CN111591965A - A kind of hemi-dihydrate phosphoric acid rapid extraction and crystallization production system and process - Google Patents
A kind of hemi-dihydrate phosphoric acid rapid extraction and crystallization production system and process Download PDFInfo
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 53
- 230000008025 crystallization Effects 0.000 title claims abstract description 53
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 title claims abstract description 17
- 230000008569 process Effects 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000003595 mist Substances 0.000 claims abstract description 19
- 238000007789 sealing Methods 0.000 claims abstract description 19
- 239000007791 liquid phase Substances 0.000 claims abstract description 18
- 239000012071 phase Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims description 48
- 239000007789 gas Substances 0.000 claims description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 16
- 150000004683 dihydrates Chemical class 0.000 claims description 14
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 10
- 239000003546 flue gas Substances 0.000 claims description 10
- 230000009471 action Effects 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 239000002367 phosphate rock Substances 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 239000010440 gypsum Substances 0.000 claims description 5
- 229910052602 gypsum Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000005201 scrubbing Methods 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- DWSKLNHACTWZQD-UHFFFAOYSA-N O.O.O.O.O.P(=O)(O)(O)O.P(=O)(O)(O)O Chemical compound O.O.O.O.O.P(=O)(O)(O)O.P(=O)(O)(O)O DWSKLNHACTWZQD-UHFFFAOYSA-N 0.000 claims 2
- 238000001704 evaporation Methods 0.000 abstract description 6
- 230000008020 evaporation Effects 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- JIUIIWVYHWSFAZ-UHFFFAOYSA-N ac1o0v2m Chemical compound O.O.O.O.O JIUIIWVYHWSFAZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Inorganic materials [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000243 solution Substances 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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
- C01B25/228—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen one form of calcium sulfate being formed and then converted to another form
- C01B25/229—Hemihydrate-dihydrate process
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明公开了一种半水‑二水法磷酸快速萃取结晶生产系统及工艺，包括溶解槽和结晶槽，溶解槽的容积为结晶槽的2～4倍，结晶槽上连接有闪蒸分离器，闪蒸分离器底端的液相出口连接有闪蒸分离液封槽，闪蒸分离液封槽的上部通过管道与结晶槽连通；闪蒸分离液封槽的下部通过半水给料泵连接有半水过滤装置，半水过滤装置上连接有转化槽，转化槽通过二水给料泵连接有二水过滤装置；闪蒸分离器顶端的气相出口连通有雾沫分离器，雾沫分离器下端的液相出口连通闪蒸分离液封槽，雾沫分离器上端的气相出口连接有闪蒸洗涤系统。该系统和工艺可大幅缩短全系统物料停留时间，缩减幅度高达50%，有助于增加产量，降低能耗和生产成本，适用于连续大规模生产。
The invention discloses a production system and process for rapid extraction and crystallization of phosphoric acid by hemi-dihydrate method, comprising a dissolving tank and a crystallization tank. The volume of the dissolving tank is 2 to 4 times that of the crystallization tank, and a flash separator is connected to the crystallization tank. The liquid phase outlet at the bottom of the flash separator is connected with a flash separation liquid sealing tank, the upper part of the flash separation liquid sealing tank is connected with the crystallization tank through a pipeline; the lower part of the flash separation liquid sealing tank is connected with a semi-water feed pump. The semi-water filter device is connected with a conversion tank, and the conversion tank is connected with a two-water filter device through a two-water feed pump; the gas phase outlet at the top of the flash separator is connected with a mist separator, and the lower end of the mist separator is connected The liquid phase outlet of the liquid phase outlet is connected to the flash separation liquid sealing tank, and the gas phase outlet at the upper end of the mist separator is connected with a flash evaporation washing system. The system and process can greatly reduce the material residence time of the whole system by up to 50%, which helps to increase production, reduce energy consumption and production costs, and is suitable for continuous large-scale production.
Description
技术领域technical field
本发明属于磷酸生产技术领域，具体涉及一种半水-二水法磷酸快速萃取结晶生产系统及工艺。The invention belongs to the technical field of phosphoric acid production, and in particular relates to a production system and process for rapid extraction and crystallization of phosphoric acid by hemi-dihydrate method.
背景技术Background technique
磷酸的工业生产方法可分为两大类，一类是热法生产，另一类是湿法生产。湿法生产是用强无机酸（如硫酸、盐酸、硝酸、氟硅酸等）分解磷矿而制取的磷酸。湿法生产成本较低，但产物中夹带有一定杂质，目前主要用于生产磷肥，也部分取代热法生产中低端磷产品原料。The industrial production methods of phosphoric acid can be divided into two categories, one is thermal production and the other is wet production. Wet production is phosphoric acid produced by decomposing phosphate rock with strong inorganic acids (such as sulfuric acid, hydrochloric acid, nitric acid, fluorosilicic acid, etc.). The wet production cost is low, but the product contains certain impurities. Currently, it is mainly used for the production of phosphate fertilizers, and also partially replaces the raw materials of low-end phosphorus products produced by the thermal method.
在反应温度、硫酸添加量等条件不同时，硫酸钙结晶形态通常有二水物CaSO4·2H2O、半水物α-CaSO4·1/2H2O和无水物CaSO4三类。其中半水-二水法生产工艺主要是控制反应条件，使物料先结晶成半水硫酸钙，再伴随高浓度磷酸，并改变反应条件，半水硫酸钙重新结晶成二水硫酸钙，此方法即为半水-二水法工艺。When the reaction temperature and the amount of sulfuric acid added are different, the crystal forms of calcium sulfate usually have three types: dihydrate CaSO 4 ·2H 2 O, hemihydrate α-CaSO 4 ·1/2H 2 O and anhydrous CaSO 4 . Among them, the production process of the hemihydrate-dihydrate method is mainly to control the reaction conditions, so that the material is first crystallized into calcium sulfate hemihydrate, and then accompanied by high-concentration phosphoric acid, and the reaction conditions are changed, and the calcium sulfate hemihydrate is recrystallized into calcium sulfate dihydrate. This method That is, the semi-water-dihydrate process.
众所周知，目前国内湿法磷酸半水-二水法生产装置，全系统物料停留时间大多控制在9.5～14h，造成规模产能的半水-二水法萃取槽占地面积大、装置运行能耗高，目前也没有很好的解决这一难题的方法。As we all know, in the current domestic wet-process phosphoric acid hemi-dihydrate production equipment, the residence time of materials in the whole system is mostly controlled at 9.5 to 14 hours, resulting in large-scale production capacity of the semi-water-dihydrate extraction tank with large footprint and high energy consumption for device operation. , and there is currently no good solution to this problem.
发明内容SUMMARY OF THE INVENTION
本发明提供了一种半水-二水法磷酸快速萃取结晶生产系统及工艺，目的在于解决现有磷酸生产物料停留时间长，生产速度较慢的问题。The invention provides a production system and process for rapid extraction and crystallization of phosphoric acid by hemi-dihydrate method, aiming at solving the problems of long residence time and slow production speed of existing phosphoric acid production materials.
为此，本发明采用如下技术方案：For this reason, the present invention adopts following technical scheme:
一种半水-二水法磷酸快速萃取结晶生产系统，包括溶解槽、结晶槽、半水料浆泵、闪蒸分离器、雾沫分离器，所述溶解槽的容积为结晶槽的2～4倍，结晶槽通过溢流管与溶解槽连接，结晶槽与溶解槽之间还连接有回流管和半水料浆循环泵，溶解槽和结晶槽内均设有搅拌装置；A hemi-dihydrate phosphoric acid rapid extraction and crystallization production system, comprising a dissolving tank, a crystallization tank, a hemi-aqueous slurry pump, a flash separator, and a mist separator, wherein the volume of the dissolving tank is 2 to 2 of the crystallization tank. 4 times, the crystallizing tank is connected with the dissolving tank through the overflow pipe, a return pipe and a semi-water slurry circulating pump are also connected between the crystallizing tank and the dissolving tank, and both the dissolving tank and the crystallizing tank are equipped with stirring devices;
所述闪蒸分离器的顶部设有气相出口、上部设有进料口、底部设有液相出口，所述半水料浆泵的一端通过管道连接结晶槽、另一端连接闪蒸分离器的进料口，所述闪蒸分离器的进料口处设有料浆喷射装置；闪蒸分离器的气相出口连接雾沫分离器，闪蒸分离器的液相出口连接闪蒸分离液封槽，所述闪蒸分离液封槽内的料浆一部分经管道通入结晶槽内、一部分经半水给料泵送入半水过滤装置；所述半水过滤装置连接有转化槽，所述转化槽通过二水给料泵连接有二水过滤装置；The top of the flash separator is provided with a gas phase outlet, the upper part is provided with a feed inlet, and the bottom is provided with a liquid phase outlet, one end of the semi-aqueous slurry pump is connected to the crystallization tank through a pipeline, and the other end is connected to the flash separator. The feed port, the feed port of the flash separator is provided with a slurry injection device; the gas phase outlet of the flash separator is connected to the mist separator, and the liquid phase outlet of the flash separator is connected to the flash separation liquid sealing tank, A part of the slurry in the flash separation liquid sealing tank is passed into the crystallization tank through a pipeline, and a part is sent to a semi-aqueous filter device through a semi-water feed pump; the semi-aqueous filter device is connected with a conversion tank, and the conversion tank A secondary water filter device is connected through the secondary water feed pump;
所述雾沫分离器的侧部设有进气口、顶部设有气相出口、底部设有液相出口，雾沫分离器的液相出口连接闪蒸分离液封槽、气相出口连接闪蒸洗涤系统。The side part of the mist separator is provided with an air inlet, the top is provided with a gas phase outlet, and the bottom is provided with a liquid phase outlet, the liquid phase outlet of the mist separator is connected to the flash separation liquid sealing tank, and the gas phase outlet is connected to the flash washing system.
进一步地，所述溶解槽和结晶槽的上方连接有烟气回收管，所述烟气回收管的另一端连接烟气洗涤系统。Further, a flue gas recovery pipe is connected above the dissolving tank and the crystallization tank, and the other end of the flue gas recovery pipe is connected to a flue gas washing system.
进一步地，所述转化槽内设有搅拌装置。Further, a stirring device is provided in the conversion tank.
一种半水-二水法磷酸快速萃取结晶生产工艺，采用上述的半水-二水法磷酸快速萃取结晶生产系统，其具体过程如下：A hemi-dihydrate phosphoric acid rapid extraction and crystallization production process adopts the above-mentioned hemi-dihydrate phosphoric acid rapid extraction and crystallization production system, and its specific process is as follows:
将粉碎后的磷矿原料和浓硫酸加入溶解槽中，充分搅拌使物料循环进行反应，磷矿在浓硫酸的分解作用下反应生成半水硫酸钙；反应后料浆溢流至结晶槽内，向结晶槽中加入过量浓硫酸，料浆在过量浓硫酸和活性二氧化硅的作用下促使半水硫酸钙晶体不断增长；控制物料在溶解槽内的停留时间为2～2.5h，结晶槽内的停留时间为1～1.5h；The pulverized phosphate rock raw material and concentrated sulfuric acid are added into the dissolving tank, and the materials are fully stirred to react in a cycle, and the phosphate rock reacts under the decomposition of concentrated sulfuric acid to form calcium sulfate hemihydrate; Add excess concentrated sulfuric acid into the crystallization tank, and the slurry promotes the continuous growth of calcium sulfate hemihydrate crystals under the action of excess concentrated sulfuric acid and active silica; control the residence time of the material in the dissolution tank to be 2-2.5h, and in the crystallization tank The residence time is 1 ~ 1.5h;
结晶槽内的料浆通过半水料浆泵进入闪蒸分离器进行降温冷却，控制闪蒸分离器压力10～15KPa，进出口温差10～25℃；料浆通过喷射装置喷入闪蒸分离器内，冷却后的含氟气体经气相出口进入雾沫分离器进行进一步的气液分离，分离后的气体进入尾气洗涤系统；冷却后的料浆在重力作用下由液相出口流至闪蒸分离液封槽中，闪蒸分离液封槽中的料浆一部分回流至结晶槽中、另一部分经半水给料泵送入半水过滤装置进行过滤，过滤后得到半水石膏和滤酸，滤酸即为产品磷酸，半水石膏进入转化槽；转化槽中，半水石膏在浓硫酸的作用下进行二水反应，反应后料浆经二水给料泵送入二水过滤装置进行过滤，分离得到二水石膏，控制物料在转化槽内的反应时间为1.5～2h，控制物料在系统内的总停留时间为5.5～6h。The slurry in the crystallization tank enters the flash separator for cooling and cooling through the semi-water slurry pump, and the pressure of the flash separator is controlled to 10-15KPa, and the temperature difference between the inlet and the outlet is 10-25°C; the slurry is sprayed into the flash separator through a spray device. Inside, the cooled fluorine-containing gas enters the mist separator through the gas phase outlet for further gas-liquid separation, and the separated gas enters the tail gas scrubbing system; the cooled slurry flows from the liquid phase outlet to flash separation under the action of gravity In the liquid sealing tank, a part of the slurry in the flash separation liquid sealing tank is returned to the crystallization tank, and the other part is sent to the hemi-water filtration device by the hemi-water feed pump for filtration. After filtration, hemihydrate gypsum and filtered acid are obtained. The acid is the product phosphoric acid, and the hemihydrate gypsum enters the conversion tank; in the conversion tank, the hemihydrate gypsum is reacted with dihydrate under the action of concentrated sulfuric acid, and the slurry after the reaction is sent to the dihydrate filtration device through the dihydrate feed pump for filtration. Dihydrate gypsum is obtained by separation, the reaction time of the control material in the conversion tank is 1.5-2h, and the total residence time of the control material in the system is 5.5-6h.
进一步地，所述溶解槽和结晶槽内的半水料浆固液比为2：1～3：1。Further, the solid-to-liquid ratio of the hemi-water slurry in the dissolution tank and the crystallization tank is 2:1 to 3:1.
本发明的有益效果在于：The beneficial effects of the present invention are:
1.该系统和工艺可大幅缩短全系统物料停留时间，缩减幅度高达50%，有助于增加产量，降低能耗和生产成本，适用于连续大规模生产；1. The system and process can greatly shorten the material residence time of the whole system, and the reduction rate is as high as 50%, which helps to increase the output, reduce energy consumption and production cost, and is suitable for continuous large-scale production;
2.该工艺可大大减少成品磷酸中的淤浆含量，有效提高磷酸品质，可取代部分低等级热法磷酸产品；2. This process can greatly reduce the slurry content in the finished phosphoric acid, effectively improve the quality of phosphoric acid, and can replace some low-grade thermal phosphoric acid products;
3.该工艺中的水循环利用，减少排放，减小水资源的消耗。3. The water in this process is recycled to reduce emissions and reduce water consumption.
附图说明Description of drawings
图1是本发明的系统原理图；Fig. 1 is the system principle diagram of the present invention;
图中：1-溶解槽，2-结晶槽，3-半水料浆泵，4-闪蒸分离器，5-雾沫分离器，6-闪蒸分离液封槽，7-半水给料泵，8-半水料浆循环泵，9-半水过滤装置，10-转化槽，11-二水给料泵，12-二水过滤装置。In the picture: 1- Dissolution tank, 2- Crystallization tank, 3- Semi-water slurry pump, 4- Flash separator, 5- Mist separator, 6- Flash separation liquid sealing tank, 7- Semi-water feed Pump, 8-semi-water slurry circulating pump, 9-semi-water filtration device, 10-transformation tank, 11- two-water feed pump, 12- two-water filter device.
具体实施方式Detailed ways
下面结合附图对本发明作进一步说明：The present invention will be further described below in conjunction with the accompanying drawings:
如图所示，一种半水-二水法磷酸快速萃取结晶生产系统，包括溶解槽1和结晶槽2，溶解槽1的容积为结晶槽2的2～3倍，结晶槽2通过溢流管与溶解槽1连接。由于半水反应在溶解槽1内进行，溶解槽1的半水料浆的P2O5浓度高达38%以上，加之杂质离子的影响，导致反应料浆粘度大，饱和度高，搅拌效果差，反应速度慢。增大溶解槽1的容积后，可延长反应时间，获得较高的萃取率，结晶槽2内的半水结晶在适当过量的SO3条件下会进一步长大，使其转化成易于过滤的半水结晶。As shown in the figure, a hemi-dihydrate phosphoric acid rapid extraction and crystallization production system includes a dissolving
结晶槽2与溶解槽1之间还连接有回流管和半水料浆循环泵8，半水料浆循环泵8可将结晶槽2内的料浆通过回流管输送至溶解槽1中。溶解槽1和结晶槽2内均设有搅拌装置，溶解槽1和结晶槽2的上方还连接有烟气回收管道，烟气回收管道的另一端连接有烟气尾洗系统。Between the crystallization tank 2 and the dissolving
闪蒸分离器4的顶部设有气相出口、上部设有进料口、底部设有液相出口，半水料浆泵3的一端通过管道连接结晶槽2、另一端连接闪蒸分离器4的进料口，闪蒸分离器4的进料口处设有料浆喷射装置；闪蒸分离器4的气相出口连接雾沫分离器5，闪蒸分离器4的液相出口连接闪蒸分离液封槽6，闪蒸分离液封槽6内的料浆一部分经管道通入结晶槽2内、一部分经半水给料泵7送入半水过滤装置；半水过滤装置连接有转化槽10，转化槽10内设有搅拌装置，转化槽10通过二水给料泵11连接有二水过滤装置12。The top of the
雾沫分离器5的侧部设有进气口、顶部设有气相出口、底部设有液相出口，雾沫分离器5的液相出口连接闪蒸分离液封槽6、气相出口连接闪蒸洗涤系统。The side part of the
一种半水-二水法磷酸快速萃取结晶生产工艺，该工艺依托上述设备进行，该工艺的步骤和原理如下：将粉碎后的磷矿原料和浓硫酸加入溶解槽1中，充分搅拌使物料循环进行反应，磷矿在浓硫酸的分解作用下反应生成半水硫酸钙。反应式如下：A hemi-dihydrate phosphoric acid rapid extraction and crystallization production process, the process is carried out by relying on the above-mentioned equipment, and the steps and principles of the process are as follows: the crushed phosphate rock raw materials and concentrated sulfuric acid are added into a dissolving
Ca5F(PO4)3+5H2SO4+2*1/2H2O＝3H3PO4+5CaSO4·1/2H2O ↓+HF↑Ca 5 F(PO 4 ) 3 +5H 2 SO 4 +2*1/2H 2 O=3H 3 PO 4 +5CaSO 4 ·1/2H 2 O ↓+HF↑
反应后料浆溢流至结晶槽2内，向结晶槽2中加入过量浓硫酸，料浆在过量浓硫酸和活性二氧化硅的作用下促使半水硫酸钙晶体不断增长；控制物料在溶解槽内的停留时间为2～2.5h，结晶槽内的停留时间为1～1.5h。After the reaction, the slurry overflows into the crystallization tank 2, and excess concentrated sulfuric acid is added to the crystallization tank 2, and the slurry promotes the continuous growth of calcium sulfate hemihydrate crystals under the action of the excess concentrated sulfuric acid and active silica; control the material in the dissolution tank. The residence time in the crystallization tank is 2-2.5h, and the residence time in the crystallization tank is 1-1.5h.
结晶槽2内的料浆通过半水料浆泵3进入闪蒸分离器4进行降温冷却，控制闪蒸分离器4压力10～15KPa；料浆通过喷射装置喷入闪蒸分离器4内。使料浆在闪蒸分离器4内形成液膜双效蒸发，既增大料浆蒸发面积，又消除了料浆急剧蒸发降温出现的爆沸现象；同时降低了真空度，减少了蒸发气体伴随的雾沫夹带量。经过闪蒸分离器4后，半水料浆由95℃以上降低至70℃以下，可将半水料浆温差控制在25℃以内。冷却后的含氟气体经气相出口进入雾沫分离器5进行进一步的气液分离，分离后的气体进入尾气洗涤系统；冷却后的料浆在重力作用下由液相出口流至闪蒸分离液封槽6中，闪蒸分离液封槽6中的料浆一部分回流至结晶槽中、另一部分经半水给料泵7送入半水过滤装置进行过滤，过滤后得到半水石膏和滤酸，滤酸即为产品磷酸，半水石膏进入转化槽10；转化槽10中，半水石膏在浓硫酸的作用下进行二水反应。反应式如下：The slurry in the crystallization tank 2 enters the
CaSO4·1/2H2O+1/2H2O＝CaSO4·2H2O↓+QCaSO 4 ·1/2H 2 O+1/2H 2 O=CaSO 4 ·2H 2 O↓+Q
反应后料浆经二水给料泵送入二水过滤装置进行过滤，分离得到二水石膏，控制物料在转化槽内的反应时间为1.5～2h，控制物料在系统内的总停留时间为5.5～6h。After the reaction, the slurry is sent to the dihydrate filtration device by the dihydrate feed pump for filtration, and the dihydrate gypsum is separated to obtain the dihydrate gypsum. ~6h.
与常规工艺之处在于，闪蒸分离器4的入口位于上部，料浆进入后从上向下移动，更有利于气液分离，可大大提高分离速度和分离效果。系统中的浓硫酸为98.5%wt的浓硫酸，采用本发明工艺产出的磷酸浓度在45%wt以上，产出石膏干基P2O5的含量在0.25%wt以下，反应总时间缩短至5.5～6h，技术效果非常显著。Compared with the conventional process, the inlet of the
需要说明的是，以上仅是本发明的部分实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和替换，这些改进和替换也应视为本发明的保护范围。It should be noted that the above are only some embodiments of the present invention. It should be pointed out that for those skilled in the art, some improvements and replacements can be made without departing from the technical principles of the present invention. Improvement and replacement should also be regarded as the protection scope of the present invention.
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