CN103274550B - Brine impurity removal method in sodium chlorate production technology - Google Patents
Brine impurity removal method in sodium chlorate production technology Download PDFInfo
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Abstract
The invention discloses a brine impurity removal method in a sodium chlorate production technology. When crude brine is taken as the raw material for producing sodium chlorate, the brine impurity removal method comprises three processes including chemical impurity removal, ion exchange and micro-filtration; and when brine or seawater is taken as the raw material for producing sodium chlorate, the brine impurity removal method comprises five processes including micro-filtration, reverse osmosis concentration, chemical impurity removal, ion exchange and micro-filtration. The content of total calcium and magnesium ion is reduced to lower than 0.5 mg/L in the brine processed by the brine impurity removal method, so that corrosion of an electrolysis bath anode can be relieved, the production power consumption can be reduced, the tank washing period can be prolonged, and the production efficiency can be improved.
Description
Technical field
The present invention relates to a kind of impurity-removing method, specifically the salt solution impurity-removing method in a kind of production of sodium chlorate technique.
Background technology
Production of sodium chlorate technological process comprises brine treatment operation, electrowinning process, crystallizing and drying operation etc. substantially.The quality of salt solution directly affects power consumption and washing trough cycle, and the existence of impurity also can be corroded anode, so brine treatment operation plays a part very important in whole production technique.
Abroad production of sodium chlorate producer all focuses on the purifying treatment of salt solution very much.North America, European countries' production of sodium chlorate sodium-chlor used are refining sodium-chlor, and its calcium-magnesium content is extremely low, and foreign matter content is few, therefore salt refining operation production line is short, bed drain purge is few.This refining sodium chloride brine treatment process only needs can be reduced to 0.5mg/L by impurity massfraction in salt solution after ion exchange treatment.
Domestic sodium chlorate raw material adopts crude salt, bittern, seawater, and raw material impurity is more, the refining line length of producing.Because feed purification is simply equipped, generally only adopt chemical subtraction operation, content of calcium and magnesium high (5-10mg/L) in refined brine, so cause bath voltage to rise soon, the washing trough cycle is short, generally at three months, washes once.Washing trough has not only been shortened the production time continually, and has improved production cost.
Summary of the invention
Technical problem to be solved by this invention is to provide the salt solution impurity-removing method in a kind of production of sodium chlorate technique; making to enter the mesohalobic calcium magnesium of electrolyzer total content greatly reduces; not only be conducive to protect anode, also can reduce power consumption, extend the washing trough cycle, enhance productivity.
The present invention solves the problems of the technologies described above with following technical scheme:
Salt solution impurity-removing method in production of sodium chlorate technique of the present invention, it comprises following operation steps:
1) by raw material, be to send in refinery pit after solid crude salt, bittern or brine disposal become saturated or approach saturated sodium chloride solution, add enough sodium carbonate and sodium hydroxide in sodium chloride solution, make pH to 9-12, the mol ratio of sodium carbonate and sodium hydroxide is 1:1;
2) after question response produces and precipitates completely, sodium chloride solution, by strainer, is isolated the metal salt precipitate filter residue of generation, adds hydrochloric acid soln regulation system pH value 8-9, then be sent to cationic exchange coloum removal of impurities in filtrate;
3) through step 2) the sodium-chlor mother liquor processed is by micro-strainer, removes solid filter residue, obtains Ca
2+and Mg
2+total ion concentration be less than the refined brine of 0.5mg/L, after send to liquid blending device.
In step 1), when raw material is solid crude salt, crude salt solid and bariumchloride solid are added to water-solubleization, make to reach capacity or approach saturated, and measure the content of sulfate anion in brine system ion, in the bariumchloride mole number adding and crude brine, the mole number ratio of sulfate ion is 1:1.
In step 1), when raw material is bittern or seawater, add barium chloride solution with sulfate precipitate radical ion, in bariumchloride mole number and bittern or seawater, the mole number ratio of sulfate ion is 1:1; Sodium chloride solution is delivered in micro-strainer, bittern or seawater after micro-filtration concentrate by reverse osmosis membrane apparatus again.
The reverse osmosis membrane operational conditions of reverse osmosis membrane apparatus is: 0～40 ℃ of voltage of supply 380V ± 30V, operating ambient temperature; 20～45 ℃ of working temperatures; 10～20 ℃ of temperature of cooling water; With water conductivity 5～15 μ s/cm; Turbidity 0.5～1.0NTU; Operating pressure 1.0～2.0MPa; 20～45 ℃ of cleaning temperatures; Cleaning pressure 0.2～0.4MPa; Clean-out system pH value 2～11.
In step 1), the temperature of refinery pit is controlled at 30-100 ℃.
In step 1), the temperature of refinery pit is preferably controlled at 35-45 ℃.
In step 2) in, described cationic exchange coloum adopts positively charged ion chelate exchange resin post, and ion-exchange column temperature is controlled at 5-35 ℃.
In step 3), the micro-strainer that the micropore size of described micro-strainer is 50nm-100nm.
In step 2) in, sodium chloride solution is 2L/min～2.5L/min through the speed of cationic exchange coloum.
In step 3), sodium chloride solution is 3L/min～3.5L/min by the speed of micro-strainer.
The present invention be take crude salt during as production sodium chlorate raw material, and this salt solution impurity-removing method comprises chemical subtraction, ion-exchange, three processes of micro-filtration; Take bittern or seawater during as production sodium chlorate raw material, and this salt solution impurity-removing method comprises micro-filtration, reverse osmosis concentration, chemical subtraction, ion-exchange, five processes of micro-filtration.The object of the invention is to make in refining salt solution the cation impurity levels such as calcium magnesium to be reduced to and be less than 0.5mg/L; this can not only protect the anode of electrolyzer effectively, and slowing down corrosion also can reduce the power consumption of production; extend the cleaning interval of electrolyzer, enhance productivity.
The inventive method is particularly useful for the domestic production of sodium chlorate technique that solid crude salt, bittern, seawater be raw material of take.
Specific implementation method
Below the invention will be further described.
The salt solution removal of impurities treatment process process that the solid crude salt of take is raw material as:
In salt dissolving tank, crude salt solid and bariumchloride solid are added to suitable quantity of water and dissolve, make to reach capacity or approach saturated (sodium chloride concentration is 300g/L～370g/L).The content of measuring sulfate anion in brine system ion, in the bariumchloride mole number adding and crude brine, the mole number ratio of sulfate ion is 1:1.Crude brine is overflowed and is entered in treatment tank by salt dissolving tank top, at this, adds enough solid sodium carbonates and solid sodium hydroxide in sodium chloride solution, makes pH reach 9-12.The mol ratio of sodium carbonate and sodium hydroxide is 1:1.Sodium carbonate and sodium hydroxide are preferably chemically pure reagent.
In treatment tank, is furnished with whipping appts, to accelerate the generation of the precipitations such as calcium carbonate, calcium sulfate and magnesium hydroxide.Along with the rising of temperature, the solubleness of calcium-magnesium ratio compound can increase, and can make more impurity be dissolved in salt solution simultaneously.The content of the temperature for the treatment of tank calcium magnesium precipitate thing in 30-100 ℃ can not affect salt solution, relatively high temperature can also improve the speed of reaction on the contrary, shortens and produces the required time of precipitation.From the angle of energy consumption, consider, the temperature for the treatment of tank preferably remains on 35-45 ℃ and is advisable.After precipitation to be generated is complete, salt solution, by strainer, is isolated the metal salt precipitate filter residue of generation, and filtrate is sent to cationic exchange coloum removal of impurities.Filter method is applicable to all known filter methods of the present invention and all can uses, as filter press, belt press filtration, vacuum filtration etc.In sodium-chlor filtrate, add hydrochloric acid soln regulation system pH value between 8-9, filtrate is passed through positively charged ion chelate exchange resin post with the speed of 2L/min～2.5L/min, further removes alkaline earth metal impurity.Ion-exchange column temperature is controlled at 5-35 ℃, and temperature is higher than 35 ℃ of oxidizable inefficacies of resin, and temperature can reduce lower than 5 ℃ of velocity of ion exchanges.And pH value is not strict with, the pH value of pillar work is the pH value of the sodium chloride solution that needs purification, about 8-9 conventionally.What the present invention used is positively charged ion chelating ion exchange resin, and other Zeo-karb is not suitable for using, because na concn is too high in solution.
The sodium-chlor mother liquor of crossing through ion exchange resin treatment, then the micro-strainer that the speed of 3L/min～3.5L/min of take is 50nm～100nm by micropore size, remove the filter residues such as some small solid impurities (as calcium sulfate and magnesium hydroxide solid) and toner, finally obtain Ca
2+and Mg
2+total ion concentration be less than the refined brine of 0.5mg/L, after send to liquid blending device.In liquid blending device, add sodium dichromate 99 and hydrochloric acid, regulate salt solution pH value to 7.Salt solution is sent into electrowinning process along pipeline.The effect of sodium dichromate 99 is generation and the protection negative electrode of side reaction while suppressing electrolysis, and in refined brine, adding sodium dichromate 99 concentration is 3g/L.
When the flow velocity of salt solution by microfiltration membrane reduces 30%-40%, need clean microfiltration membrane.Cleaning should adopt chemical pure or analytical pure with pharmaceutical chemicals, in case cause secondary pollution.
When ion exchange resin lifting capacity is less than 60-80%, need to above-mentioned Zeo-karb, regenerate with hydrochloric acid, metal ion is exchanged from Zeo-karb.The method of Zeo-karb regeneration is: with hydrochloric acid cleaning, adsorbed the Zeo-karb of alkaline-earth metal ions, and be swapped out metal ion; Water or sodium hydroxide or sodium chloride solution or their mixture, remove the hydrochloric acid in resin cation (R.C.) again.
Micro-filtration belongs to pressure-driven type membrane separation technique, and the diameter of separated portion is 0.01～10 μ m.The present invention can apply inorganic ceramic composite membrane filtered brine, can effectively remove micron particle, submicron particles and sub-submicron particles material (various solid impurity) in salt solution, reduce the particle contamination in electrolyzer, and Filter Tree cosmetics and prevent that microbial contamination from entering electrolytic system effectively.And inorganic ceramic film can use steam to equipment disinfection, available high pressure fluid counterflush regeneration, film cleans easy, and regenerability is excellent, therefore should use convenience very.
If production sodium chlorate process using bittern or seawater are raw material, before removal of impurities, also need to carry out reverse osmosis concentration operation, make in stock liquid sodium chloride content reach capacity or approach that saturated (sodium chloride concentration is 300g/L～370g/L.Reverse osmosis membrane separation technology is widely used in sea water desaltination at present, food, brewing industry, cosmetics production, the aspects such as pharmaceutical technology.Compare with traditional hot method of enrichment, reverse osmosis method concentrates following advantage: lower energy consumption; Lower facility investment and floor space; Good quality stability; Non-environmental-pollution etc.
Take removal of impurities treatment process that bittern or seawater be raw material production sodium chlorate compared with crude brine treatment process, and something in common is all to need through chemical subtraction operation, ion-exchange removal of impurities operation and micro-filtration operation, and working method is same as above.Difference is, bittern or seawater are generally the unsaturated solution of sodium-chlor, so can omit the step that solid salt is dissolved, but need to increase a reverse osmosis membrane enrichment process before chemical subtraction operation in whole brine treatment technique, make sodium chloride content in salt solution reach or approach saturated.
Concrete operations flow process is as follows:
In salt solution reservoir, store bittern or seawater, be sodium-chlor unsaturated solution, add barium chloride solution with sulfate precipitate radical ion, in bariumchloride mole number and bittern or seawater, the mole number ratio of sulfate ion is 1:1.Sodium chloride solution is delivered in micro-strainer, must pass through micro-strainer, otherwise can stop up very soon the runner in membrane element before entering reverse osmosis system, to such an extent as to reverse osmosis membrane concentrates work, cannot carry out, and some meetings cause the flux degradation of film, the lost of life.
Bittern or seawater after micro-filtration concentrate by reverse osmosis membrane apparatus.Reverse osmosis membrane operation working conditions: voltage of supply: 380V ± 30V; Operating ambient temperature: 0～40 ℃; Working temperature: 20～45 ℃; Temperature of cooling water: 10～20 ℃; Water (comprising the waters such as feed liquid, film cleaning) specific conductivity: 5～15 μ s/cm; Turbidity: 0.5～1.0NTU; Operating pressure: 1.0～2.0MPa; Cleaning temperature: 20～45 ℃; Cleaning pressure: 0.2～0.4MPa; Clean-out system pH value: 2～11.When after concentrating by reverse osmosis membrane, in salt solution, sodium chloride content reaches capacity or approaches saturated (sodium chloride concentration is 300g/L～370g/L), salt solution is sent to other removal of impurities operation along pipeline.When reverse osmosis membrane flux reduces 30%-40%, in time reverse osmosis membrane is cleaned.
Salt solution after concentrated is delivered in refinery pit, at this, adds enough sodium carbonate and sodium hydroxide in sodium chloride solution, regulates pH value to 9-12, and the mol ratio of sodium carbonate and sodium hydroxide is 1:1.After precipitation to be generated is complete, by strainer, isolate the metal salt precipitate filter residue of generation, filtrate is sent to cationic exchange coloum removal of impurities.The sodium-chlor mother liquor of crossing through ion exchange resin treatment, by micro-strainer, is removed solid filter residue 10, makes Ca
2+and Mg
2+total ion concentration be less than 0.5mg/L, after send to liquid blending device 8, at this, add sodium dichromate 99 and hydrochloric acid, regulate salt solution pH value to 7, last salt solution is sent into electrowinning process along pipeline.In bittern or seawater, adding sodium dichromate 99 concentration is 3g/L.
Embodiment 1
In salt dissolving tank, 36kg crude salt solid and 42g solid bariumchloride are added to water-solubleization of 100L at 35 ℃, be made into the sodium chloride solution that concentration is 360g/L.Sodium chloride solution is delivered in refinery pit by pipeline, at this, adds 0.06kg sodium carbonate and sodium hydroxide (mol ratio is 1:1) in sodium chloride solution, to make pH to 9.After precipitation to be generated is complete, filter to isolate the metal salt precipitate of generation.In sodium-chlor filtrate, adding hydrochloric acid soln regulation system pH value is 8, and then filtrate take the positively charged ion chelate exchange resin post that the speed of 2L/min is 35 ℃ by column temperature, further removes alkaline earth metal impurity.
The sodium chloride solution of crossing through ion exchange resin treatment, the microfiltration membrane that the 3L/min of then take is 50nm by micropore size, removes some small solid impurities (as calcium sulfate and magnesium hydroxide solid) and toner, finally obtains Ca
2+and Mg
2+the total ion concentration refined brine that is 0.2mg/L, after by pipeline, send to tune liquid.In liquid blending device, add 0.3kg sodium dichromate 99, adding hydrochloric acid to regulate salt solution pH value is 7, and salt solution is sent into electrowinning process along pipeline.
This technique is effectively removed the calcium ions and magnesium ions in salt solution, its total content is lower than 0.5mg/L, make the power consumption of producing sodium chlorate per ton save approximately 100 yuan, the cleaning interval of electrolyzer cleaned once to extend to by original three months and cleans once half a year, had not only reduced production cost but also improved production efficiency.
Embodiment 2
At salt solution reservoir, in the bittern that is 100g/L to 100L sodium chloride-containing concentration, add 12g/L barium chloride solution 1L, after question response is complete, the micro-strainer that is 100nm by micropore size by bittern, to remove macrobead solid impurity, after be sent to reverse osmosis membrane apparatus and concentrate.Working temperature: 20 ℃; Temperature of cooling water: 20 ℃; Operating pressure: 1MPa.When after concentrating by reverse osmosis membrane, in salt solution, sodium chloride content reaches 350g/L, salt solution is sent to other removal of impurities operation along pipeline.When reverse osmosis membrane flux reduces 30%～40%, the cleaning of in time reverse osmosis membrane being carried out.
Bittern after concentrated is delivered in refinery pit, at this, adds 0.02kg sodium carbonate and sodium hydroxide (sodium carbonate and sodium hydroxide mol ratio are 1:1), regulates brine ph to 10.After precipitation to be generated is complete, filter to isolate the alkaline earth salt precipitation of generation.Adding hydrochloric acid soln regulation system pH value is 9, and the positively charged ion chelate exchange resin post that the speed of 2.5L/min of take after mother liquor is 15 ℃ by column temperature, further removes alkaline earth metal impurity.
The sodium-chlor mother liquor of crossing through ion exchange resin treatment, the microfiltration membrane that the 3.5L/min of then take is 50nm by micropore size, removes some small solid impurities (as calcium sulfate and magnesium hydroxide solid) and toner, finally obtains Ca
2+and Mg
2+the total ion concentration refined brine that is 0.3mg/L, after by pipeline, deliver in liquid blending device and add 0.3kg sodium dichromate 99, adding hydrochloric acid to regulate brine ph is 7, salt solution is sent into electrowinning process along pipeline.
This technique is effectively removed the calcium ions and magnesium ions in salt solution, its total content is lower than 0.5mg/L, make the power consumption of producing sodium chlorate per ton save approximately 100 yuan, the cleaning interval of electrolyzer cleaned once to extend to by original three months and cleans once half a year, had not only reduced production cost but also improved production efficiency.
Embodiment 3
At salt solution reservoir, in the seawater that is 150g/L to 100L sodium chloride-containing concentration, add 18g/L barium chloride solution 1L, after question response is complete, the micro-strainer that is 100nm by micropore size by seawater, to remove macrobead solid impurity, after be sent to reverse osmosis membrane apparatus and concentrate.Working temperature: 40 ℃; Temperature of cooling water: 10 ℃; Operating pressure: 2MPa.When after concentrating by reverse osmosis membrane, in salt solution, sodium chloride content reaches 340g/L, salt solution is sent to other removal of impurities operation along pipeline.
Seawater after concentrated is delivered in refinery pit, at this, adds 0.03kg sodium carbonate and sodium hydroxide (sodium carbonate and sodium hydroxide mol ratio are 1:1), regulator solution pH value to 12.After precipitation to be generated is complete, filter to isolate the alkaline earth salt precipitation of generation.Adding hydrochloric acid soln regulation system pH value is 9, and the positively charged ion chelate exchange resin post that the speed of 2.5L/min of take after mother liquor is 5 ℃ by column temperature, further removes alkaline earth metal impurity.
The sodium-chlor mother liquor of crossing through ion exchange resin treatment, the microfiltration membrane that the 3.5L/min of then take is 50nm by micropore size, removes some small solid impurities (as calcium sulfate and magnesium hydroxide solid) and toner, finally obtains Ca
2+and Mg
2+the total ion concentration refined brine that is 0.4mg/L, after by pipeline, deliver in liquid blending device and add 0.3kg sodium dichromate 99, adding hydrochloric acid to regulate seawater pH value is 7, salt solution is sent into electrowinning process along pipeline.
This technique is effectively removed the calcium ions and magnesium ions in salt solution, its total content is lower than 0.5mg/L, make the power consumption of producing sodium chlorate per ton save approximately 100 yuan, the cleaning interval of electrolyzer cleaned once to extend to by original three months and cleans once half a year, had not only reduced production cost but also improved production efficiency.
Claims (8)
1. the salt solution impurity-removing method in production of sodium chlorate technique, is characterized in that, it comprises following operation steps:
1) add barium chloride solution with sulfate precipitate radical ion in bittern or seawater, in bariumchloride mole number and bittern or seawater, the mole number ratio of sulfate ion is 1:1; Sodium chloride solution is delivered in micro-strainer, bittern or seawater after micro-filtration concentrate by reverse osmosis membrane apparatus again;
2) send in refinery pit after bittern or brine disposal are become to saturated or approach saturated sodium chloride solution, add enough sodium carbonate and sodium hydroxide in sodium chloride solution, make pH to 9-12, the mol ratio of sodium carbonate and sodium hydroxide is 1:1;
3) after question response produces and precipitates completely, sodium chloride solution, by strainer, is isolated the metal salt precipitate filter residue of generation, adds hydrochloric acid soln regulation system pH value 8-9, then be sent to cationic exchange coloum removal of impurities in filtrate;
4) through step 3) the sodium-chlor mother liquor processed is by micro-strainer, removes solid filter residue, obtains Ca
2+and Mg
2+total ion concentration be less than the refined brine of 0.5mg/L, after send to liquid blending device.
2. the salt solution impurity-removing method in production of sodium chlorate technique according to claim 1, is characterized in that described step 1) in, the reverse osmosis membrane operational conditions of reverse osmosis membrane apparatus is: 0～40 ℃ of voltage of supply 380V ± 30V, operating ambient temperature; 20～45 ℃ of working temperatures; 10～20 ℃ of temperature of cooling water; With water conductivity 5～15 μ s/cm; Turbidity 0.5～1.0NTU; Operating pressure 1.0～2.0MPa; 20～45 ℃ of cleaning temperatures; Cleaning pressure 0.2～0.4MPa; Clean-out system pH value 2～11.
3. the salt solution impurity-removing method in production of sodium chlorate technique according to claim 1, is characterized in that, in step 2) in, the temperature of refinery pit is controlled at 30-100 ℃.
4. the salt solution impurity-removing method in production of sodium chlorate technique according to claim 3, is characterized in that, in step 2) in, the temperature of refinery pit is preferably controlled at 35-45 ℃.
5. the salt solution impurity-removing method in production of sodium chlorate technique according to claim 1, is characterized in that, in step 3) in, described cationic exchange coloum adopts positively charged ion chelate exchange resin post, and ion-exchange column temperature is controlled at 5-35 ℃.
6. the salt solution impurity-removing method in production of sodium chlorate technique according to claim 1, is characterized in that, in step 4) in, the micro-strainer that the micropore size of described micro-strainer is 50nm-100nm.
7. the salt solution impurity-removing method in production of sodium chlorate technique according to claim 1, is characterized in that, in step 3) in, sodium chloride solution is 2L/min～2.5L/min through the speed of cationic exchange coloum.
8. the salt solution impurity-removing method in production of sodium chlorate technique according to claim 1, is characterized in that, in step 4) in, sodium chloride solution is 3L/min～3.5L/min by the speed of micro-strainer.
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| CN103754828A (en) * | 2013-12-23 | 2014-04-30 | 内蒙古工业大学 | Sodium dichromate closed circulation clean production method for preparing sodium chlorate |
| CN105293532A (en) * | 2014-07-28 | 2016-02-03 | 李明雄 | Calcium removal process for lithium chloride solution during production |
| CN105925799A (en) * | 2016-05-26 | 2016-09-07 | 四川思达能环保科技有限公司 | Wet metallurgy film concentration process |
| CN106006881A (en) * | 2016-06-21 | 2016-10-12 | 首钢京唐钢铁联合有限责任公司 | Method and device for preparing bactericide |
| CN107348466A (en) * | 2017-06-30 | 2017-11-17 | 益盐堂（应城）健康盐制盐有限公司 | A kind of energy-saving and emission-reduction production method of edible salt |
| CN116119620A (en) * | 2023-03-03 | 2023-05-16 | 湖南恒光科技股份有限公司 | Sodium chlorate mirabilite chromium removal process |
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| CN1147429C (en) * | 2000-12-12 | 2004-04-28 | 戈尔过滤产品（上海）有限公司 | Process for finely preparing salt water by tank type counter-flushing liquid filter made of balked polytetrafluorethylene film |
| CN100460326C (en) * | 2006-03-15 | 2009-02-11 | 南京九思高科技有限公司 | Method of refining salt by membrane filtration |
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| CN101214975B (en) * | 2008-01-21 | 2010-12-29 | 上海西恩化工设备有限公司 | Advanced treatment technique for brine |
| CN102009987B (en) * | 2010-12-02 | 2012-06-27 | 河南神马氯碱化工股份有限公司 | Brine refining process for removing calcium and magnesium by one step |
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