CN111874870B - Device and method for regulating and controlling element sulfur crystallization transformation in zinc smelting high-sulfur slag - Google Patents
Device and method for regulating and controlling element sulfur crystallization transformation in zinc smelting high-sulfur slag Download PDFInfo
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 87
- 230000008025 crystallization Effects 0.000 title claims abstract description 86
- 230000009466 transformation Effects 0.000 title claims abstract description 84
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 62
- 239000011593 sulfur Substances 0.000 title claims abstract description 62
- 239000002893 slag Substances 0.000 title claims abstract description 53
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 37
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000011701 zinc Substances 0.000 title claims abstract description 29
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 29
- 238000003723 Smelting Methods 0.000 title claims abstract description 21
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 6
- 230000001276 controlling effect Effects 0.000 title claims description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 23
- 239000002002 slurry Substances 0.000 claims description 19
- 230000002093 peripheral effect Effects 0.000 claims description 14
- 230000007704 transition Effects 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000003507 refrigerant Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000005188 flotation Methods 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 3
- 238000010494 dissociation reaction Methods 0.000 abstract description 3
- 230000005593 dissociations Effects 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 3
- 230000012010 growth Effects 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 6
- 238000009854 hydrometallurgy Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000007713 directional crystallization Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- 238000010908 decantation Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005363 electrowinning Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052950 sphalerite Inorganic materials 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- 238000011426 transformation method Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/027—Recovery of sulfur from material containing elemental sulfur, e.g. luxmasses or sulfur containing ores; Purification of the recovered sulfur
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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- General Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
技术领域technical field
本发明属于湿法冶金技术领域，尤其涉及一种锌冶炼高硫渣中元素硫晶化转型调控装置及其方法。The invention belongs to the technical field of hydrometallurgy, and in particular relates to a device and method for regulating and controlling crystallization transformation of elemental sulfur in high-sulfur slag of zinc smelting.
背景技术Background technique
锌在自然界中主要以硫化物形态存在，锌的硫化矿主要是闪锌矿和高铁闪锌矿。硫化锌精矿炼锌工艺分为火法和湿法炼锌工艺，其中主流的湿法炼锌工艺包括常规湿法锌冶炼(焙烧-浸出-净化-电积)和直接浸出工艺(氧压/常压浸出-净化-电积)。常规湿法炼锌工艺焙烧过程中会产生大量SO2烟气，存在工艺流程长、硫酸销售储存困难和环境污染严重等问题。锌直接浸出工艺取消了氧化焙烧工序，锌精矿中的硫氧化成单质硫进入酸浸渣中，避免了SO2烟气污染，尤其适用于地处偏远及硫酸销售困难的生产企业。这种方法能够很好的处理对锌冶炼不利的含铁、铅、硅高的锌精矿，锌回收率高达97％以上。Zinc exists mainly in the form of sulfide in nature, and the sulfide ores of zinc are mainly sphalerite and high-iron sphalerite. The zinc sulphide concentrate zinc smelting process is divided into pyrometallurgy and hydrometallurgy zinc smelting process, among which the mainstream hydrometallurgy zinc smelting process includes conventional hydrometallurgy zinc smelting (roasting-leaching-purification-electrowinning) and direct leaching process (oxygen pressure/ Atmospheric pressure leaching - purification - electrowinning). A large amount of SO 2 flue gas is produced during the roasting process of the conventional zinc hydrometallurgy process, and there are problems such as long process flow, difficult sales and storage of sulfuric acid, and serious environmental pollution. The zinc direct leaching process cancels the oxidation and roasting process, and the sulfur in the zinc concentrate is oxidized into elemental sulfur and enters the acid leaching residue, avoiding SO 2 flue gas pollution, and is especially suitable for production enterprises located in remote areas and difficult to sell sulfuric acid. This method can well deal with the zinc concentrate containing high iron, lead and silicon which is unfavorable to zinc smelting, and the recovery rate of zinc is as high as 97%.
从锌直接浸出高硫渣中回收单质硫的方法有很多，主要有高压倾析法、真空蒸馏法及浮选-热滤法等物理方法和二甲苯浸出法、硫化铵浸出法及四氯乙烯浸出法等化学方法，其中物理法在实际生产中有所应用，但各类物理法在硫回收应用时均存在不足之处。高压倾析法设备昂贵，产出的硫磺质量不高；虽然真空蒸馏法生产出的硫磺纯度高，但设备复杂、生产成本高；浮选-热滤法工艺简单、生产成本低，适于大规模工业生产，但硫磺直收率不高。因此单质硫晶相可控生长与迁移聚合，强化单质硫与其他矿相的高效分离，继而提高浮选-热滤工艺流程单质硫直收率的技术问题亟待解决。There are many methods for recovering elemental sulfur from high-sulfur slag leached directly from zinc, mainly including physical methods such as high-pressure decantation, vacuum distillation, flotation-hot filtration, and xylene leaching, ammonium sulfide leaching, and tetrachlorethylene leaching. Chemical methods such as leaching, among which physical methods have been applied in actual production, but all kinds of physical methods have shortcomings in the application of sulfur recovery. The equipment of high-pressure decantation method is expensive, and the quality of the sulfur produced is not high; although the sulfur produced by vacuum distillation method has high purity, the equipment is complicated and the production cost is high; the flotation-thermal filtration method has simple process and low production cost, and is suitable for large Large-scale industrial production, but the rate of direct sulfur recovery is not high. Therefore, the technical problems of controlling the growth, migration and aggregation of elemental sulfur crystal phase, strengthening the efficient separation of elemental sulfur from other mineral phases, and then improving the direct recovery rate of elemental sulfur in the flotation-thermal filtration process need to be solved urgently.
发明内容Contents of the invention
为了解决上述技术问题，本发明提供一种锌冶炼高硫渣中元素硫晶化转型调控装置及其方法，通过晶化转型调控与转化，实现单质硫晶体的可控生长和迁移聚合，为后续单质硫的空化解离和浮选提硫创造有利条件。In order to solve the above technical problems, the present invention provides a device and method for controlling elemental sulfur crystallization transformation in zinc smelting high-sulfur slag, through the crystallization transformation regulation and transformation, the controllable growth and migration polymerization of elemental sulfur crystals can be realized, which will provide a better way for the follow-up Cavitation dissociation of elemental sulfur and flotation sulfur extraction create favorable conditions.
为解决上述技术问题，本发明采用如下技术方案：In order to solve the problems of the technologies described above, the present invention adopts the following technical solutions:
本发明一种锌冶炼高硫渣中元素硫晶化转型调控装置，包括加热器、循环泵和晶化转型反应釜，所述晶化转型反应釜为立式结构，所述晶化转型反应釜一侧下端设置有出料口，一侧上端设置有溢流口，顶部为进料口，所述循环泵安装在所述加热器的加热器入口与所述晶化转型反应釜的溢流口之间的管道上，所述加热器出口与所述晶化转型反应釜的进料口之间通过循环管相连；所述加热器入口的一侧端还设置有新料进入口。The present invention is a control device for crystallization transition of elemental sulfur in zinc smelting high-sulfur slag, comprising a heater, a circulation pump and a crystallization transition reactor, the crystallization transition reactor is a vertical structure, and the crystallization transition reactor The lower end of one side is provided with a discharge port, the upper end of one side is provided with an overflow port, and the top is a feed port, and the circulation pump is installed between the heater inlet of the heater and the overflow port of the crystallization transformation reactor. On the pipe between, the outlet of the heater is connected with the feed port of the crystallization transformation reactor through a circulation pipe; one side of the inlet of the heater is also provided with a new material inlet.
进一步的，所述晶化转型反应釜内部设有中央下行管，所述中央下行管的上部是蒸汽出口，所述蒸汽出口内侧设有网状分离器。Further, a central downcomer is arranged inside the crystallization transformation reactor, the upper part of the central downcomer is a steam outlet, and a mesh separator is arranged inside the steam outlet.
进一步的，所述晶化转型反应釜的直径从上到下逐渐减小。Further, the diameter of the crystallization transformation reactor gradually decreases from top to bottom.
进一步的，所述晶化转型反应釜的外周侧安装有用于通入冷媒或热媒的外围夹套。Further, the outer peripheral side of the crystallization transformation reactor is installed with a peripheral jacket for introducing refrigerant or heating medium.
进一步的，所述外围夹套的流动方向为下进上出，工况正常情况下通冷媒，所述外围夹套的夹套入口用于将冷媒送入外围夹套内部，用于使得高硫渣矿浆降温到120℃以下，使其产生过饱和度并在晶化转型反应釜中析出晶体，其中所述外围夹套的夹套入口低于所述夹套出口。Further, the flow direction of the peripheral jacket is bottom-in and top-out, and refrigerant is passed through under normal working conditions, and the jacket inlet of the peripheral jacket is used to send refrigerant into the interior of the peripheral jacket to make the high-sulfur The temperature of the slag ore slurry is lowered to below 120° C. to generate supersaturation and precipitate crystals in the crystal transformation reactor, wherein the jacket inlet of the peripheral jacket is lower than the jacket outlet.
进一步的，所述晶化转型反应釜的溢流口处设置有用于控制矿浆溢流速度的调节阀。Further, the overflow port of the crystallization transformation reactor is provided with a regulating valve for controlling the overflow velocity of the slurry.
进一步的，所述加热器工作时，蒸汽通过所述加热器侧端的蒸汽入口进入加热器换热管道中，经传递热量之后降温形成冷凝水，通过冷凝水出口排出。Further, when the heater is working, the steam enters the heat exchange pipe of the heater through the steam inlet at the side end of the heater, and after transferring heat, the temperature is lowered to form condensed water, which is discharged through the condensed water outlet.
进一步的，所述加热器的工作温度为120-155℃，压力为200-550KPa。Further, the working temperature of the heater is 120-155°C, and the pressure is 200-550KPa.
一种锌冶炼高硫渣中元素硫晶化转型调控方法，所述方法包括：A method for controlling elemental sulfur crystallization transformation in zinc smelting high-sulfur slag, the method comprising:
A、加热溶解过程：将高硫渣在加热器中进行加热获得熔融流动性好的矿浆；A. Heating and dissolving process: heating high-sulfur slag in a heater to obtain ore pulp with good melting fluidity;
B、物料输送过程：熔融的高硫渣矿浆经过循环管流向晶化转型反应釜入料口，通过中央下行管进入晶化转型反应釜内侧；气体通过蒸汽出口排出，被夹带的高硫渣小颗粒被网状分离器挡住，落入到晶化转型反应釜中央下行管中；B. Material transportation process: The molten high-sulfur slag slurry flows through the circulation pipe to the feed port of the crystallization transformation reactor, and enters the inner side of the crystallization transformation reactor through the central downcomer; the gas is discharged through the steam outlet, and the entrained high-sulfur slag is small The particles are blocked by the mesh separator and fall into the central descending pipe of the crystallization transformation reactor;
C、晶化转型过程：控制高硫渣矿浆在一定酸度和搅拌速度范围内，在晶化转型反应釜外围夹套的冷却作用下降温到120℃以下，得到过饱和溶液，析出单质硫晶体结晶，沉降落入反应釜底部的分级腿中，进行粒度分级后得到最终的粒度均匀的产品。C. Crystallization transformation process: control the high-sulfur slag slurry within a certain range of acidity and stirring speed, and cool down to below 120°C under the cooling action of the outer jacket of the crystallization transformation reactor to obtain a supersaturated solution and precipitate elemental sulfur crystals. , settle down and fall into the grading legs at the bottom of the reactor, and get the final product with uniform particle size after particle size classification.
D、外循环过程：未充分长大的细晶颗粒及未充分转型的高硫渣矿浆通过反应釜上部的溢流口流出，在循环泵的作用下返回步骤A，与新料混合，开始下一循环。D. External circulation process: The fine-grained particles that have not grown sufficiently and the high-sulfur slag slurry that has not fully transformed flow out through the overflow port on the upper part of the reactor, and return to step A under the action of the circulating pump, mix with the new material, and start the next step. one cycle.
进一步的，所述高硫渣矿浆的酸度为70-100g/L；所述晶化转型反应釜内转化温度为80-119℃，所述搅拌速度为100-600r/min。Further, the acidity of the high-sulfur slag pulp is 70-100g/L; the conversion temperature in the crystallization transformation reactor is 80-119°C, and the stirring speed is 100-600r/min.
进一步的，所述高硫渣包括而不限定于加压氧浸和常压氧浸处理硫化锌精矿产出的浸出渣。Further, the high-sulfur slag includes, but is not limited to, leaching slag produced from zinc sulfide concentrates treated with pressurized oxygen leaching and atmospheric pressure oxygen leaching.
与现有技术相比，本发明的有益技术效果：Compared with prior art, beneficial technical effect of the present invention:
本发明提供的锌冶炼高硫渣中元素硫晶化转型调控装置，将加热器和晶化转型反应釜联合使用，通过加热器的加热作用，使高硫渣矿浆中单质硫的溶解度大大增加，而在晶化转型反应釜外围夹套的降温作用下单质硫的溶解度降低，形成过饱和溶液析出硫晶体，最终可得到粒径均匀、可浮选性能好的单质硫，为后续单质硫的空化解离和浮选提硫奠定基础。这种晶化转型装置可以大大提高高硫渣中元素硫的晶型转化效率，集中布局，减少占地；能够生产粒度较大且均匀的晶体。The device for controlling the crystallization transition of elemental sulfur in zinc smelting high-sulfur slag provided by the present invention uses a heater and a crystallization transition reactor in combination, and through the heating effect of the heater, the solubility of elemental sulfur in the high-sulfur slag slurry is greatly increased, However, under the cooling effect of the outer jacket of the crystallization transformation reactor, the solubility of elemental sulfur decreases, forming a supersaturated solution to precipitate sulfur crystals, and finally obtaining elemental sulfur with uniform particle size and good flotation performance, which is the space for subsequent elemental sulfur. It lays the foundation for dissociation and flotation sulfur extraction. This crystallization transformation device can greatly improve the crystal conversion efficiency of elemental sulfur in high-sulfur slag, with centralized layout and reduced land occupation; it can produce large and uniform crystals.
附图说明Description of drawings
下面结合附图说明对本发明作进一步说明。The present invention will be further described below in conjunction with the accompanying drawings.
图1为本发明锌冶炼高硫渣中元素硫晶化转型调控装置的结构示意图；Fig. 1 is a structural schematic diagram of the elemental sulfur crystallization transition control device in zinc smelting high-sulfur slag of the present invention;
附图标记说明：1-循环泵；2-循环管；3-新料进入口；4-夹套入口；5-晶化转型反应釜；6-出料口；7-外围夹套；8-中央下行管；9-夹套出口；10-进料口；11-网状分离器；12-蒸汽出口；13-溢流口；14-调节阀；15-加热器出口；16-蒸汽入口；17-加热器；18-冷凝水出口；19-加热器入口。Explanation of reference signs: 1-circulation pump; 2-circulation pipe; 3-new material inlet; 4-jacket inlet; 5-crystallization transformation reactor; 6-outlet; 7-peripheral jacket; Central downpipe; 9-jacket outlet; 10-feed inlet; 11-mesh separator; 12-steam outlet; 13-overflow port; 14-regulating valve; 15-heater outlet; 16-steam inlet; 17-heater; 18-condensate outlet; 19-heater inlet.
具体实施方式Detailed ways
如图1所示，一种锌冶炼高硫渣中元素硫晶化转型调控装置，包括加热器17、循环泵2和晶化转型反应釜5，所述晶化转型反应釜5上设置有进料口10、出料口6和溢流口13，循环泵1安装在加热器17的加热器入口19与晶化转型反应釜5的溢流口13之间的循环管2上，加热器出口15与晶化转型反应釜进料口10之间通过循环管2相连；加热器入口19的一侧端设置有新料进入口3。所述晶化转型反应釜5内部设有中央下行管8，所述中央下行管8的上部是蒸汽出口12，所述蒸汽出口12内侧设有网状分离器11，中央下行管8的末端延伸至靠近于晶化转型反应釜5的底部，并低于出料口6所在位置。所述晶化转型反应釜5的外周侧还设置有外围夹套7，其内部可以通冷媒(或热媒)，流动方向为下进上出，工况正常情况下通冷媒，夹套入口4用于将冷媒送入外围夹套内部，用于使得高硫渣矿浆降温到120℃以下，使其产生过饱和度并在晶化转型反应釜中析出晶体，夹套入口4低于所述夹套出口9。晶化转型反应釜5的溢流口13设有调节阀14，用于控制矿浆溢流速度。加热器17工作时，蒸汽通过其侧端的蒸汽入口16进入加热器换热管道中，经传递热量之后降温形成冷凝水，通过冷凝水出口18排出。加热器的工作温度为120-155℃，压力为200-550KPa。As shown in Figure 1, a control device for the crystallization transformation of elemental sulfur in high-sulfur slag from zinc smelting includes a heater 17, a circulation pump 2 and a crystallization transformation reactor 5, and the crystallization transformation reactor 5 is provided with an advanced Feed port 10, discharge port 6 and overflow port 13, circulation pump 1 is installed on the circulation pipe 2 between the heater inlet 19 of heater 17 and the overflow port 13 of crystal transformation reactor 5, heater outlet 15 is connected to the feed port 10 of the crystallization transformation reactor through a circulation pipe 2; one side end of the heater inlet 19 is provided with a fresh material inlet 3. The inside of the crystallization transformation reaction kettle 5 is provided with a central downcomer 8, the upper part of the central downcomer 8 is a steam outlet 12, and the inner side of the steam outlet 12 is provided with a mesh separator 11, and the end of the central downcomer 8 extends To the bottom close to the crystallization transformation reactor 5, and lower than the position of the outlet 6. The outer peripheral side of the crystallization transformation reaction kettle 5 is also provided with a peripheral jacket 7, the inside of which can pass through refrigerant (or heat medium), and the flow direction is from the bottom to the top. It is used to send the refrigerant into the outer jacket to cool the high-sulfur slag slurry to below 120°C so that it can generate supersaturation and precipitate crystals in the crystallization transformation reaction kettle. The inlet 4 of the jacket is lower than the jacket Set of outlets9. The overflow port 13 of the crystallization transformation reactor 5 is provided with a regulating valve 14 for controlling the overflow speed of the ore slurry. When the heater 17 is working, the steam enters the heat exchange pipe of the heater through the steam inlet 16 at the side end, and after transferring heat, the temperature is lowered to form condensed water, which is discharged through the condensed water outlet 18 . The working temperature of the heater is 120-155°C, and the pressure is 200-550KPa.
采用上述装置的晶化转型方法，包括如下步骤：The crystallization transformation method using the above-mentioned device comprises the following steps:
A、加热溶解过程：将高硫渣在加热器中进行加热获得熔融流动性好的矿浆；A. Heating and dissolving process: heating high-sulfur slag in a heater to obtain ore pulp with good melting fluidity;
B、物料输送过程：熔融的高硫渣矿浆经过循环管流向晶化转型反应釜入料口，通过中央下行管进入晶化转型反应釜内侧；气体通过蒸汽出口排出，被夹带的高硫渣小颗粒被网状分离器挡住，落入到晶化转型反应釜中央下行管中；B. Material transportation process: The molten high-sulfur slag slurry flows through the circulation pipe to the feed port of the crystallization transformation reactor, and enters the inner side of the crystallization transformation reactor through the central downcomer; the gas is discharged through the steam outlet, and the entrained high-sulfur slag is small The particles are blocked by the mesh separator and fall into the central descending pipe of the crystallization transformation reactor;
C、晶化转型过程：控制高硫渣矿浆在一定酸度和搅拌速度范围内，在晶化转型反应釜外围夹套的冷却作用下降温到120℃以下，得到过饱和溶液，析出单质硫晶体结晶，沉降落入反应釜底部的分级腿中，进行粒度分级后得到最终的粒度均匀的产品。C. Crystallization transformation process: control the high-sulfur slag slurry within a certain range of acidity and stirring speed, and cool down to below 120°C under the cooling action of the outer jacket of the crystallization transformation reactor to obtain a supersaturated solution and precipitate elemental sulfur crystals. , settle down and fall into the grading legs at the bottom of the reactor, and get the final product with uniform particle size after particle size classification.
D、外循环过程：未充分长大的细晶颗粒及未充分转型的高硫渣矿浆通过反应釜上部的溢流口流出，在循环泵的作用下返回步骤A，与新料混合，开始下一循环。D. External circulation process: The fine-grained particles that have not grown sufficiently and the high-sulfur slag slurry that has not fully transformed flow out through the overflow port on the upper part of the reactor, and return to step A under the action of the circulating pump, mix with the new material, and start the next step. one cycle.
下面通过具体实施例来说明本发明。The present invention is illustrated below through specific examples.
实施例1Example 1
将高硫渣置于加热器中加热获得高硫渣矿浆，通过循环管和晶化转型反应釜中央下行管进入晶化转型反应釜内侧，晶化转型反应釜在外围夹套的冷却作用下降温到85℃，搅拌桨搅拌速度为500r/min，高硫渣矿浆酸度为90g/L，在晶化转型反应釜内经过定向晶化转型，最终得到粒度均匀的转型产品。Put the high-sulfur slag in the heater to heat to obtain the high-sulfur slag slurry, which enters the inner side of the crystallization transformation reactor through the circulation pipe and the central down pipe of the crystallization transformation reactor, and the crystallization transformation reactor cools down under the cooling effect of the outer jacket At 85°C, the stirring speed of the stirring blade is 500r/min, and the acidity of the high-sulfur slag pulp is 90g/L. After directional crystallization transformation in the crystallization transformation reactor, a transformation product with uniform particle size is finally obtained.
结论：经过粒度分析仪测定，单质硫颗粒粒径分布在2-120μm，体积中值直径d(0.5)＝36μm。Conclusion: As determined by the particle size analyzer, the particle size distribution of elemental sulfur particles is 2-120 μm, and the volume median diameter d(0.5)=36 μm.
实施例2Example 2
将高硫渣置于加热器中加热获得高硫渣矿浆，通过循环管和晶化转型反应釜中央下行管进入晶化转型反应釜内侧，晶化转型反应釜在外围夹套的冷却作用下降温到100℃，搅拌桨搅拌速度为100r/min，高硫渣矿浆酸度为75g/L，在晶化转型反应釜内经过定向晶化转型，最终得到粒度均匀的转型产品。Put the high-sulfur slag in the heater to heat to obtain the high-sulfur slag slurry, which enters the inner side of the crystallization transformation reactor through the circulation pipe and the central down pipe of the crystallization transformation reactor, and the crystallization transformation reactor cools down under the cooling effect of the outer jacket At 100°C, the stirring speed of the stirring paddle is 100r/min, and the acidity of the high-sulfur slag pulp is 75g/L. After directional crystallization transformation in the crystallization transformation reactor, a transformation product with uniform particle size is finally obtained.
结论：经过粒度分析仪测定，单质硫颗粒粒径分布在5-110μm，体积中值直径d(0.5)＝30μm。Conclusion: As determined by the particle size analyzer, the particle size distribution of elemental sulfur particles is 5-110 μm, and the volume median diameter d(0.5)=30 μm.
实施例3Example 3
将高硫渣置于加热器中加热获得高硫渣矿浆，通过循环管和晶化转型反应釜中央下行管进入晶化转型反应釜内侧，晶化转型反应釜在外围夹套的冷却作用下降温到110℃，搅拌桨搅拌速度为250r/min，高硫渣矿浆酸度为80g/L，在晶化转型反应釜内经过定向晶化转型，最终得到粒度均匀的转型产品。Put the high-sulfur slag in the heater to heat to obtain the high-sulfur slag slurry, which enters the inner side of the crystallization transformation reactor through the circulation pipe and the central down pipe of the crystallization transformation reactor, and the crystallization transformation reactor cools down under the cooling effect of the outer jacket At 110°C, the stirring speed of the stirring paddle is 250r/min, and the acidity of the high-sulfur slag pulp is 80g/L. After directional crystallization transformation in the crystallization transformation reactor, a transformation product with uniform particle size is finally obtained.
结论：经过粒度分析仪测定，单质硫颗粒粒径分布在5-145μm，体积中值直径d(0.5)＝41μm。Conclusion: As determined by the particle size analyzer, the particle size distribution of elemental sulfur particles is 5-145 μm, and the volume median diameter d(0.5)=41 μm.
以上所述的实施例仅是对本发明的优选方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通技术人员对本发明的技术方案做出的各种变形和改进，均应落入本发明权利要求书确定的保护范围内。The above-mentioned embodiments are only to describe the preferred mode of the present invention, and are not intended to limit the scope of the present invention. Variations and improvements should fall within the scope of protection defined by the claims of the present invention.
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