CN105129852A - Efficient self-recycling system for continuously preparing sodium bichromate by wet method - Google Patents
Efficient self-recycling system for continuously preparing sodium bichromate by wet method Download PDFInfo
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- CN105129852A CN105129852A CN201510589639.2A CN201510589639A CN105129852A CN 105129852 A CN105129852 A CN 105129852A CN 201510589639 A CN201510589639 A CN 201510589639A CN 105129852 A CN105129852 A CN 105129852A
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- feed liquid
- concentrating unit
- oxygen
- phase oxidation
- steam
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- KIEOKOFEPABQKJ-UHFFFAOYSA-N Sodium dichromate Chemical compound [Na+].[Na+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KIEOKOFEPABQKJ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000004064 recycling Methods 0.000 title abstract 2
- 239000007788 liquid Substances 0.000 claims abstract description 82
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 64
- 239000001301 oxygen Substances 0.000 claims abstract description 60
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 60
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000007791 liquid phase Substances 0.000 claims abstract description 51
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 38
- 238000010009 beating Methods 0.000 claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 28
- 238000002425 crystallisation Methods 0.000 claims abstract description 21
- 230000005712 crystallization Effects 0.000 claims abstract description 21
- 239000011734 sodium Substances 0.000 claims abstract description 20
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 19
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 14
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 14
- 238000007701 flash-distillation Methods 0.000 claims description 30
- 238000010000 carbonizing Methods 0.000 claims description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000005255 carburizing Methods 0.000 claims description 19
- 239000003153 chemical reaction reagent Substances 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 17
- 238000010924 continuous production Methods 0.000 claims description 16
- VAIONUZUJWZJSR-UHFFFAOYSA-J C([O-])(O)=O.[Na+].[Cr+3].C([O-])(O)=O.C([O-])(O)=O.C([O-])(O)=O Chemical compound C([O-])(O)=O.[Na+].[Cr+3].C([O-])(O)=O.C([O-])(O)=O.C([O-])(O)=O VAIONUZUJWZJSR-UHFFFAOYSA-J 0.000 claims description 14
- 229910000604 Ferrochrome Inorganic materials 0.000 claims description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 11
- 238000001149 thermolysis Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 7
- 239000001187 sodium carbonate Substances 0.000 claims description 7
- 238000007664 blowing Methods 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000001256 steam distillation Methods 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 125000004435 hydrogen atoms Chemical class [H]* 0.000 claims description 3
- 229910052596 spinel Inorganic materials 0.000 claims description 3
- 239000011029 spinel Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 21
- 239000011651 chromium Substances 0.000 abstract description 19
- 230000003647 oxidation Effects 0.000 abstract description 17
- VYZAMTAEIAYCRO-UHFFFAOYSA-N chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 13
- 238000003763 carbonization Methods 0.000 abstract description 13
- 229910052804 chromium Inorganic materials 0.000 abstract description 13
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 9
- 239000000047 product Substances 0.000 abstract description 6
- 239000006227 byproduct Substances 0.000 abstract description 5
- 238000001704 evaporation Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000004615 ingredient Substances 0.000 abstract 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 27
- 238000004519 manufacturing process Methods 0.000 description 16
- 239000002893 slag Substances 0.000 description 16
- 238000000034 method Methods 0.000 description 14
- 230000001590 oxidative Effects 0.000 description 14
- 230000020477 pH reduction Effects 0.000 description 9
- 235000017550 sodium carbonate Nutrition 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- 230000001131 transforming Effects 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 150000001718 carbodiimides Chemical class 0.000 description 6
- 235000008504 concentrate Nutrition 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000011268 mixed slurry Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000007599 discharging Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 4
- 235000011089 carbon dioxide Nutrition 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- 238000005304 joining Methods 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- PXLIDIMHPNPGMH-UHFFFAOYSA-N Sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking Effects 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 230000000875 corresponding Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000001502 supplementation Effects 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 241000143392 Oar Species 0.000 description 1
- 206010039509 Scab Diseases 0.000 description 1
- 235000012970 cakes Nutrition 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- -1 chromite Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000014666 liquid concentrate Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003245 working Effects 0.000 description 1
Classifications
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses an efficient self-recycling system for continuously preparing sodium bichromate by a wet method. The system comprises a beating tank, an oxygen supply device, and a first delivery pump, a preheating device, a liquid-phase oxidation reaction device, a flash evaporation device, a first separation device, a first concentration device, a carbonization device, a second separation device, an electrolytic bath, a second concentration device, a cooling crystallization device and a centrifugation device, which are sequentially connected with the beating tank through a feed liquid delivery pipeline, wherein the oxygen supply device is used for introducing oxygen into the liquid-phase oxidation reaction device; CO2 generated by preheating decomposition, CO2 and steam, which are generated by oxidation, and steam generated by flash evaporation can be delivered to the concentration devices, the steam is used for feed liquid concentration, and CO2 is led into the carbonization device for carbonization reaction; chromium-containing sodium bicarbonate obtained by separation in the second separation device can be delivered to the beating tank as an ingredient. According to the system, the byproducts CO2 and steam are used for carbonization and feed liquid concentration and the product sodium bicarbonate is used as the ingredient, so that sodium, CO2 and heat are efficiently self-recycled, and energy waste is reduced.
Description
Technical field
The invention belongs to the preparation field of sodium dichromate, particularly a kind of system of high-efficiency self-circulation wet method continuous production sodium dichromate.
Background technology
Sodium dichromate is one of important Inorganic Chemicals as chromic salts basic product, occupies critical role, have purposes very widely in national economy.Its traditional processing technology front end adopts the raw materials such as chromite, soda ash, return slag in rotary kiln in more than 1000 DEG C calcinings, roasting grog obtains chromium acid sodium solution through leaching, rear end adopts sulfuric acid acidation Sodium chromate to obtain sodium dichromate solution, obtains sodium dichromate product through evaporative crystallization dehydration.But the problems such as this production technique device exists serious secondary pollution, the wasting of resources, energy consumption is high, production efficiency is low, cause high risks to local environment, the Sustainable development of serious restriction Chrome Salt Industry.Therefore, be solve the defect that traditional technology device exists, it is extremely urgent to seek new Technology.
Disclose in CN201210466756 " method that single stage method prepares sodium dichromate ", the preparation mentioning sodium dichromate in document adopts chrome iron powder, under certain temperature and pressure, carries out hydrothermal oxidization reaction in the presence of oxygen, under carbon dioxide catalyst exists containing the dispersion of soda and water, sodium dichromate solution is obtained through supplementing acidifying, this technique breaches traditional technology, substantially reduce technical process, and energy consumption is low, production environment is friendly, is the favourable production ways preparing sodium dichromate.But this technique has great requirement to production unit, and need calcine by product sodium bicarbonate, hand labor intensity increases, and production equipment cannot meet continuous seepage, and resource cannot be fully exploited, and the heat recovery and utilization rate produced is low.Therefore, improve new production equipment and become trend.
Summary of the invention
An object of the present invention is to solve at least the problems referred to above and/or defect, and the advantage will illustrated at least is below provided.
A further object of the invention is to provide a kind of system of high-efficiency self-circulation wet method continuous production sodium dichromate, it achieves the high-efficiency self-circulation preparing sodium element, carbonic acid gas and heat energy in sodium dichromate process and utilizes, decrease the waste of the energy, fully utilize the by product produced in technological process.
In order to realize, according to these objects of the present invention and other advantages, providing a kind of system of high-efficiency self-circulation wet method continuous production sodium dichromate, comprising:
Making beating tank, is provided with the feeding mouth of input oxide spinel hydrogen sodium, ferrochrome powder, sodium carbonate and water;
Making beating tank connects the first transferpump, primary heater unit, liquid phase oxidation reaction device, flash distillation plant, the first tripping device, the first concentrating unit, carbonizing plant, the second tripping device, electrolyzer, the second concentrating unit, equipment of crystallisation by cooling and centrifugal device successively by feed liquid transport pipe;
Apparatus of oxygen supply, it is connected by pipeline with described liquid phase oxidation reaction device; For passing into oxygen to described liquid phase oxidation reaction device;
Wherein, the CO that in described primary heater unit, pre-thermolysis produces
2, be oxidized the CO of generation in liquid phase oxidation reaction device
2be delivered to the first concentrating unit and the second concentrating unit with the steam produced in steam and flash distillation plant by gas transmission pipeline, steam is used for feed liquid and concentrates; CO
2gas respectively from the blowing mouth of the first concentrating unit and the second concentrating unit export and dewatered by freeze drier, CO
2described carbonizing plant is inputted for carburizing reagent after compressor compresses; What in described second tripping device, separation obtained is used as to prepare burden by the feeding mouth of Cemented filling to making beating tank containing chromium sodium bicarbonate.
Preferably, the feeding mouth of described making beating tank has four, is respectively sodium bicarbonate entrance, ferrochrome powder entrance, sodium carbonate entrance and water inlet.
Preferably, described apparatus of oxygen supply comprises oxygen air separation facility, oxygen compressor and oxygen surge tank, oxygen compressor is communicated with oxygen surge tank with described oxygen air separation facility respectively, and described oxygen surge tank and described liquid phase oxidation reaction device pass through pipeline communication.
Preferably, described first concentrating unit is provided with the first concentrating unit steam drain, described second concentrating unit is provided with the second concentrating unit steam drain.
Preferably, described first tripping device and the second tripping device are vertical automatic plate frame press filter.
Preferably, described primary heater unit is provided with the thermometer for detecting temperature in primary heater unit.
Preferably, described flash distillation plant is level Four flash tank.
Preferably, the feed liquid transport pipe between described liquid phase oxidation reaction device and flash distillation plant connects the second transferpump; Feed liquid transport pipe between described flash distillation plant and the first tripping device connects the 3rd transferpump; Feed liquid transport pipe between described first concentrating unit and carbonizing plant connects the 4th transferpump; Feed liquid transport pipe between described carbonizing plant and the second tripping device connects the 5th transferpump; Feed liquid transport pipe between described electrolyzer and the second concentrating unit connects the 6th transferpump; Described second concentrating unit is connected the 7th transferpump with on the feed liquid transport pipe between equipment of crystallisation by cooling; Described equipment of crystallisation by cooling is connected the 8th transferpump with on the feed liquid transport pipe between centrifugal device.
The present invention at least comprises following beneficial effect:
(1) cleaner production: complete sodium dichromate whole process wet method continuous production Technology, revolutionize traditional rotary kiln calcining production model, realize sodium dichromate manufacturing process system totally-enclosed, three-waste free discharge, reduce environmental pollution, reach plant-scale sodium dichromate cleaner production.
(2) realize resource high-efficiency circulation comprehensive and utilize system: in the present invention, the sodium bicarbonate that rear end carbonization workshop section produces passes into front end ferrochrome liquid-phase oxidation workshop section through transport pipe, the carbonic acid gas of oxidizing reaction by-product and steam are used for rear end Sodium chromate carbonization and feed liquid concentrates, achieve sodium element, carbonic acid gas and heat energy high-efficiency self-circulation to utilize, reduce the waste of the energy, the by product that comprehensive utilization process process produces.
(3) sodium dichromate manufacturing cost is reduced: the present invention changes the mode such as reaction, filtration, evaporation of chromic salts tradition extensive style, introduce also independent development key device and the support equipments such as vertical automatic plate frame press filter, high-efficiency evaporator, oxidation reactor, carbonization reactor, chemical pump automatic cooling water control system, system solve that sodium bicarbonate " scabs ", the problem such as equipment attrition is large, chromium yield is low, significantly reduce sodium dichromate manufacturing cost.
Part is embodied by explanation below by other advantage of the present invention, target and feature, part also will by research and practice of the present invention by those skilled in the art is understood.
Accompanying drawing illustrates:
Fig. 1 is the structural representation of the system of high-efficiency self-circulation wet method continuous production sodium dichromate of the present invention;
Fig. 2 is the structural representation of the horizontal reacting still described in one embodiment of the invention.
Embodiment:
Below in conjunction with accompanying drawing, the present invention is described in further detail, can implement according to this with reference to specification sheets word to make those skilled in the art.
Should be appreciated that used hereinly such as " to have ", other element one or more do not allotted in " comprising " and " comprising " term or the existence of its combination or interpolation.
Fig. 1 shows the system of a kind of high-efficiency self-circulation wet method continuous production sodium dichromate of the present invention, comprising:
Making beating tank 5, is provided with the sodium bicarbonate entrance 1 of input raw material, ferrochrome powder entrance 2, sodium carbonate entrance 3 and water inlet 4;
Making beating tank 5 connects the first transferpump 7, primary heater unit 8, liquid phase oxidation reaction device 17, flash distillation plant 21, first tripping device 26, first concentrating unit 30, carbonizing plant 35, second tripping device 39, electrolyzer 43, second concentrating unit 46, equipment of crystallisation by cooling 51 and centrifugal device 54 successively by feed liquid transport pipe;
Apparatus of oxygen supply 12, it is connected by pipeline with described liquid phase oxidation reaction device 17; For passing into oxygen to described liquid phase oxidation reaction device 17;
Wherein, the CO that in described primary heater unit 8, pre-thermolysis produces
2, be oxidized the CO of generation in liquid phase oxidation reaction device 17
2be delivered to the first concentrating unit 30 and the second concentrating unit 46 with the steam produced in steam and flash distillation plant 21 by gas transmission pipeline 64, the steam transported concentrates for feed liquid; CO
2gas respectively from the first blowing mouth 19 of the first concentrating unit 30 and the second blowing mouth 65 of the second concentrating unit 46 export and dewatered by freeze drier 66, CO
2compressor 67 compresses the described carbonizing plant 35 of rear input for carburizing reagent; What in described second tripping device 39, separation obtained is used as to prepare burden by the sodium bicarbonate entrance 1 of Cemented filling to making beating tank 5 containing chromium sodium bicarbonate.
In this technical scheme, oxide spinel hydrogen sodium, ferrochrome powder, sodium carbonate and water add making beating tank 5 from sodium bicarbonate entrance 1, ferrochrome powder entrance 2, sodium carbonate entrance 3 and water inlet 4 respectively and pull an oar, feed liquid after making beating exports from slurry outlet 6, after the first transferpump 7 is delivered to primary heater unit feeding mouth 9 from feed liquid transport pipe, enter primary heater unit 8, the feed liquid of preheating is delivered to after liquid phase oxidation reaction device feeding mouth 11 through feed liquid transport pipe and enters liquid phase oxidation reaction device 17, meanwhile, apparatus of oxygen supply 12 is used for reaction by entering liquid phase oxidation reaction device after oxygen delivery to liquid phase oxidation reaction device oxygen intake 16, the feed liquid produced after reaction in liquid phase oxidation reaction device 17 enters flash distillation plant 21 by flash distillation plant feeding mouth 22 after liquid phase oxidation reaction device discharge port 20 exports, after feed liquid being processed in flash distillation plant 21, after feed liquid being exported from flash distillation plant discharge port 24, enter the first tripping device 26 by the first tripping device feeding mouth 25, in the process, the CO that in described primary heater unit 8, pre-thermolysis produces
2, be oxidized the CO of generation in liquid phase oxidation reaction device 17
2to export respectively by thermal pneumatic outlet 10, liquid phase oxidation reaction device pneumatic outlet 18 and flash distillation plant pneumatic outlet 23 with the steam produced in steam and flash distillation plant 21 and enter the first concentrating unit 30 and the second concentrating unit 46 respectively after be delivered to the first concentrating unit gas inlet 33 and the second concentrating unit gas inlet 48 by gas transmission pipeline 64, steam is used to concentrated feed liquid, be utilized in liquid form after concentrated, achieve the recycle of steam, and CO
2still exist in gaseous form, and then CO
2gas respectively from the first blowing mouth 19 of the first concentrating unit 30 and the second blowing mouth 65 of the second concentrating unit 46 export and dewatered by freeze drier 66, CO
2compressor 67 compresses rear input carbonizing plant gas inlet 36 and enters described carbonizing plant 35 for carburizing reagent, realize the recycle of carbonic acid gas, feed liquid is through solid-liquid separation in the first tripping device 26, and the rich siderochrome slag of the solid filtered to isolate is discharged through rich siderochrome slag outlet 27, and the rich siderochrome slag of discharge washes with water, and washing water can input the water inlet 4 of making beating tank 5 for making beating, realize water circulation use, the feed liquid filtered to isolate is chromium acid sodium solution, feed liquid enters the first concentrating unit 30 by the first concentrating unit feeding mouth 29 and carries out concentration after the first tripping device material liquid outlet 28 exports, can utilize simultaneously and from the steam in liquid-phase oxidation device 17 and flash distillation plant 21, feed liquid be concentrated, feed liquid after concentrated enters carbonizing plant 35 by carbonizing plant feeding mouth 34 and carries out carburizing reagent after the first concentrating unit discharge port 32 exports, and can utilize simultaneously and produce CO from primary heater unit 8 and liquid phase oxidation reaction device 17
2carry out carburizing reagent, realize CO
2recycle, the feed liquid completing carburizing reagent in carbonizing plant 35 enters the second tripping device 39 by the second tripping device feeding mouth 38 after carbonizing plant discharge port 37 exports, feed liquid is separated in the second tripping device 39, what obtain discharges containing the sodium bicarbonate outlet 41 of chromium sodium bicarbonate by the second tripping device 39, and by pipeline, the sodium bicarbonate entrance 1 being delivered to making beating tank 5 containing chromium sodium bicarbonate is used as raw material, realize the recycle of sodium bicarbonate, be separated the feed liquid obtained and enter electrolyzer 43 by electrolyzer feeding mouth 42 after the second tripping device discharge port 40 exports, electrolyzer 43 pairs of feed liquids are carried out electrolysis and are supplemented acidification, improve the acidification rate of feed liquid, the feed liquid of supplementing acidification through electrolysis enters the second concentrating unit 46 by the second concentrating unit feeding mouth 45 and concentrates after electrolyzer discharge port 44 exports, can utilize simultaneously and from the steam in liquid-phase oxidation device 17 and flash distillation plant 21, feed liquid be concentrated, feed liquid after concentrated enters equipment of crystallisation by cooling 51 by equipment of crystallisation by cooling feeding mouth 50 and carries out crystallisation by cooling after the second concentrating unit discharge port 49 exports, the crystal solution obtained enters centrifugal device 54 by centrifugal device feeding mouth 53 and carries out centrifugal treating after crystallization apparatus discharge port 52 output, the feed liquid processed by centrifugal device 54 is deviate from from centrifugal device material liquid outlet 55, the sodium dichromate obtained exports from centrifugal device sodium dichromate outlet 56, obtain sodium dichromate.
In technique scheme, described liquid phase oxidation reaction device 17 is horizontal reacting still, and its structure comprises: kettle 68, and it is the hollow cylinder in horizontal placement, described kettle is provided with opening for feed 11 and discharge port 20, discharge port 20 horizontal by miter angle, and is communicated with by stainless steel tube with hollow cylinder, three over-passs 69, it is inner that it is arranged on described kettle, and kettle internal space is divided into I, II, III and IV chamber along kettle length direction, and I, II, III chamber carries out oxidizing reaction, IV chamber discharging, four agitators 70, it is separately positioned in I, II, III and IV chamber, each agitator forms by agitator arm 71 and the first blade 72 be fixedly connected with agitator arm and the second blade 73, first blade is self-priming, second blade is open type worm gear, agitator arm is connected to a drive unit 74, first blade is arranged on the second blade top, and lower than height first blade of adjacent over-pass, feed liquid is upwards seethed, second blade by material to pressing down, make mixing of materials even like this, and fully can react with oxygen, improve transformation efficiency, wherein, opening for feed 11 and discharge port 20 respectively with described kettle I chamber and IV chamber, and the bottom of II of kettle, III and IV chamber is provided with oxygen intake 16, and oxygen intake 16 is connected with apparatus of oxygen supply 12, oxygen intake 16 place is provided with inserted filtering element stainless steel gas distributor, and aperture is 1 ~ 5 μm effectively can prevent feed blocking, material enters I chamber of kettle by opening for feed, pass into oxygen and stir, material and oxygen is made fully to mix and react, when material reaches I chamber over-pass height, material overflows to II chamber, the oxygen admission port opened in II chamber passes into oxygen, material is carried out secondary oxidation reaction, when material reaches II chamber over-pass height, material overflows to III chamber, the oxygen admission port opened in III chamber passes into oxygen, material is carried out three oxidizing reactions, when material reaches III chamber over-pass height, material overflows to IV chamber, flash distillation plant 21 is delivered to by discharge port 20, chuck condensing works 75, it is set in described kettle periphery, and chuck condensing works one side lower part is provided with cooling water inlet 76 for passing into water coolant, and opposite side top is provided with cooling water outlet 77 for discharging water coolant, pneumatic outlet 18, it is arranged on kettle top near cooling water outlet, for CO
2with the output of steam, kettle top has been opened multiple upper rinse mouth 78, four cavity bottom and has all been opened lower rinse mouth 79, kettle bottom is provided with cooling groove 80, and be communicated with lower rinse mouth, the material in kettle is cleared up for thoroughly quick when reactor needs parking technological transformation by upper and lower rinse mouth, and the material after cleaning is passed into cooling groove and carry out cooling process and storage, kettle outside is provided with the change for real-time monitored still internal pressure, liquid level and temperature of tensimeter 81, liquidometer 82 and temperature monitor 83, so that adjust, the high order end of kettle offers to be convenient to staff and to come in and go out and overhaul after inspection manhole 84 breaks down for reactor.
In technique scheme, over-pass is provided with between each chamber of horizontal reacting still adopted, rise along baffle plate when continuously feeding participates in reacted material, the residence time is longer, sufficient reacting, when reaching height of baffle plate, next chamber will be overflowed to, this chamber enters oxygen simultaneously, under the effect of stirring, carry out secondary oxidation, when feed liquid reaches the height of baffle plate of this chamber, next chamber can be overflowed to again and continue oxidation, until feed liquid reaches last chamber, by pressure itself in still, feed liquid is discharged, be delivered to feed liquid storage tank.In the process, material is constantly added oxidation, sufficient reacting, and transformation efficiency and transformation efficiency are largely increased.In addition, the agitator that this reactor adopts, its middle and upper part blade is self-priming, bottom blade is open type turbine, upper and lower paddle is divided the work separately, material seethes up and down in still, prevent material from forming dead band, be evenly distributed, oxygen enters in still by inserted filtering element stainless steel gas distributor from inlet mouth, this gas distributor aperture is 1 ~ 5 μm, effectively can prevent feed blocking, ensure good oxygen-enriched environment, along with the rotation of stirring blade fully contacts with material, make it abundant reaction, reach desirable oxidation effectiveness.
In another kind of embodiment, as shown in Figure 1, described apparatus of oxygen supply 12 comprises oxygen air separation facility 13, oxygen compressor 14 and oxygen surge tank 15, oxygen compressor 14 is communicated with 15 with described oxygen air separation facility 13 with oxygen surge tank respectively, described oxygen surge tank 15 passes through pipeline communication with described liquid phase oxidation reaction device 17, fully the oxygen in air can be carried out compression by this apparatus of oxygen supply 12 to utilize, achieving showing of oxygen does existing use, takes full advantage of air resource.
In another kind of embodiment, as shown in Figure 1, described first concentrating unit 30 is provided with the first concentrating unit steam drain 31, described second concentrating unit 46 is provided with the second concentrating unit steam drain 47, the effect of the first concentrating unit venting port 31 and the second concentrating unit venting port 47 is effectively discharged by the steam after the concentrated utilization in the first concentrating unit 30 second concentrating unit 46, ensure that the normal operation of equipment, achieve the object that feed liquid is concentrated.
In another kind of embodiment, described first tripping device 26 and the second tripping device 39 are vertical automatic plate frame press filter, this equipment has the advantages that filtration area is large, filtration production capacity is high, input and output material is unimpeded, level of automation is high, filtration cakes torrefaction degree is high, and can extend the work-ing life of filter cloth.
In another kind of embodiment, described primary heater unit 8 is provided with the thermometer for detecting temperature in primary heater unit 8, thermometer can detect the temperature of preheating, preheating temperature can be regulated to the temperature of reaction by the display of thermometer in warm.
In another kind of embodiment, described flash distillation plant 21 is level Four flash tank, and level Four flash tank has that material heated time is short, velocity of evaporation is fast, and concentration ratio is great, effectively keeps the former effect of material, feature that anti-scaling property is good.
In another kind of embodiment, the feed liquid transport pipe between described liquid phase oxidation reaction device 17 and flash distillation plant 21 connects the second transferpump 57; Feed liquid transport pipe between described flash distillation plant 21 and the first tripping device 26 connects the 3rd transferpump 58; Feed liquid transport pipe between described first concentrating unit 30 and carbonizing plant 35 connects the 4th transferpump 59; Feed liquid transport pipe between described carbonizing plant 35 and the second tripping device 39 connects the 5th transferpump 60; Feed liquid transport pipe between described electrolyzer 43 and the second concentrating unit 46 connects the 6th transferpump 16; Described second concentrating unit 46 is connected the 7th transferpump 62 with on the feed liquid transport pipe between equipment of crystallisation by cooling 51; Described equipment of crystallisation by cooling 51 is connected the 8th transferpump 63 with on the feed liquid transport pipe between centrifugal device 54, these transferpumps are metering diaphragm pump, feed liquid effectively can be delivered to corresponding equipment by this metering diaphragm pump, and corresponding transfer rate can be set, improve the production production capacity of sodium dichromate.
In another kind of embodiment, be the soda ash of 99% containing simple substance Cr by the ferrochrome, the content that are 68%, content be 89% from the second tripping device 39 obtain containing chromium sodium bicarbonate, be mixed with mixed slurry from joining in making beating tank 5 in mass fraction 1:0.65:1.13:2.89 ratio containing chromium wash water of the rich siderochrome slag of washing;
With the first transferpump 7, mixed slurry is pressed 2.0m
3/ h squeezes into primary heater unit 8 continuously, is preheated to 180 DEG C of input liquid phase oxidation reaction devices 17 (oxidation stripping tank) continuously, the CO that pre-thermolysis produces
2gas inputs carburizing reagent device 35 for carburizing reagent after dewatering, compressing;
Control liquid phase oxidation reaction device 17 (oxidation stripping tank) interior reaction material liquid temp 250 DEG C, apparatus of oxygen supply 12 evenly passes into oxygen and maintains stagnation pressure 4.5MPa in liquid phase oxidation reaction device 17 (oxidation stripping tank), in exhaust, steam inputs the first concentrating unit 30 and the second concentrating unit 46 and concentrates for rear end feed liquid, and carbon dioxide inputs carburizing reagent device 35 for for carburizing reagent after dewatering, compressing;
Control liquid phase oxidation reaction device 17 (oxidation stripping tank) discharging flow 2.0m
3/ h continuous discharge, reaction feed liquid is lowered the temperature step by step by flash distillation plant (level Four flash tank), step-down, enters cooling transfer tank after final stage flash tank out-feed liquid temperature is down to 110 DEG C;
With pump, feed liquid in cooling groove is squeezed into the first tripping device 26 (vertical board and frame machine), filter to isolate rich siderochrome slag from rich siderochrome slag outlet 27, obtain Na
2crO
4content is the chromium acid sodium solution of 426.8g/L, and in ferrochrome, Cr transformation efficiency is 92.3%, and the wash water washing rich siderochrome slag can be used for front end making beating tank 5 and prepares burden;
The chromium acid sodium solution obtained is squeezed into carbonizing plant with the 4th transferpump and is carried out carbonization after the first concentrating unit 30 is concentrated, first concentrating unit steam used all comes from the steam of front end liquid phase oxidation reaction device 17 oxidizing reaction generation and the secondary steam of flash distillation plant 21 generation, CO used in carbonizing plant 35
2all from the CO that the pre-thermolysis of front end primary heater unit 8 and liquid-phase oxidation device 17 (oxidation stripping tank) oxidizing reaction produce
2feed liquid after carbonization is filtered by the first tripping device 39 (vertical board and frame machine) and is obtained the carbodiimide solution that acidification rate is 90.2%, isolated containing sodium bicarbonate outlet 41 discharge of chromium sodium bicarbonate from the second tripping device 39, and by pipeline, the sodium bicarbonate entrance 1 being delivered to making beating tank 5 containing chromium sodium bicarbonate is used as raw material;
Carbodiimide solution input electrolyzer carries out acidifying, acidification rate brings up to 100.5%, acidizing fluid is through concentrated, equipment of crystallisation by cooling 51 crystallisation by cooling of the second concentrating unit 46, and the crystal solution obtained is deviate from mother liquor by centrifugal device 54 and obtained sodium dichromate, detects Na in this obtained sodium dichromate product through sampling
2cr
2o
7h
2o content 99.61%, SO
4 2 -content 0.17%, Cl
-content is 0.06%.
In another kind of embodiment, be the soda ash of 99% containing simple substance Cr by the ferrochrome, the content that are 68%, content be 89% from the second tripping device 39 obtain containing chromium sodium bicarbonate, be mixed with mixed slurry from joining in making beating tank 5 in mass fraction 1:0.76:0.98:2.75 ratio containing chromium wash water of the rich siderochrome slag of washing;
With the first transferpump 7, mixed slurry is pressed 3.5m
3/ h squeezes into primary heater unit 8 continuously, is preheated to 170 DEG C of inputs liquid phase oxidation reaction device 17 (horizontal reacting still) continuously, the CO that pre-thermolysis produces
2gas inputs carburizing reagent device 35 for carburizing reagent after dewatering, compressing;
Control liquid phase oxidation reaction device 17 (horizontal reacting still) interior reaction material liquid temp 280 DEG C, apparatus of oxygen supply 12 evenly passes into oxygen and maintains stagnation pressure 6.5MPa in liquid phase oxidation reaction device 17 (horizontal reacting still), in exhaust, steam inputs the first concentrating unit 30 and the second concentrating unit 46 and concentrates for rear end feed liquid, and carbon dioxide inputs carburizing reagent device 35 for for carburizing reagent after dewatering, compressing;
Control liquid phase oxidation reaction device 17 (horizontal reacting still) discharging flow 3.5m
3/ h continuous discharge, reaction feed liquid is lowered the temperature step by step by flash distillation plant (level Four flash tank), step-down, enters cooling transfer tank after final stage flash tank out-feed liquid temperature is down to 120 DEG C;
With pump, feed liquid in cooling groove is squeezed into the first tripping device 26 (vertical board and frame machine), filter to isolate rich siderochrome slag from rich siderochrome slag outlet 27, obtain Na
2crO
4content is the chromium acid sodium solution of 473.7g/L, and in ferrochrome, Cr transformation efficiency is 93.3%, and the wash water washing rich siderochrome slag can be used for front end making beating tank 5 and prepares burden;
The chromium acid sodium solution obtained is squeezed into carbonizing plant with the 4th transferpump and is carried out carbonization after the first concentrating unit 30 is concentrated, first concentrating unit steam used all comes from the steam of front end liquid phase oxidation reaction device 17 (horizontal reacting still) oxidizing reaction generation and the secondary steam of flash distillation plant 21 generation, CO used in carbonizing plant 35
2all from the CO that the pre-thermolysis of front end primary heater unit 8 and liquid-phase oxidation device 17 oxidizing reaction produce
2feed liquid after carbonization is filtered by the first tripping device 39 (vertical board and frame machine) and is obtained the carbodiimide solution that acidification rate is 94.6%, isolated containing sodium bicarbonate outlet 41 discharge of chromium sodium bicarbonate from the second tripping device 39, and by pipeline, the sodium bicarbonate entrance 1 being delivered to making beating tank 5 containing chromium sodium bicarbonate is used as raw material;
Carbodiimide solution input electrolyzer carries out acidifying, acidification rate brings up to 100.5%, acidizing fluid is through concentrated, equipment of crystallisation by cooling 51 crystallisation by cooling of the second concentrating unit 46, and the crystal solution obtained is deviate from mother liquor by centrifugal device 54 and obtained sodium dichromate, detects Na in this obtained sodium dichromate product through sampling
2cr
2o
7h
2o content 99.64%, SO
4 2-content 0.16%, Cl
-content is 0.06%.
In another kind of embodiment, be the soda ash of 99% containing simple substance Cr by the ferrochrome, the content that are 68%, content be 89% from the second tripping device 39 obtain containing chromium sodium bicarbonate, be mixed with mixed slurry from joining in making beating tank 5 in mass fraction 1:0.48:1.42:3.07 ratio containing chromium wash water of the rich siderochrome slag of washing;
With the first transferpump 7, mixed slurry is pressed 5m
3/ h squeezes into primary heater unit 8 continuously, is preheated to 150 DEG C of inputs liquid phase oxidation reaction device 17 (oxidizing reactor group) continuously, the CO that pre-thermolysis produces
2gas inputs carburizing reagent device 35 for carburizing reagent after dewatering, compressing;
Control liquid phase oxidation reaction device 17 (horizontal reacting still) interior reaction material liquid temp 260 DEG C, apparatus of oxygen supply 12 evenly passes into oxygen and maintains stagnation pressure 5.5MPa in liquid phase oxidation reaction device 17 (oxidizing reactor group), in exhaust, steam inputs the first concentrating unit 30 and the second concentrating unit 46 and concentrates for rear end feed liquid, and carbon dioxide inputs carburizing reagent device 35 for for carburizing reagent after dewatering, compressing;
Control liquid phase oxidation reaction device 17 (oxidizing reactor group) discharging flow 5m
3/ h continuous discharge, reaction feed liquid is lowered the temperature step by step by flash distillation plant (level Four flash tank), step-down, enters cooling transfer tank after final stage flash tank out-feed liquid temperature is down to 100 DEG C;
With pump, feed liquid in cooling groove is squeezed into the first tripping device 26 (vertical board and frame machine), filter to isolate rich siderochrome slag from rich siderochrome slag outlet 27, obtain Na
2crO
4content is the chromium acid sodium solution of 451.9g/L, and in ferrochrome, Cr transformation efficiency is 91.3%, and the wash water washing rich siderochrome slag can be used for front end making beating tank 5 and prepares burden;
The chromium acid sodium solution obtained is squeezed into carbonizing plant with the 4th transferpump and is carried out carbonization after the first concentrating unit 30 is concentrated, first concentrating unit steam used all comes from the steam of front end liquid phase oxidation reaction device 17 (oxidizing reactor group) oxidizing reaction generation and the secondary steam of flash distillation plant 21 generation, CO used in carbonizing plant 35
2all from the CO that the pre-thermolysis of front end primary heater unit 8 and liquid-phase oxidation device 17 (oxidizing reactor group) oxidizing reaction produce
2feed liquid after carbonization is filtered by the first tripping device 39 (vertical board and frame machine) and is obtained the carbodiimide solution that acidification rate is 91.8%, isolated containing sodium bicarbonate outlet 41 discharge of chromium sodium bicarbonate from the second tripping device 39, and by pipeline, the sodium bicarbonate entrance 1 being delivered to making beating tank 5 containing chromium sodium bicarbonate is used as raw material;
Carbodiimide solution input electrolyzer carries out acidifying, acidification rate brings up to 100.5%, acidizing fluid is through concentrated, equipment of crystallisation by cooling 51 crystallisation by cooling of the second concentrating unit 46, and the crystal solution obtained is deviate from mother liquor by centrifugal device 54 and obtained sodium dichromate, detects Na in this obtained sodium dichromate product through sampling
2cr
2o
7h
2o content 99.71%, SO
4 2-content 0.15%, Cl
-content is 0.05%.
Here the number of devices illustrated and treatment scale are used to simplify explanation of the present invention.The systematic difference of high-efficiency self-circulation wet method continuous production sodium dichromate of the present invention, modifications and variations be will be readily apparent to persons skilled in the art.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (8)
1. a system for high-efficiency self-circulation wet method continuous production sodium dichromate, is characterized in that, comprising:
Making beating tank, is provided with the feeding mouth of input oxide spinel hydrogen sodium, ferrochrome powder, sodium carbonate and water;
Making beating tank connects the first transferpump, primary heater unit, liquid phase oxidation reaction device, flash distillation plant, the first tripping device, the first concentrating unit, carbonizing plant, the second tripping device, electrolyzer, the second concentrating unit, equipment of crystallisation by cooling and centrifugal device successively by feed liquid transport pipe;
Apparatus of oxygen supply, it is connected by pipeline with described liquid phase oxidation reaction device; For passing into oxygen to described liquid phase oxidation reaction device;
Wherein, the CO that in described primary heater unit, pre-thermolysis produces
2, be oxidized the CO of generation in liquid phase oxidation reaction device
2be delivered to the first concentrating unit and the second concentrating unit with the steam produced in steam and flash distillation plant by gas transmission pipeline, steam is used for feed liquid and concentrates; CO
2gas respectively from the blowing mouth of the first concentrating unit and the second concentrating unit export and dewatered by freeze drier, CO
2described carbonizing plant is inputted for carburizing reagent after compressor compresses; What in described second tripping device, separation obtained is used as to prepare burden by the feeding mouth of Cemented filling to making beating tank containing chromium sodium bicarbonate.
2. the system of high-efficiency self-circulation wet method continuous production sodium dichromate as claimed in claim 1, it is characterized in that, the feeding mouth of described making beating tank has four, is respectively sodium bicarbonate entrance, ferrochrome powder entrance, sodium carbonate entrance and water inlet.
3. the system of high-efficiency self-circulation wet method continuous production sodium dichromate as claimed in claim 1, it is characterized in that, described apparatus of oxygen supply comprises oxygen air separation facility, oxygen compressor and oxygen surge tank, oxygen compressor is communicated with oxygen surge tank with described oxygen air separation facility respectively, and described oxygen surge tank and described liquid phase oxidation reaction device pass through pipeline communication.
4. the system of high-efficiency self-circulation wet method continuous production sodium dichromate as claimed in claim 1, is characterized in that, described first concentrating unit is provided with the first concentrating unit steam drain, described second concentrating unit is provided with the second concentrating unit steam drain.
5. the system of high-efficiency self-circulation wet method continuous production sodium dichromate as claimed in claim 1, it is characterized in that, described first tripping device and the second tripping device are vertical automatic plate frame press filter.
6. the system of high-efficiency self-circulation wet method continuous production sodium dichromate as claimed in claim 1, is characterized in that, described primary heater unit being provided with the thermometer for detecting temperature in primary heater unit.
7. the system of high-efficiency self-circulation wet method continuous production sodium dichromate as claimed in claim 1, it is characterized in that, described flash distillation plant is level Four flash tank.
8. the system of high-efficiency self-circulation wet method continuous production sodium dichromate as claimed in claim 1, is characterized in that, the feed liquid transport pipe between described liquid phase oxidation reaction device and flash distillation plant connects the second transferpump; Feed liquid transport pipe between described flash distillation plant and the first tripping device connects the 3rd transferpump; Feed liquid transport pipe between described first concentrating unit and carbonizing plant connects the 4th transferpump; Feed liquid transport pipe between described carbonizing plant and the second tripping device connects the 5th transferpump; Feed liquid transport pipe between described electrolyzer and the second concentrating unit connects the 6th transferpump; Described second concentrating unit is connected the 7th transferpump with on the feed liquid transport pipe between equipment of crystallisation by cooling; Described equipment of crystallisation by cooling is connected the 8th transferpump with on the feed liquid transport pipe between centrifugal device.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108101109A (en) * | 2017-12-22 | 2018-06-01 | 四川省银河化学股份有限公司 | A kind of sodium, carbon, the system of recycle heat system production chromic salts series of products |
| CN110482605A (en) * | 2019-08-29 | 2019-11-22 | 昆明理工大学 | A kind of method and device preparing sodium dichromate using chromite as one step of raw material |
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| CN103193271A (en) * | 2013-04-02 | 2013-07-10 | 四川省银河化学股份有限公司 | Method for producing high-quality sodium bichromate |
| CN103446776A (en) * | 2013-07-24 | 2013-12-18 | 深圳市捷晶能源科技有限公司 | Sodium bichromate concentration and crystallization equipment and technology |
| CN205023875U (en) * | 2015-09-15 | 2016-02-10 | 四川省银河化学股份有限公司 | System for sodium dichromate is prepared in succession to high -efficient self -loopa wet process |
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| JPS56139103A (en) * | 1980-03-31 | 1981-10-30 | Yoshio Aoyama | Crystallization of purified crystal |
| CN103193271A (en) * | 2013-04-02 | 2013-07-10 | 四川省银河化学股份有限公司 | Method for producing high-quality sodium bichromate |
| CN103446776A (en) * | 2013-07-24 | 2013-12-18 | 深圳市捷晶能源科技有限公司 | Sodium bichromate concentration and crystallization equipment and technology |
| CN205023875U (en) * | 2015-09-15 | 2016-02-10 | 四川省银河化学股份有限公司 | System for sodium dichromate is prepared in succession to high -efficient self -loopa wet process |
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| CN108101109A (en) * | 2017-12-22 | 2018-06-01 | 四川省银河化学股份有限公司 | A kind of sodium, carbon, the system of recycle heat system production chromic salts series of products |
| CN110482605A (en) * | 2019-08-29 | 2019-11-22 | 昆明理工大学 | A kind of method and device preparing sodium dichromate using chromite as one step of raw material |
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| CN105129852B (en) | 2017-07-11 |
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Denomination of invention: A system for continuous preparation of sodium jarosite by high efficiency self circulation wet method Effective date of registration: 20220413 Granted publication date: 20170711 Pledgee: China Construction Bank Corporation Mianyang Branch Pledgor: SICHUAN YINHE CHEMICAL Co.,Ltd. Registration number: Y2022980004215 |
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