CN102153125A - A method for preparing sulfuric acid slag as sulfate by chemical method - Google Patents
A method for preparing sulfuric acid slag as sulfate by chemical method Download PDFInfo
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 40
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title claims abstract description 30
- 239000000126 substance Substances 0.000 title claims abstract description 14
- 239000002893 slag Substances 0.000 title description 42
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 36
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 32
- 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 19
- 238000005260 corrosion Methods 0.000 claims abstract description 18
- 230000007797 corrosion Effects 0.000 claims abstract description 18
- 238000010306 acid treatment Methods 0.000 claims abstract description 17
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 16
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 16
- 238000000746 purification Methods 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 13
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims abstract description 13
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims abstract description 13
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000012065 filter cake Substances 0.000 claims abstract description 12
- 239000003818 cinder Substances 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims abstract description 11
- 238000004821 distillation Methods 0.000 claims abstract description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000001110 calcium chloride Substances 0.000 claims abstract description 6
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 6
- 229910021332 silicide Inorganic materials 0.000 claims abstract description 6
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract 4
- 239000007788 liquid Substances 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000012047 saturated solution Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims 4
- 238000012856 packing Methods 0.000 claims 2
- 230000002194 synthesizing effect Effects 0.000 claims 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000001117 sulphuric acid Substances 0.000 claims 1
- 235000011149 sulphuric acid Nutrition 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract description 5
- 150000001805 chlorine compounds Chemical class 0.000 abstract description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 5
- 150000003467 sulfuric acid derivatives Chemical class 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 14
- 229910052683 pyrite Inorganic materials 0.000 description 14
- 239000011028 pyrite Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 9
- 229910052717 sulfur Inorganic materials 0.000 description 9
- 239000011593 sulfur Substances 0.000 description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 229910000358 iron sulfate Inorganic materials 0.000 description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- -1 ferrous metals Chemical class 0.000 description 4
- 238000007710 freezing Methods 0.000 description 4
- 230000008014 freezing Effects 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000005292 vacuum distillation Methods 0.000 description 4
- WAKTWVHWRCNIKU-UHFFFAOYSA-N S(=O)(=O)(O)O.[AlH3] Chemical compound S(=O)(=O)(O)O.[AlH3] WAKTWVHWRCNIKU-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 229940037003 alum Drugs 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 208000006399 Premature Obstetric Labor Diseases 0.000 description 1
- 206010036600 Premature labour Diseases 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- OIPILFWXSMYKGL-UHFFFAOYSA-N acetylcholine Chemical compound CC(=O)OCC[N+](C)(C)C OIPILFWXSMYKGL-UHFFFAOYSA-N 0.000 description 1
- 229960004373 acetylcholine Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229940103272 aluminum potassium sulfate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 208000002296 eclampsia Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229940098829 magnesium sulfate injection Drugs 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 230000004118 muscle contraction Effects 0.000 description 1
- 210000002464 muscle smooth vascular Anatomy 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 210000000715 neuromuscular junction Anatomy 0.000 description 1
- 210000005259 peripheral blood Anatomy 0.000 description 1
- 239000011886 peripheral blood Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 208000026440 premature labor Diseases 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 230000013948 uterine smooth muscle contraction Effects 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
技术领域：Technical field:
本发明属于无机化工硫酸行业废弃烧渣治理和利用的技术领域，尤其是一种用化学法制备硫酸烧渣为硫酸盐的方法。The invention belongs to the technical field of treatment and utilization of waste slag in the sulfuric acid industry in the inorganic chemical industry, in particular to a method for preparing sulfuric acid slag into sulfate by a chemical method.
技术背景：technical background:
硫酸工业是以硫铁矿为原料接触法生产的硫酸，主要由原料、焙烧、净化、转化和吸收五个工序组成。一般习惯上以净化工艺流程，经硫酸生产分成干法和湿法两大类。湿法净化又有酸洗、热浓酸洗和水洗之分。目前我国硫铁矿制酸少数工厂是酸洗流程，多数仍为水洗流程。The sulfuric acid industry uses pyrite as raw material to produce sulfuric acid by contact method, which is mainly composed of five processes: raw material, roasting, purification, conversion and absorption. Generally, the purification process is generally used to divide sulfuric acid production into two categories: dry method and wet method. Wet cleaning can be divided into pickling, hot concentrated pickling and water washing. At present, a small number of pyrite acid production plants in my country are pickling processes, and most of them are still water washing processes.
硫铁矿主要由硫和铁组成，伴有少量的有色金属和稀有金属。硫铁矿烧渣为硫铁矿焙烧提取硫后排出的残渣。硫铁矿中除了硫被利用外，铁及其他元素仍留在烧渣中。烧渣是用来炼铁，提取有色金属和制造建筑材料的原料。Pyrite is mainly composed of sulfur and iron, accompanied by a small amount of non-ferrous metals and rare metals. Pyrite slag is the residue discharged after pyrite roasting to extract sulfur. In addition to the utilization of sulfur in pyrite, iron and other elements remain in the slag. Cinder is a raw material used to smelt iron, extract non-ferrous metals and make building materials.
单位硫酸产品的排放量与硫铁矿的品位及工艺条件有关。在相同的工艺条件下硫铁矿的品位越高则排渣量就越少，反之则高。当硫铁矿含硫量为25～35％时，一般生产每吨约产生0.7～1吨的烧结渣。下面硫酸烧渣的各种成分的百分含量为四氧化三铁含量为43.31％，三氧化二铝含量为8.13％，氧化钙含量为1.63％，氧化镁含量为0.46％，氧化硅含量为35.73％，硫的含量为0.16％。The emission per unit of sulfuric acid product is related to the grade and process conditions of pyrite ore. Under the same process conditions, the higher the pyrite grade, the less the slag discharge, and vice versa. When the sulfur content of pyrite is 25-35%, generally 0.7-1 ton of sinter slag is produced per ton of production. The percentages of the various components of the following sulfuric acid slag are 43.31% for ferric oxide, 8.13% for aluminum oxide, 1.63% for calcium oxide, 0.46% for magnesium oxide, and 35.73% for silicon oxide. %, the sulfur content is 0.16%.
其一，对硫酸烧渣的利用应不断提高产出物的价值，产出一些市场紧缺的、附加值大的产品，以提高硫酸烧渣利用的经济效益。First, the utilization of sulfuric acid slag should continuously increase the value of the output, and produce some products that are in short supply in the market and have high added value, so as to improve the economic benefits of sulfuric acid slag utilization.
其二，众所周知，硫酸烧渣的利用与硫酸盐有关。硫酸镁注射液的镁离子可抑制中枢神经的活动，抑制运动神经～肌肉接头乙酰胆碱的释放，阻断神经肌肉联接处的传导，降低或解除肌肉收缩作用，同时对血管平滑肌有舒张作用，使痉挛的外周血管扩张，降低血压，因而对子痫有预防和治疗作用，对子宫平滑肌收缩也有抑制作用，可用于治疗早产。硫酸铝是一个被广泛运用的工业试剂，通常会与明矾混淆；明矾是硫酸铝与硫酸钾的复盐，而硫酸铝是单盐。复盐又称重盐，由两种以上单盐组成，在溶液中电离为单盐离子；硫酸铝通常被作为絮凝剂，用于提纯饮用水及污水处理设备当中，也用于造纸工业。硫酸铁常用作分析试剂、糖定量测定、铁催化剂、媒染剂、净水剂制颜料、药物。Second, as we all know, the utilization of sulfuric acid slag is related to sulfate. Magnesium ions in magnesium sulfate injection can inhibit the activity of the central nervous system, inhibit the release of acetylcholine from the motor nerve to muscle junction, block the conduction at the neuromuscular junction, reduce or relieve muscle contraction, and at the same time have a relaxing effect on vascular smooth muscle, causing spasm Peripheral blood vessels dilate and lower blood pressure, so it has preventive and therapeutic effects on eclampsia, and also has inhibitory effects on uterine smooth muscle contraction, and can be used to treat premature labor. Aluminum sulfate is a widely used industrial reagent and is often confused with alum; alum is a double salt of aluminum sulfate and potassium sulfate, while aluminum sulfate is a single salt. Double salt, also known as heavy salt, is composed of two or more single salts, which are ionized into single salt ions in the solution; aluminum sulfate is usually used as a flocculant for purification of drinking water and sewage treatment equipment, and is also used in the paper industry. Ferric sulfate is often used as analytical reagent, quantitative determination of sugar, iron catalyst, mordant, water purifying agent, pigment and medicine.
发明内容：Invention content:
本发明旨在针对硫酸烧渣的利用和市场需求，提供一种用化学法制备硫酸烧渣为硫酸盐的方法。The invention aims at the utilization and market demand of sulfuric acid slag, and provides a method for preparing sulfuric acid slag into sulfate by chemical method.
为了实现上述目的，本发明一种用化学法制备硫酸烧渣为硫酸盐的方法的技术方案如下。In order to achieve the above object, a kind of technical scheme of the method for the sulfuric acid slag prepared by chemical method of the present invention is as follows.
一种用化学法制备硫酸烧渣为硫酸盐的方法，硫酸烧渣通过酸处理回收及合成纯化工艺，制得硫酸盐；A method for preparing sulfuric acid slag as sulfate by chemical method, the sulfuric acid slag is recycled by acid treatment and synthesized and purified to obtain sulfate;
所述酸处理回收工艺为：将硫酸烧渣中的氯化铝与盐酸以纯质量比1∶1.95～2.35投入第一耐腐蚀反应器中，同时打开搅拌器缓缓搅拌使物质进行化学反应；20分钟后反应生成氯化铝、氯化铁、氯化钙、氯化镁等氯化物；过滤得到黑色滤饼硅化物和单质硫送去另外深加工，同时得到澄清的氯化物液体进行下一步提纯；The acid treatment and recovery process is as follows: put the aluminum chloride and hydrochloric acid in the sulfuric acid slag into the first corrosion-resistant reactor at a pure mass ratio of 1:1.95 to 2.35, and simultaneously turn on the agitator and stir slowly to make the material undergo a chemical reaction; 20 Minutes later, the reaction will generate aluminum chloride, ferric chloride, calcium chloride, magnesium chloride and other chlorides; the black filter cake silicide and elemental sulfur will be obtained by filtration, which will be further processed, and the clarified chloride liquid will be obtained for further purification;
所述合成纯化工艺为：将所述酸处理回收工艺得到的氯化铝与稀硫酸以纯质量比1∶0.9～1.3送入第二耐腐蚀反应器中，开动搅拌器在缓缓的搅拌下反应生成硫酸铝、硫酸铁、硫酸钙、硫酸镁等硫酸盐；过滤得到白色滤饼硫酸钙经洗涤干燥、粉碎包装得到硫酸钙产品。同时得到澄清的硫酸铝、硫酸铁、硫酸镁、盐酸混合溶液进行下一步提取；The synthesis and purification process is as follows: the aluminum chloride and dilute sulfuric acid obtained in the acid treatment and recovery process are sent to the second corrosion-resistant reactor at a pure mass ratio of 1:0.9-1.3, and the agitator is started to react under slow stirring. Generate aluminum sulfate, iron sulfate, calcium sulfate, magnesium sulfate and other sulfates; filter to obtain white filter cake calcium sulfate, wash and dry, crush and pack to obtain calcium sulfate products. At the same time, a clarified mixed solution of aluminum sulfate, iron sulfate, magnesium sulfate and hydrochloric acid is obtained for the next step of extraction;
将澄清硫酸盐溶液送入耐腐蚀减压蒸馏器里进行减压蒸馏，当蒸馏液体达到了饱和溶液时排出来进入冷却器进行分级冷却；根据他们的凝固点不同将依次冷却出硫酸铁、硫酸铝、硫酸镁晶体；再经洗涤甩干、包装检斤得到三种硫酸盐晶体产品。最后蒸馏剩下的液体为盐酸溶液返回上道工艺循环利用。Send the clarified sulfate solution into a corrosion-resistant vacuum distiller for vacuum distillation. When the distilled liquid reaches a saturated solution, it is discharged into the cooler for graded cooling; according to their different freezing points, iron sulfate and aluminum sulfate will be cooled in turn. 1. Magnesium sulfate crystals; then washed, dried, packaged and weighed to obtain three sulfate crystal products. Finally, the remaining liquid after distillation is returned to the upper process for recycling as hydrochloric acid solution.
本发明所用的硫酸烧渣为生产硫铁矿为原料接触法生产的硫酸烧渣，其组分是这样的：四氧化三铁，三氧化二铝，氧化钙，氧化镁，氧化硅，硫。The sulfuric acid slag used in the present invention is the sulfuric acid slag produced by pyrite as a raw material contact method, and its components are as follows: ferric oxide, aluminum oxide, calcium oxide, magnesium oxide, silicon oxide, and sulfur.
本发明的化学反应式为：Al2O3+6HCl＝＝＝＝2AlCl3+3H2OThe chemical reaction formula of the present invention is: Al 2 O 3 +6HCl====2AlCl 3 +3H 2 O
2AlCl3+3H2SO4＝＝＝＝Al2(SO4)3+6HCl2AlCl 3 +3H 2 SO 4 ====Al 2 (SO4) 3 +6HCl
本发明的有益效果在于：其一，提供了一种用化学法制备硫酸烧渣为硫酸盐的方法，为有效处理硫酸烧渣开辟一条途径。其二，制取物包括硫酸铁、硫酸铝、硫酸镁都是经济价值较大的畅销产品，提高了处理硫酸烧渣的经济效益。其三，投资少，对处理生产硫铁矿为原料接触法生产的硫酸烧渣及类似组分的硫酸烧渣尤为适用，可以说开辟了一条新路。其四，制取物的纯度高，质量有保证。The beneficial effects of the present invention are as follows: firstly, it provides a method for preparing sulfuric acid slag into sulfate by chemical method, and opens up a way for effectively treating sulfuric acid slag. Second, the products produced include ferric sulfate, aluminum sulfate, and magnesium sulfate, all of which are best-selling products with high economic value, which improves the economic benefits of treating sulfuric acid slag. Third, the investment is low, and it is especially suitable for the treatment of sulfuric acid slag produced by the contact method of pyrite as a raw material and the sulfuric acid slag of similar components, which can be said to open up a new road. Its four, the purity of preparation is high, and quality is guaranteed.
具体实施方式Detailed ways
实施例一Embodiment one
一种用化学法制备硫酸烧渣为硫酸盐的方法，硫酸烧渣通过酸处理回收及合成纯化工艺，制得硫酸盐；A method for preparing sulfuric acid slag as sulfate by chemical method, the sulfuric acid slag is recycled by acid treatment and synthesized and purified to obtain sulfate;
所述酸处理回收工艺为：取硫酸烧渣500公斤(其中含三氧化二铝含量为8.13％)将硫酸烧渣中的氯化铝与盐酸以纯质量比1∶2.15投入第一耐腐蚀反应器中，同时打开搅拌器缓缓搅拌使物质进行化学反应；20分钟后反应生成106.8公斤氯化铝和氯化铁、氯化钙、氯化镁等氯化物；过滤得到黑色滤饼硅化物和单质硫送去另外深加工，同时得到澄清的氯化物液体进行下一步提纯；The acid treatment and recovery process is as follows: take 500 kg of sulfuric acid slag (which contains 8.13% aluminum oxide content) and put aluminum chloride and hydrochloric acid in the sulfuric acid slag into the first corrosion-resistant reactor with a pure mass ratio of 1:2.15 At the same time, turn on the agitator and stir slowly to make the material undergo a chemical reaction; after 20 minutes, the reaction generates 106.8 kg of aluminum chloride, ferric chloride, calcium chloride, magnesium chloride and other chlorides; filter to obtain black filter cake silicide and elemental sulfur. Go to another deep processing, and at the same time obtain a clarified chloride liquid for further purification;
所述合成纯化工艺为：将所述酸处理回收工艺得到的氯化铝与稀硫酸以纯质量比1∶1.1送入第二耐腐蚀反应器中，开动搅拌器在缓缓的搅拌下反应生成硫酸铝、硫酸铁、硫酸钙、硫酸镁等硫酸盐；过滤得到白色滤饼硫酸钙经洗涤干燥、粉碎包装得到硫酸钙产品。同时得到澄清的硫酸铝、硫酸铁、硫酸镁、盐酸混合溶液进行下一步提取；The synthesis and purification process is as follows: the aluminum chloride and dilute sulfuric acid obtained by the acid treatment and recovery process are sent into the second corrosion-resistant reactor at a pure mass ratio of 1:1.1, and the agitator is started to react under slow stirring to generate sulfuric acid Aluminum, ferric sulfate, calcium sulfate, magnesium sulfate and other sulfates; filter to obtain white filter cake calcium sulfate, wash and dry, crush and pack to obtain calcium sulfate products. At the same time, a clarified mixed solution of aluminum sulfate, iron sulfate, magnesium sulfate and hydrochloric acid is obtained for the next step of extraction;
将澄清硫酸盐溶液送入耐腐蚀减压蒸馏器里进行减压蒸馏，当蒸馏液体达到了饱和溶液时排出来进入冷却器进行分级冷却；根据他们的凝固点不同将依次冷却出136.66公斤硫酸铝晶体和硫酸铁、硫酸镁晶体；再经洗涤甩干、包装检斤得到三种硫酸盐晶体产品。最后蒸馏剩下的液体为盐酸溶液返回上道工艺循环利用。Send the clarified sulfate solution into a corrosion-resistant vacuum distiller for vacuum distillation. When the distilled liquid reaches a saturated solution, it will be discharged into the cooler for graded cooling; 136.66 kg of aluminum sulfate crystals will be cooled in turn according to their different freezing points and ferric sulfate and magnesium sulfate crystals; then washed, dried, packaged and weighed to obtain three sulfate crystal products. Finally, the remaining liquid after distillation is returned to the upper process for recycling as hydrochloric acid solution.
本发明所用的硫酸烧渣为生产硫铁矿为原料接触法生产的硫酸烧渣，其组分是这样的：四氧化三铁含量为43.31％，三氧化二铝含量为8.13％，氧化钙含量为1.63％，氧化镁含量为0.46％，氧化硅含量为35.73％，硫的含量为0.16％。The sulfuric acid slag used in the present invention is the production of pyrite as the sulfuric acid slag produced by the raw material contact method, and its components are as follows: the content of ferric oxide is 43.31%, the content of aluminum oxide is 8.13%, and the content of calcium oxide The content of magnesium oxide is 1.63%, the content of magnesium oxide is 0.46%, the content of silicon oxide is 35.73%, and the content of sulfur is 0.16%.
实施例二Embodiment two
一种用化学法制备硫酸烧渣为硫酸盐的方法，硫酸烧渣通过酸处理回收及合成纯化工艺，制得硫酸盐；A method for preparing sulfuric acid slag as sulfate by chemical method, the sulfuric acid slag is recycled by acid treatment and synthesized and purified to obtain sulfate;
所述酸处理回收工艺为：取硫酸烧渣500公斤(其中含三氧化二铝含量为8.13％)将硫酸烧渣中的氯化铝与盐酸以纯质量比1∶2.35投入第一耐腐蚀反应器中，同时打开搅拌器缓缓搅拌使物质进行化学反应；20分钟后反应生成116.7公斤氯化铝和氯化铁、氯化钙、氯化镁等氯化物；过滤得到黑色滤饼硅化物和单质硫送去另外深加工，同时得到澄清的氯化物液体进行下一步提纯；The acid treatment and recovery process is as follows: take 500 kg of sulfuric acid slag (which contains 8.13% aluminum oxide content) and put aluminum chloride and hydrochloric acid in the sulfuric acid slag into the first corrosion-resistant reactor with a pure mass ratio of 1:2.35 At the same time, turn on the agitator and stir slowly to make the material react chemically; after 20 minutes, the reaction produces 116.7 kg of aluminum chloride, ferric chloride, calcium chloride, magnesium chloride and other chlorides; filter to obtain black filter cake silicide and elemental sulfur. Go to another deep processing, and at the same time obtain a clarified chloride liquid for further purification;
所述合成纯化工艺为：将所述酸处理回收工艺得到的氯化铝与稀硫酸以纯质量比1∶1.3送入第二耐腐蚀反应器中，开动搅拌器在缓缓的搅拌下反应生成硫酸铝、硫酸铁、硫酸钙、硫酸镁等硫酸盐；过滤得到白色滤饼硫酸钙经洗涤干燥、粉碎包装得到硫酸钙产品。同时得到澄清的硫酸铝、硫酸铁、硫酸镁、盐酸混合溶液进行下一步提取；The synthesis and purification process is as follows: the aluminum chloride and dilute sulfuric acid obtained in the acid treatment and recovery process are sent into the second corrosion-resistant reactor at a pure mass ratio of 1:1.3, and the agitator is started to react under slow stirring to generate sulfuric acid Aluminum, ferric sulfate, calcium sulfate, magnesium sulfate and other sulfates; filter to obtain white filter cake calcium sulfate, wash and dry, crush and pack to obtain calcium sulfate products. At the same time, a clarified mixed solution of aluminum sulfate, iron sulfate, magnesium sulfate and hydrochloric acid is obtained for the next step of extraction;
将澄清硫酸盐溶液送入耐腐蚀减压蒸馏器里进行减压蒸馏，当蒸馏液体达到了饱和溶液时排出来进入冷却器进行分级冷却；根据他们的凝固点不同将依次冷却出176.5公斤硫酸铝晶体和硫酸铁、硫酸镁晶体；再经洗涤甩干、包装检斤得到三种硫酸盐晶体产品。最后蒸馏剩下的液体为盐酸溶液返回上道工艺循环利用。Send the clarified sulfate solution into a corrosion-resistant vacuum distiller for vacuum distillation. When the distilled liquid reaches a saturated solution, it will be discharged into the cooler for graded cooling; 176.5 kg of aluminum sulfate crystals will be cooled in turn according to their different freezing points and ferric sulfate and magnesium sulfate crystals; then washed, dried, packaged and weighed to obtain three sulfate crystal products. Finally, the remaining liquid after distillation is returned to the upper process for recycling as hydrochloric acid solution.
本发明所用的硫酸烧渣为生产硫铁矿为原料接触法生产的硫酸烧渣，其组分是这样的：四氧化三铁含量为43.31％，三氧化二铝含量为8.13％，氧化钙含量为1.63％，氧化镁含量为0.46％，氧化硅含量为35.73％，硫的含量为0.16％。The sulfuric acid slag used in the present invention is the production of pyrite as the sulfuric acid slag produced by the raw material contact method, and its components are as follows: the content of ferric oxide is 43.31%, the content of aluminum oxide is 8.13%, and the content of calcium oxide The content of magnesium oxide is 1.63%, the content of magnesium oxide is 0.46%, the content of silicon oxide is 35.73%, and the content of sulfur is 0.16%.
实施例三Embodiment three
一种用化学法制备硫酸烧渣为硫酸盐的方法，硫酸烧渣通过酸处理回收及合成纯化工艺，制得硫酸盐；A method for preparing sulfuric acid slag as sulfate by chemical method, the sulfuric acid slag is recycled by acid treatment and synthesized and purified to obtain sulfate;
所述酸处理回收工艺为：取硫酸烧渣500公斤(其中含三氧化二铝含量为8.13％)将硫酸烧渣中的氯化铝与盐酸以纯质量比1∶1.95投入第一耐腐蚀反应器中，同时打开搅拌器缓缓搅拌使物质进行化学反应；20分钟后反应生成96.9公斤氯化铝和氯化铁、氯化钙、氯化镁等氯化物；过滤得到黑色滤饼硅化物和单质硫送去另外深加工，同时得到澄清的氯化物液体进行下一步提纯；The acid treatment and recovery process is as follows: take 500 kg of sulfuric acid slag (which contains 8.13% aluminum oxide content) and put aluminum chloride and hydrochloric acid in the sulfuric acid slag into the first corrosion-resistant reactor with a pure mass ratio of 1:1.95 At the same time, turn on the agitator and stir slowly to make the material undergo a chemical reaction; after 20 minutes, the reaction produces 96.9 kg of aluminum chloride, ferric chloride, calcium chloride, magnesium chloride and other chlorides; filter to obtain black filter cake silicide and elemental sulfur. Go to another deep processing, and at the same time obtain a clarified chloride liquid for further purification;
所述合成纯化工艺为：将所述酸处理回收工艺得到的氯化铝与稀硫酸以纯质量比1∶0.9送入第二耐腐蚀反应器中，开动搅拌器在缓缓的搅拌下反应生成硫酸铝、硫酸铁、硫酸钙、硫酸镁等硫酸盐；过滤得到白色滤饼硫酸钙经洗涤干燥、粉碎包装得到硫酸钙产品。同时得到澄清的硫酸铝、硫酸铁、硫酸镁、盐酸混合溶液进行下一步提取；The synthesis and purification process is as follows: the aluminum chloride and dilute sulfuric acid obtained in the acid treatment and recovery process are sent to the second corrosion-resistant reactor at a pure mass ratio of 1:0.9, and the agitator is started to react under slow stirring to generate sulfuric acid Aluminum, ferric sulfate, calcium sulfate, magnesium sulfate and other sulfates; filter to obtain white filter cake calcium sulfate, wash and dry, crush and pack to obtain calcium sulfate products. At the same time, a clarified mixed solution of aluminum sulfate, iron sulfate, magnesium sulfate and hydrochloric acid is obtained for the next step of extraction;
将澄清硫酸盐溶液送入耐腐蚀减压蒸馏器里进行减压蒸馏，当蒸馏液体达到了饱和溶液时排出来进入冷却器进行分级冷却；根据他们的凝固点不同将依次冷却出101.4公斤硫酸铝晶体和硫酸铁、硫酸镁晶体；再经洗涤甩干、包装检斤得到三种硫酸盐晶体产品。最后蒸馏剩下的液体为盐酸溶液返回上道工艺循环利用。Send the clarified sulfate solution into a corrosion-resistant vacuum distiller for vacuum distillation. When the distilled liquid reaches a saturated solution, it will be discharged into the cooler for graded cooling; 101.4 kg of aluminum sulfate crystals will be cooled in turn according to their freezing points. and ferric sulfate and magnesium sulfate crystals; then washed, dried, packaged and weighed to obtain three sulfate crystal products. Finally, the remaining liquid after distillation is returned to the upper process for recycling as hydrochloric acid solution.
本发明所用的硫酸烧渣为生产硫铁矿为原料接触法生产的硫酸烧渣，其组分是这样的：四氧化三铁含量为43.31％，三氧化二铝含量为8.13％，氧化钙含量为1.63％，氧化镁含量为0.46％，氧化硅含量为35.73％，硫的含量为0.16％。The sulfuric acid slag used in the present invention is the production of pyrite as the sulfuric acid slag produced by the raw material contact method, and its components are as follows: the content of ferric oxide is 43.31%, the content of aluminum oxide is 8.13%, and the content of calcium oxide The content of magnesium oxide is 1.63%, the content of magnesium oxide is 0.46%, the content of silicon oxide is 35.73%, and the content of sulfur is 0.16%.
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