wherein: aluminum sulfate is 20~25wt%, potassium sulfate is 10~13wt%, and the rest is water; ℃ and 150-500r/min rotating speed conditions, stirring for 1-2h to prepare potassium alum crystallization mother liquor Ⅰ;
步骤二、在常压或在真空度为0.02~0.05MPa的条件下，将步骤一制得的钾明矾结晶母液Ⅰ蒸发浓缩至溶液密度为1.25~1.35g/mL，制得钾明矾结晶母液Ⅱ； Step 2. Under normal pressure or under the condition that the degree of vacuum is 0.02~0.05MPa, the potassium alum crystallization mother liquor I prepared in step 1 is evaporated and concentrated to a solution density of 1.25~1.35g/mL, and the potassium alum crystallization mother liquor II is obtained. ;
步骤三、在常压、80~100℃和150～500r/min的转速条件下，向步骤二制得的钾明矾结晶母液Ⅱ中加入晶种，保温搅拌0.5~1h，制得悬浊晶浆； Step 3: Under the conditions of normal pressure, 80-100°C and 150-500r/min, add crystal seeds to the potassium alum crystallization mother liquor II prepared in step 2, keep stirring for 0.5-1h, and prepare a suspended crystal slurry ;
步骤四、在常压和150～500r/min的转速条件下，将步骤三制得的悬浊晶浆以1～10℃/h的速率降温至25~35℃，然后过滤，洗涤，干燥；制得平均粒径大于1.5mm的钾明矾晶体，滤液以及洗涤水返回步骤一循环套用。 Step 4. Under normal pressure and a rotational speed of 150-500r/min, cool the suspended magma prepared in Step 3 to 25-35°C at a rate of 1-10°C/h, then filter, wash and dry; Potassium alum crystals with an average particle size greater than 1.5 mm are obtained, and the filtrate and washing water are returned to step 1 for recycling.
所述的晶种是十二水硫酸铝钾晶体，晶种加入量为钾明矾结晶产品总质量的0.1～5wt%。 The seed crystals are potassium aluminum sulfate dodecahydrate crystals, and the seed crystals are added in an amount of 0.1-5 wt% of the total mass of potassium alum crystallization products.
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| CN201410701042.8A CN105692673A (en) | 2014-11-28 | 2014-11-28 | Preparation method of potassium alum |
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| CN201410701042.8A CN105692673A (en) | 2014-11-28 | 2014-11-28 | Preparation method of potassium alum |
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Application publication date: 20160622 |
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