CN102249334A - Method for preparing manganese sulfate, manganese hydroxide and potassium sulfate - Google Patents
Method for preparing manganese sulfate, manganese hydroxide and potassium sulfate Download PDFInfo
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- CN102249334A CN102249334A CN2010105979405A CN201010597940A CN102249334A CN 102249334 A CN102249334 A CN 102249334A CN 2010105979405 A CN2010105979405 A CN 2010105979405A CN 201010597940 A CN201010597940 A CN 201010597940A CN 102249334 A CN102249334 A CN 102249334A
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- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 title claims abstract description 54
- 229940099596 manganese sulfate Drugs 0.000 title claims abstract description 48
- 239000011702 manganese sulphate Substances 0.000 title claims abstract description 48
- 235000007079 manganese sulphate Nutrition 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 33
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 title claims abstract description 30
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 title claims abstract description 17
- 229910052939 potassium sulfate Inorganic materials 0.000 title claims abstract description 17
- 235000011151 potassium sulphates Nutrition 0.000 title claims abstract description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000013078 crystal Substances 0.000 claims abstract description 37
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000706 filtrate Substances 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 239000012047 saturated solution Substances 0.000 claims abstract description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract 5
- 238000001816 cooling Methods 0.000 claims abstract 4
- 238000000967 suction filtration Methods 0.000 claims abstract 3
- 238000003756 stirring Methods 0.000 claims abstract 2
- 239000002699 waste material Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 239000011572 manganese Substances 0.000 claims description 12
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 11
- 229910052748 manganese Inorganic materials 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims 4
- 208000006558 Dental Calculus Diseases 0.000 claims 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 3
- 239000011591 potassium Substances 0.000 claims 3
- 229910052700 potassium Inorganic materials 0.000 claims 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 2
- 239000011593 sulfur Substances 0.000 claims 2
- 229910052717 sulfur Inorganic materials 0.000 claims 2
- 235000010215 titanium dioxide Nutrition 0.000 claims 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 239000012065 filter cake Substances 0.000 claims 1
- 235000012054 meals Nutrition 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 239000004408 titanium dioxide Substances 0.000 abstract description 15
- 239000000843 powder Substances 0.000 abstract description 7
- 238000001914 filtration Methods 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910001200 Ferrotitanium Inorganic materials 0.000 description 1
- CZSABVBCTRZESY-UHFFFAOYSA-N [O-2].[O-2].[Ti+4].OS(O)(=O)=O Chemical compound [O-2].[O-2].[Ti+4].OS(O)(=O)=O CZSABVBCTRZESY-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- -1 sulfuric acid dihydrate Potassium Chemical compound 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明涉及无机化工三废的治理和利用技术领域，尤其涉及一种制备硫酸锰、氢氧化锰及硫酸钾的方法，其原料为用硫酸法生产钛白粉所得废液和锰矿。The invention relates to the technical field of treatment and utilization of inorganic chemical wastes, in particular to a method for preparing manganese sulfate, manganese hydroxide and potassium sulfate. The raw materials are waste liquid and manganese ore obtained by producing titanium dioxide by sulfuric acid.
背景技术 Background technique
硫酸法生产钛白粉是是将钛铁粉与浓硫酸进行酸解反应生产硫酸亚钛，经水解生成偏钛酸，再经锻烧、粉碎即得到钛白粉产品，其化学反应原理为：The production of titanium dioxide by the sulfuric acid method is to produce titanium dioxide sulfate by acidolysis reaction of ferrotitanium powder and concentrated sulfuric acid, which is hydrolyzed to generate metatitanic acid, and then calcined and pulverized to obtain titanium dioxide products. The chemical reaction principle is as follows:
、 Fe2O3+3H2SO4＝＝Fe2(SO4)3+3H2O, Fe 2 O 3 +3H 2 SO 4 ＝＝Fe 2 (SO 4 ) 3 +3H 2 O
TiO2+2H2SO4＝＝Ti(SO4)2+2H2OTiO 2 +2H 2 SO 4 ==Ti(SO 4 ) 2 +2H 2 O
Fe+Fe2(SO4)3＝＝3FeSO4 Fe+Fe 2 (SO 4 ) 3 == 3FeSO 4
Ti(SO4)2+3H2O＝＝H2TiO3↓+2H2SO4，Ti(SO 4 ) 2 +3H 2 O==H 2 TiO 3 ↓+2H 2 SO 4 ,
H2TiO3＝TiO2+H2O.H 2 TiO 3 ＝TiO 2 +H 2 O.
硫酸法生产钛白粉，其产生的工业废渣所含有的主要成分是硫酸，不仅排放量大而且排放浓度也很高。每生产一顿钛白粉约排出10吨硫酸质量百分浓度为10-25％的废渣，这些废渣本来可以采取浓缩循环工艺来制造浓硫酸，但是，存在着耗能高，所用材质要求苛刻，硫酸亚铁分离困难和回收时杂质富集等致命的问题。目前还尚未有较好的办法来解决钛白粉的废酸治理和利用的问题。The sulfuric acid method produces titanium dioxide, and the main component of the industrial waste residue is sulfuric acid, which not only has a large amount of emissions but also has a high emission concentration. About 10 tons of waste residue with a mass percent concentration of sulfuric acid of 10-25% is discharged for each ton of titanium dioxide produced. These waste residues can be produced by concentrated circulation process, but there are high energy consumption and demanding materials used. Sulfuric acid Fatal problems such as difficulty in ferrous separation and enrichment of impurities during recovery. At present, there is no better way to solve the problem of waste acid treatment and utilization of titanium dioxide.
发明内容 Contents of the invention
硫酸法生产钛白粉所得废液中所含有的主要成分为硫酸和硫酸亚铁，其中，硫酸的质量含量为10-20％。为了充分利用该废液，本发明提供一种制备硫酸锰、氢氧化锰及硫酸钾的方法，其原料为用硫酸法生产钛白粉所得废液和锰矿，该方法将硫酸法生产钛白粉所得废液经过简单的加工处理，提取和利用其中的硫酸，充分利用了硫酸法生产钛白粉所得废液的潜在价值，且不产生二次污染，是一个变废为宝，经济适用的方法。The main components contained in the waste liquid obtained by producing titanium dioxide by the sulfuric acid method are sulfuric acid and ferrous sulfate, wherein the mass content of the sulfuric acid is 10-20%. In order to make full use of the waste liquid, the present invention provides a method for preparing manganese sulfate, manganese hydroxide and potassium sulfate. After simple processing, the sulfuric acid in it is extracted and utilized, which makes full use of the potential value of the waste liquid obtained by the sulfuric acid method to produce titanium dioxide, and does not cause secondary pollution. It is an economical and applicable method to turn waste into treasure.
本发明的技术方案如下：一种制备硫酸锰、氢氧化锰及硫酸钾的方法，其原料为用硫酸法生产钛白粉所得废液和锰矿，包括如下具体步骤：Technical scheme of the present invention is as follows: a kind of method for preparing manganese sulfate, manganese hydroxide and potassium sulfate, its raw material is the waste liquid and manganese ore that produce titanium dioxide gained by sulfuric acid process, comprise following specific steps:
步骤A：硫酸法生产钛白粉所得废液中含有的硫酸浓度调整为18-30％，将方锰石磨成100-150目的粗粉，而后，将二者一起投入具有加热装置的浸泡罐(1)，浸泡8-15小时，浸泡温度为60-80℃，经抽滤机(2)抽滤浸泡液，得到澄清的滤液和滤渣；Step A: The concentration of sulfuric acid contained in the waste liquid obtained by sulfuric acid production of titanium dioxide is adjusted to 18-30%, and the square manganese is ground into a coarse powder of 100-150 mesh, and then both are put into a soaking tank with a heating device ( 1), soak for 8-15 hours, the soaking temperature is 60-80°C, and filter the soaking liquid through a suction filter (2) to obtain a clarified filtrate and filter residue;
步骤B：澄清的滤液中加入氢氧化锰除杂，过滤，得到纯净的硫酸锰溶液；Step B: adding manganese hydroxide to the clarified filtrate to remove impurities, and filtering to obtain a pure manganese sulfate solution;
步骤C：将纯净的硫酸锰溶液送入减压蒸馏器一(3)中减压蒸馏为硫酸锰饱和溶液，冷却，析出含有结晶水的硫酸锰晶体，含有结晶水的硫酸锰晶体，再经洗涤机一(4)洗涤、干燥器一(5)、粉碎机一(6)粉碎、得到硫酸锰晶体产品(7)；Step C: send pure manganese sulfate solution into underpressure distiller one (3) and distill under reduced pressure to be manganese sulfate saturated solution, cool down, separate out the manganese sulfate crystal that contains crystal water, contain the manganese sulfate crystal of crystal water, again through Washing machine one (4) washes, drier one (5), pulverizer one (6) pulverizes, obtains manganese sulfate crystal product (7);
步骤D：将纯净的硫酸锰溶液与氢氧化钾溶液以硫酸锰和氢氧化钾的纯物质的摩尔量之比1∶1.8-2.4投入耐腐蚀反应器(8)，搅拌下进行化学反应，得到含氢氧化锰和硫酸钾的混合物，经过滤器二(9)过滤，得到含硫酸钾和氢氧化锰滤液，以及少量的不溶性杂质滤饼；Step D: pure manganese sulfate solution and potassium hydroxide solution are dropped into corrosion-resistant reactor (8) with the molar ratio of the pure substance of manganese sulfate and potassium hydroxide 1: 1.8-2.4, carry out chemical reaction under stirring, obtain Containing the mixture of manganese hydroxide and potassium sulfate, filter through filter two (9), obtain containing potassium sulfate and manganese hydroxide filtrate, and a small amount of insoluble impurity filter cake;
步骤E：将含硫酸钾和氢氧化锰滤液送去减压蒸馏器二(10)蒸馏为饱和溶液，根据硫酸钾和氢氧化锰在不同温度下溶解度的不同，在不同的稳定冷却结晶，分别析出硫酸钾晶体和氢氧化锰晶体，将硫酸钾晶体和氢氧化锰晶体分别经过干燥器二(11)、粉碎机二(12)粉碎得到硫酸钾产品(13)和氢氧化锰产品(14)。Step E: send the filtrate containing potassium sulfate and manganese hydroxide to vacuum distiller two (10) and distill to be saturated solution, according to the difference of solubility at different temperatures of potassium sulfate and manganese hydroxide, crystallize in different stable cooling, respectively Precipitating potassium sulfate crystals and manganese hydroxide crystals, the potassium sulfate crystals and manganese hydroxide crystals are respectively pulverized through dryer two (11) and pulverizer two (12) to obtain potassium sulfate product (13) and manganese hydroxide product (14) .
本发明所述制备硫酸锰、氢氧化锰及硫酸钾的方法，其化学反应原理为：The method for preparing manganese sulfate, manganese hydroxide and potassium sulfate of the present invention, its chemical reaction principle is:
MnO+H2SO4＝＝＝＝＝MnSO4+H2OMnO+H 2 SO 4 =====MnSO 4 +H 2 O
MnSO4+2KOH＝＝＝＝＝Mn(OH)2+K2SO4 MnSO 4 +2KOH=====Mn(OH) 2 +K 2 SO 4
本发明的有益效果为：本发明所述制备硫酸锰、氢氧化锰及硫酸钾的方法，充分利用了硫酸法生产钛白粉所得废液的潜在价值，且不产生二次污染，是一个变废为宝，经济适用的方法。该方法操作简单，设备投资少，值得推广应用。The beneficial effects of the present invention are: the method for preparing manganese sulfate, manganese hydroxide and potassium sulfate described in the present invention fully utilizes the potential value of the waste liquid obtained by the sulfuric acid method to produce titanium dioxide, and does not produce secondary pollution, which is a waste It is a treasure, an economical and applicable method. The method is simple to operate and requires less investment in equipment, and is worthy of popularization and application.
附图说明 Description of drawings
图1为本发明所述制备硫酸锰、氢氧化锰及硫酸钾的方法的工艺流程图，其中，(1)浸泡罐，(2)抽滤机，(3)减压蒸馏器一，(4)洗涤机一，(5)干燥器一，(6)粉碎机一，(7)硫酸锰晶体产品，(8)耐腐蚀反应器，(9)过滤器二，(10)减压蒸馏器二，(11)干燥器二，(12)粉碎机二，(13)氢氧化锰产品，(14)洗涤机二，(15)干燥器三，(16)粉碎机三，(17)两水硫酸钾产品。Fig. 1 is the process flow chart of the method for preparing manganese sulfate, manganese hydroxide and potassium sulfate according to the present invention, wherein, (1) soak tank, (2) suction filter, (3) vacuum distiller one, (4) ) washing machine one, (5) dryer one, (6) pulverizer one, (7) manganese sulfate crystal product, (8) corrosion-resistant reactor, (9) filter two, (10) vacuum distiller two , (11) dryer two, (12) pulverizer two, (13) manganese hydroxide product, (14) washing machine two, (15) dryer three, (16) pulverizer three, (17) sulfuric acid dihydrate Potassium products.
具体实施方式 Detailed ways
实施例1：Example 1:
参照图1，一种制备硫酸锰、氢氧化锰及硫酸钾的方法，其原料为用硫酸法生产钛白粉所得废液和锰矿，包括如下具体步骤：With reference to Fig. 1, a kind of method for preparing manganese sulfate, manganese hydroxide and potassium sulfate, its raw material is to produce waste liquid and manganese ore gained by sulfuric acid process, comprises following specific steps:
步骤A：取500kg硫酸法生产钛白粉所得废液，调整其中含有的硫酸的质量浓度为18％，将方锰石磨成100目的粗粉，而后，将二者一起投入具有加热装置的浸泡罐(1)，浸泡8小时，浸泡温度为60℃，经抽滤机(2)抽滤浸泡液，得到澄清的滤液和滤渣；Step A: Take 500kg of the waste liquid obtained by the sulfuric acid method to produce titanium dioxide, adjust the mass concentration of the sulfuric acid contained therein to 18%, grind the square manganese into a 100-mesh coarse powder, and then put the two together into a soaking tank with a heating device (1), soak for 8 hours, the soaking temperature is 60 DEG C, and the soaking liquid is suction filtered through a suction filter (2), to obtain clarified filtrate and filter residue;
步骤B：澄清的滤液中加入氢氧化锰除杂，过滤，得到纯净的硫酸锰溶液；Step B: adding manganese hydroxide to the clarified filtrate to remove impurities, and filtering to obtain a pure manganese sulfate solution;
步骤C：将纯净的硫酸锰溶液送入减压蒸馏器一(3)中减压蒸馏为硫酸锰饱和溶液，冷却，析出含有结晶水的硫酸锰晶体，含有结晶水的硫酸锰晶体，再经洗涤机一(4)洗涤、干燥器一(5)、粉碎机一(6)粉碎、得到硫酸锰晶体产品(7)；其含有的硫酸锰的纯物质的量为138.67kg；Step C: send pure manganese sulfate solution into underpressure distiller one (3) and distill under reduced pressure to be manganese sulfate saturated solution, cool down, separate out the manganese sulfate crystal that contains crystal water, contain the manganese sulfate crystal of crystal water, again through Washing machine one (4) washes, drier one (5), pulverizer one (6) pulverizes, obtains the manganese sulfate crystal product (7); The pure substance amount of the manganese sulfate contained in it is 138.67kg;
步骤D：将纯净的硫酸锰溶液与氢氧化钾溶液以硫酸锰和氢氧化钾的纯物质的的摩尔量之比1∶1.8投入耐腐蚀反应器(8)，搅拌下进行化学反应，得到含氢氧化锰和硫酸钾的混合物，经过滤器二(9)过滤，得到含硫酸钾和氢氧化锰滤液，以及少量的不溶性杂质滤饼；Step D: pure manganese sulfate solution and potassium hydroxide solution are dropped into corrosion-resistant reactor (8) with the molar ratio of the pure substance of manganese sulfate and potassium hydroxide 1: 1.8, carry out chemical reaction under stirring, obtain containing The mixture of manganese hydroxide and potassium sulfate is filtered through filter two (9), obtains potassium sulfate and manganese hydroxide filtrate, and a small amount of insoluble impurity filter cake;
步骤E：将含硫酸钾和氢氧化锰滤液送去减压蒸馏器二(10)蒸馏为饱和溶液，根据硫酸钾和氢氧化锰在不同温度下溶解度的不同，在不同的稳定冷却结晶，分别析出硫酸钾晶体和氢氧化锰晶体，将硫酸钾晶体和氢氧化锰晶体分别经过干燥器二(11)、粉碎机二(12)粉碎得到硫酸钾产品(13)和氢氧化锰产品(14)，其含有的硫酸钾的纯物质的质量为144.07kg，其含有的氢氧化锰的纯物质的质量为73.69kg。Step E: send the filtrate containing potassium sulfate and manganese hydroxide to vacuum distiller two (10) and distill to be saturated solution, according to the difference of solubility at different temperatures of potassium sulfate and manganese hydroxide, crystallize in different stable cooling, respectively Precipitating potassium sulfate crystals and manganese hydroxide crystals, the potassium sulfate crystals and manganese hydroxide crystals are respectively pulverized through dryer two (11) and pulverizer two (12) to obtain potassium sulfate product (13) and manganese hydroxide product (14) , the quality of the pure substance of the potassium sulfate it contains is 144.07kg, and the quality of the pure substance of the manganese hydroxide it contains is 73.69kg.
实施例2：Example 2:
参照图1，一种制备硫酸锰、氢氧化锰及硫酸钾的方法，其原料为用硫酸法生产钛白粉所得废液和锰矿，包括如下具体步骤：With reference to Fig. 1, a kind of method for preparing manganese sulfate, manganese hydroxide and potassium sulfate, its raw material is to produce waste liquid and manganese ore gained by sulfuric acid process, comprises following specific steps:
步骤A：取500kg硫酸法生产钛白粉所得废液，调整其中含有的硫酸的质量浓度为20％，将方锰石磨成120目的粗粉，而后，将二者一起投入具有加热装置的浸泡罐(1)，浸泡12小时，浸泡温度为70℃，经抽滤机(2)抽滤浸泡液，得到澄清的滤液和滤渣；Step A: Take 500kg of the waste liquid obtained by the sulfuric acid method to produce titanium dioxide, adjust the mass concentration of the sulfuric acid contained therein to 20%, grind the square manganese into a 120-mesh coarse powder, and then put the two together into a soaking tank with a heating device (1), soak for 12 hours, the soaking temperature is 70 DEG C, and the soaking liquid is filtered through a suction filter (2), to obtain clarified filtrate and filter residue;
步骤B：澄清的滤液中加入氢氧化锰除杂，过滤，得到纯净的硫酸锰溶液；Step B: adding manganese hydroxide to the clarified filtrate to remove impurities, and filtering to obtain a pure manganese sulfate solution;
步骤C：将纯净的硫酸锰溶液送入减压蒸馏器一(3)中减压蒸馏为硫酸锰饱和溶液，冷却，析出含有结晶水的硫酸锰晶体，含有结晶水的硫酸锰晶体，再经洗涤机一(4)洗涤、干燥器一(5)、粉碎机一(6)粉碎、得到硫酸锰晶体产品(7)，其含有的硫酸锰的纯物质的量为154.08kg；Step C: send pure manganese sulfate solution into underpressure distiller one (3) and distill under reduced pressure to be manganese sulfate saturated solution, cool down, separate out the manganese sulfate crystal that contains crystal water, contain the manganese sulfate crystal of crystal water, again through Washing machine one (4) washes, drier one (5), pulverizer one (6) pulverizes, obtains the manganese sulfate crystal product (7), and the pure substance amount of the manganese sulfate contained in it is 154.08kg;
步骤D：将纯净的硫酸锰溶液与氢氧化钾溶液以硫酸锰和氢氧化钾的纯物质的的摩尔量之比1∶2投入耐腐蚀反应器(8)，搅拌下进行化学反应，得到含氢氧化锰和硫酸钾的混合物，经过滤器二(9)过滤，得到含硫酸钾和氢氧化锰滤液，以及少量的不溶性杂质滤饼；Step D: pure manganese sulfate solution and potassium hydroxide solution are dropped into corrosion-resistant reactor (8) with the molar ratio of the pure substance of manganese sulfate and potassium hydroxide 1: 2, carry out chemical reaction under stirring, obtain containing The mixture of manganese hydroxide and potassium sulfate is filtered through filter two (9), obtains potassium sulfate and manganese hydroxide filtrate, and a small amount of insoluble impurity filter cake;
步骤E：将含硫酸钾和氢氧化锰滤液送去减压蒸馏器二(10)蒸馏为饱和溶液，根据硫酸钾和氢氧化锰在不同温度下溶解度的不同，在不同的稳定冷却结晶，分别析出硫酸钾晶体和氢氧化锰晶体，将硫酸钾晶体和氢氧化锰晶体分别经过干燥器二(11)、粉碎机二(12)粉碎得到硫酸钾产品(13)和氢氧化锰产品(14)，其含有的硫酸钾的纯物质的质量为177.55kg，其含有的氢氧化锰的纯物质的质量为90.82kg。Step E: send the filtrate containing potassium sulfate and manganese hydroxide to vacuum distiller two (10) and distill to be saturated solution, according to the difference of solubility at different temperatures of potassium sulfate and manganese hydroxide, crystallize in different stable cooling, respectively Precipitating potassium sulfate crystals and manganese hydroxide crystals, the potassium sulfate crystals and manganese hydroxide crystals are respectively pulverized through dryer two (11) and pulverizer two (12) to obtain potassium sulfate product (13) and manganese hydroxide product (14) , the quality of the pure substance of the potassium sulfate it contains is 177.55kg, and the quality of the pure substance of the manganese hydroxide it contains is 90.82kg.
实施例3：Example 3:
参照图1，一种制备硫酸锰、氢氧化锰及硫酸钾的方法，其原料为用硫酸法生产钛白粉所得废液和锰矿，包括如下具体步骤：With reference to Fig. 1, a kind of method for preparing manganese sulfate, manganese hydroxide and potassium sulfate, its raw material is to produce waste liquid and manganese ore gained by sulfuric acid process, comprises following specific steps:
步骤A：取500kg硫酸法生产钛白粉所得废液，调整其中含有的硫酸的质量浓度为30％，将方锰石磨成150目的粗粉，而后，将二者一起投入具有加热装置的浸泡罐(1)，浸泡15小时，浸泡温度为80℃，经抽滤机(2)抽滤浸泡液，得到澄清的滤液和滤渣；Step A: Take 500kg of the waste liquid obtained by the sulfuric acid method to produce titanium dioxide, adjust the mass concentration of the sulfuric acid contained therein to 30%, grind the square manganese into a 150-mesh coarse powder, and then put the two together into a soaking tank with a heating device (1), soak for 15 hours, the soaking temperature is 80 DEG C, and the soaking liquid is filtered through a suction filter (2), to obtain clarified filtrate and filter residue;
步骤B：澄清的滤液中加入氢氧化锰除杂，过滤，得到纯净的硫酸锰溶液；Step B: adding manganese hydroxide to the clarified filtrate to remove impurities, and filtering to obtain a pure manganese sulfate solution;
步骤C：将纯净的硫酸锰溶液送入减压蒸馏器一(3)中减压蒸馏为硫酸锰饱和溶液，冷却，析出含有结晶水的硫酸锰晶体，含有结晶水的硫酸锰晶体，再经洗涤机一(4)洗涤、干燥器一(5)、粉碎机一(6)粉碎、得到硫酸锰晶体产品(7)，其含有的硫酸锰的纯物质的量为231.12kg；Step C: send pure manganese sulfate solution into underpressure distiller one (3) and distill under reduced pressure to be manganese sulfate saturated solution, cool down, separate out the manganese sulfate crystal that contains crystal water, contain the manganese sulfate crystal of crystal water, again through Washing machine one (4) washes, drier one (5), pulverizer one (6) pulverizes, obtains the manganese sulfate crystal product (7), and the pure substance amount of the manganese sulfate contained in it is 231.12kg;
步骤D：将纯净的硫酸锰溶液与氢氧化钾溶液以硫酸锰和氢氧化钾的纯物质的的摩尔量之比1∶2.4投入耐腐蚀反应器(8)，搅拌下进行化学反应，得到含氢氧化锰和硫酸钾的混合物，经过滤器二(9)过滤，得到含硫酸钾和氢氧化锰滤液，以及少量的不溶性杂质滤饼；Step D: pure manganese sulfate solution and potassium hydroxide solution are dropped into corrosion-resistant reactor (8) with the molar ratio of the pure substance of manganese sulfate and potassium hydroxide 1: 2.4, carry out chemical reaction under stirring, obtain containing The mixture of manganese hydroxide and potassium sulfate is filtered through filter two (9), obtains potassium sulfate and manganese hydroxide filtrate, and a small amount of insoluble impurity filter cake;
步骤E：将含硫酸钾和氢氧化锰滤液送去减压蒸馏器二(10)蒸馏为饱和溶液，根据硫酸钾和氢氧化锰在不同温度下溶解度的不同，在不同的稳定冷却结晶，分别析出硫酸钾晶体和氢氧化锰晶体，将硫酸钾晶体和氢氧化锰晶体分别经过干燥器二(11)、粉碎机二(12)粉碎得到硫酸钾产品(13)和氢氧化锰产品(14)，其含有的硫酸钾的纯物质的质量为266.33kg，其含有的氢氧化锰的纯物质的质量为136.22kg。Step E: send the filtrate containing potassium sulfate and manganese hydroxide to vacuum distiller two (10) and distill to be saturated solution, according to the difference of solubility at different temperatures of potassium sulfate and manganese hydroxide, crystallize in different stable cooling, respectively Precipitating potassium sulfate crystals and manganese hydroxide crystals, the potassium sulfate crystals and manganese hydroxide crystals are respectively pulverized through dryer two (11) and pulverizer two (12) to obtain potassium sulfate product (13) and manganese hydroxide product (14) , the quality of the pure substance of the potassium sulfate it contains is 266.33kg, and the quality of the pure substance of the manganese hydroxide it contains is 136.22kg.
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，其架构形式能够灵活多变，可以派生系列产品。只是做出若干简单推演或替换，都应当视为属于本发明由所提交的权利要求书确定的专利保护范围。The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be assumed that the specific implementation of the present invention is limited to these descriptions. For those of ordinary skill in the technical field to which the present invention belongs, without departing from the concept of the present invention, its architecture can be flexible and changeable, and series of products can be derived. Just making some simple deductions or replacements should be deemed to belong to the patent protection scope of the present invention determined by the submitted claims.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105905925A (en) * | 2016-06-06 | 2016-08-31 | 五矿（湖南）铁合金有限责任公司 | Method for comprehensive recovery of valuable metal from ferromanganese melting fly ash and waste residues |
| CN109354071A (en) * | 2018-11-21 | 2019-02-19 | 安徽工业大学 | A method for producing battery-grade manganese sulfate by utilizing manganese tailings and titanium dioxide waste sulfuric acid |
| CN114249352A (en) * | 2020-09-25 | 2022-03-29 | 沈阳化工研究院有限公司 | Method for treating wastewater generated in production of 6-methoxy tetralone |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105905925A (en) * | 2016-06-06 | 2016-08-31 | 五矿（湖南）铁合金有限责任公司 | Method for comprehensive recovery of valuable metal from ferromanganese melting fly ash and waste residues |
| CN109354071A (en) * | 2018-11-21 | 2019-02-19 | 安徽工业大学 | A method for producing battery-grade manganese sulfate by utilizing manganese tailings and titanium dioxide waste sulfuric acid |
| CN109354071B (en) * | 2018-11-21 | 2020-11-24 | 安徽工业大学 | A method for producing battery-grade manganese sulfate by utilizing manganese tailings and titanium dioxide waste sulfuric acid |
| CN114249352A (en) * | 2020-09-25 | 2022-03-29 | 沈阳化工研究院有限公司 | Method for treating wastewater generated in production of 6-methoxy tetralone |
| CN114249352B (en) * | 2020-09-25 | 2023-07-28 | 沈阳化工研究院有限公司 | Method for treating wastewater generated in production of 6-methoxy tetralone |
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