CN104030319B - Brine desulfuration system and method thereof - Google Patents
Brine desulfuration system and method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of brine desulfuration system, including the baffling groove being sequentially connected with by pipeline, first reaction container, coarse filter, first inorganic ceramic film filter group, pretreatment system, tank before film, nanofiltration membrane separation device, second reaction container and the second inorganic ceramic film filter group, nanofiltration membrane separation device is also associated with freezing and crystallizing device, freezing and crystallizing device is connected to dehydration by evaporation drying device, freezing and crystallizing device is also connected with the second reaction container, brine desulfuration system of the present invention, combined by physics and chemical method, not only can prepare highly purified purification salt, the high glass gall at self product place can also be processed, both environmental pollution had been decreased, by waste liquid, useless solid process, and turn waste into wealth, the anhydrous sodium sulfate that sodium sulphate type bittern is prepared and high-quality saline, it is really achieved no pollution discharge.
Description
Technical field
The present invention relates to brine desulfuration field, particularly relate to a kind of brine desulfuration system and method thereof.
Background technology
Containing sodium sulfate impurity in salt, for salt manufacturing, can with sodium chloride eutectoid and affect the purity of salt；For alkaline, sulfate radical can enter in ionic membrane, blocks film, affects service efficiency and the life-span of film.
In salt industry, sodium sulphate type bittern major impurity is that sodium sulfate (being about 15～30g/L) is generally adopted multiple-effect evaporation technique and is prepared thenardite；Carry out salt by multiple-effect evaporation+sal prunella coproduction, nitre separates, by-product Natrii Sulfas while salt manufacturing, and minority adopts freezing method elimination sodium sulfate to prepare liquid salt, and because sodium sulfate concentration is low, freezing energy consumption is high and is eliminated by enterprise gradually.
At chlor-alkali industry, along with popularizing of ionic membrane alkali making technology, liquid salt purity is more and more prominent to the restriction of ionic membrane alkaline, and the enrichment of sulfate anion in brine system is the key factor affecting ionic membrane economic benefit at present.The main cause of bringing into of sulfate radical is that after raw materials for production containing sulfate radicals and electrolysis, saline uses chemical dechlorination to add reducing agent sodium sulfite, produces sulfate radical.Although embrane method denitration and other chemical method denitrations have obvious advantage, and increasing in the application percentage of chlor-alkali industry, the low glass gall of institute's output, not only sulfate radical content is low, and do not bring other chemical impurities into, and operating cost, cost of investment etc. are all relatively low；But the high glass gall of embrane method output is without market using value.Major part chlor-alkali enterprises is made ten liquid glauber salt by freezing and is deposited to reduce and arrange the pollution to environment outside high nitre mother solution.
There is techniques below problem in above-mentioned technique: (1). and the multiple-effect evaporation sal prunella coproduction of salt industry, the method for separating sodium sulfate, the purity of prepared sodium sulfate is relatively low；(2). nanofiltration desulfurization, the high-load sodium sulfate salt of generation about 15% is without good whereabouts, even if adopting freezing to prepare ten liquid glauber salt, but because ten liquid glauber salt are not final products, useless environmental pollution admittedly still has a certain impact.
The sodium sulfate purity being used alone full-boiled process desulfurization prepared is low, about 98%, can only achieve GB II class product requirement；It is used alone cold process and can only prepare ten liquid glauber salt, be not final products, it does not have market value, bring burden to environmental protection；Independent embrane method denitration, the high glass gall of output does not have place to go；And it being used alone chemical method desulfurization, expense is too high, and a large amount of brine sludge has greater environmental impacts.
Summary of the invention
The technical problem to be solved in the present invention is: in order to solve the problems referred to above, and the present invention provides a kind of brine desulfuration system and method thereof.
The technical solution adopted for the present invention to solve the technical problems is: a kind of brine desulfuration system, including tank, nanofiltration membrane separation device, the second reaction container and the second inorganic ceramic film filter group before the baffling groove being sequentially connected with by pipeline, the first reaction container, coarse filter, the first inorganic ceramic film filter group, pretreatment system, film；
Described nanofiltration membrane separation utensil has two outlets, the respectively outlet of light phase and concentrated phase outlet, the mouth that fades out that described second retort is with described nanofiltration membrane separation device is connected, the concentrated phase outlet of described nanofiltration membrane separation device is connected to freezing and crystallizing device, described freezing and crystallizing utensil has crystallization outlet and brine outlet, described crystallization outlet is connected to dehydration by evaporation drying device, and described brine outlet is connected with described second reaction container.
Sometimes the silt content in salt is too high, needs repeat to filter, further, it is additionally provided with the dense slime water after the first inorganic ceramic film filter group can being filtered between described coarse filter and the first inorganic ceramic film filter group and iterates through the circulating tank of the first inorganic ceramic film filter group.
So that the saline finally obtained is more consummate, further, described pretreatment system includes the static mixer, acid-regulating tank, activated carbon tower and the cartridge filter that are sequentially connected with by pipeline.
Specifically, the first described purpose ceramic-film filter group includes three the first inorganic ceramic film filters being sequentially connected with, the first inorganic ceramic film filter foremost connects the outlet of circulating tank, first inorganic ceramic film filter of least significant end connects circulating tank entrance, and each first inorganic ceramic film filter is all connected with static mixer.
Adopt the method that above-mentioned brine desulfuration system carries out brine desulfuration, as follows including step,
Step one: will containing CaSO4、MgSO4Pump in baffling groove in the salt of impurity, in baffling groove, add NaOH that concentration is 30% and concentration is the Na of 98%2CO3After pump in the first reaction container and react, remove the Ca in former halogen2+And Mg2+；By reacted salt after coarse filter filters, pump into the first inorganic ceramic film filter group and be filtered；
As preferably, the dosage of NaOH: preferably according to Mg2+Required mole conversion needs the amount of the NaOH consumed, after amount 0.1-0.3g/L,
Na2CO3Dosage: preferably according to Ca2+Required mole conversion needs the Na consumed2CO3Amount, after amount 0.2-0.4g/L,
So that the Ca in salt2+And Mg2+Remove more thorough, it is necessary to add excessive Na2CO3And NaOH, but if addition too much can consume substantial amounts of alkali, cost improves；Addition is too low, can cause that salt pH declines, so that the magnesium hydroxide formed and precipitation of calcium carbonate solubility product uprise, calcium in solution, magnesium ion are just of a relatively high and cannot eliminate, it is therefore desirable to strictly control Na2CO3Addition with NaOH.
Step 2: the salt after filtration enters tank before film after pretreatment system, before film, pretreated salt is assigned in nanofiltration membrane separation device and is easily separated sodium sulfate by tank, low glass gall after separation enters in the second reaction container, high glass gall after separation pumps into freezing and crystallizing device, the ten liquid glauber salt slurries crystallized out prepare without liquid glauber salt after dehydration by evaporation drying device thickening dehydration, by the physical partition method of film Yu freezing+full-boiled process, it is possible to the sodium sulfate of 96% in removal system, prepare anhydrous sodium sulfate product
Step 3: the chilled brine that freezing and crystallizing device produces is also in the second reaction container, and adding concentration in the second reaction container is 22% barium chloride (BaCL2) react, remove the SO in salt4 2-；Reacted saline pumps into the second inorganic ceramic film filter group and is filtered, and obtains purification salt.
BaCL2Dosage: preferably according to SO4 2-Required mole conversion needs the BaCL consumed2Amount 94%, so guarantee BaCL2Inexcessive, remaining Ba in minimizing system2+On follow-up impact.
Further, the dense slime water after the first inorganic ceramic film filter group filters in step one can be repeated filtering by circulating tank.
Specifically, it is carry out in 31% mixed in hydrochloric acid, acid-regulating tank adjusting pH value 5-7 that the step that the preprocessed system of the salt after filtering is processed in step 2 includes carrying out static mixer addition concentration, and activated carbon tower carries out filtration of adsorbing and ensure public security.Contain from purpose ceramic-film filter saline out and certain cross alkali number, it is alkaline, its acid-base value is regulated by hydrochloric acid, the pH value of saline is adjusted to 5-7 by alkalescence, this is the NF membrane requirement to saline, because pH value difference can make the electric charge difference of the display of material in solution, so that the charge interaction on material and film surface changes, concentration polarization phenomenon can be made to aggravate, make NF membrane flux reduce simultaneously and salt rejection rate declines, the wherein addition of hydrochloric acid: the amount according to the hydrochloric acid that the how many moles of conversions crossing alkali number consume.
The invention has the beneficial effects as follows, brine desulfuration system of the present invention and method thereof, (1) sodium sulfate in the brine is carried out solventing-out by the technique such as integrated use film, freezing, evaporation denitration and membrane filtration, and the chilled brine of separation goes back to liquid salt workshop, is packaged into storehouse without liquid glauber salt；Sodium sulfate in the refined brine prepared can lower than 0.05g/L, and prepared refining anhydrous sodium sulfate purity is up to more than 99.4%.
(2) present invention can avoid the shortcoming and defect of traditional method, by embrane method device with the use of, it is main for adopting physical desulfurization, and chemical method is auxiliary, effectively provides cost savings, good economy performance, and comprehensive energy consumption is low, and product quality is high, and environmentally safe.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the structured flowchart of brine desulfuration system of the present invention and method thereof.
Detailed description of the invention
In conjunction with the accompanying drawings, the present invention is further detailed explanation.These accompanying drawings are the schematic diagram of simplification, and the basic structure of the present invention is only described in a schematic way, and therefore it only shows the composition relevant with the present invention.
As it is shown in figure 1, tank, nanofiltration membrane separation device, the second reaction container and the second inorganic ceramic film filter group before the baffling groove including being sequentially connected with by pipeline, the first reaction container, coarse filter, the first inorganic ceramic film filter group, pretreatment system, film；
Described nanofiltration membrane separation utensil has two outlets, the respectively outlet of light phase and concentrated phase outlet, the mouth that fades out that described second retort is with described nanofiltration membrane separation device is connected, the concentrated phase outlet of described nanofiltration membrane separation device is connected to freezing and crystallizing device, described freezing and crystallizing utensil has crystallization outlet and brine outlet, described crystallization outlet is connected to dehydration by evaporation drying device, and described brine outlet is connected with described second reaction container.Further, the circulating tank that the dense slime water after the first inorganic ceramic film filter group filters can be iterated through the first inorganic ceramic film filter group it is additionally provided with between coarse filter and the first inorganic ceramic film filter group, wherein said pretreatment system includes the static mixer being sequentially connected with by pipeline, acid-regulating tank, activated carbon tower and cartridge filter, first inorganic ceramic film filter group includes three the first inorganic ceramic film filters being sequentially connected with, the first inorganic ceramic film filter foremost connects the outlet of circulating tank, first inorganic ceramic film filter of least significant end connects circulating tank entrance, each first inorganic ceramic film filter is all connected with static mixer.
Embodiment 1
A kind of method adopting brine desulfuration system to carry out brine desulfuration, as follows including step,
Step one: will containing CaSO4、MgSO4Salt (NaCL300g/L, Ca Deng impurity2+0.65g/L,Mg2+0.02g/L；SO4 2-10g/L), in baffling groove, add the Na of NaOH and the 2.0g/L of 0.15g/L2CO3After pump in the first reaction container and react, remove the Ca in former halogen2+And Mg2+, by reacted salt after coarse filter filters, pump into the first inorganic ceramic film filter group and be filtered.
Step 2: salt (NaCL300g/L, the Ca after filtration2++Mg2+≤ 1mg/L；SO4 2-10g/L) entering nanofiltration membrane separation device after pretreatment system, inflow is 100m3/ h, the low glass gall (SO after separation4 2-0.1g/L, flow 86m3/ h), enter in the second reaction container, the high glass gall (SO after separation4 2-70g/L, flow 14m3/ h) pump into freezing and crystallizing device, the ten liquid glauber salt slurries crystallized out prepare without liquid glauber salt, the chilled brine (SO that freezing and crystallizing device produces after drying through pervaporation, thickener thickening, centrifuge dewatering and drying bed4 2-4g/L) enter in the second reaction container, it is the mixed in hydrochloric acid of 31% that the above-mentioned step that the preprocessed system of salt after filtering is processed includes carrying out static mixer addition concentration, hydrochloric acid addition is carry out in 0.42g/L, acid-regulating tank adjusting pH value (5.5), and activated carbon tower carries out filtration of adsorbing and ensure public security.
Step 3: adding the barium chloride 1.30g/l that concentration is 22% in the second reaction container and react, reacted saline pumps into the second inorganic ceramic film filter group and is filtered, and obtains purification salt (NaCL300g/L, Ca2++Mg2+≤ 1mg/L；SO4 2-0.045g/L)。
The final anhydrous sodium sulfate prepared: product quality reaches GB (GB6009-2003) I class Grade A standard.
Sodium sulfate (Na2SO4) 99.4%, water-insoluble 0.02%, calcium and magnesium (in Mg) resultant 0.05%, chloride (in CL) 0.20%, ferrum (in Fe) 0.001%, moisture 0.01%, whiteness (R457) 86.
The detection of high-purity salt aquatic product quality is as follows:
NaCL300g/L；Ca2++Mg2+0.05mg/L；SO4 2-0.045g/L；SS0.5mg/L.
Embodiment 2
A kind of method adopting brine desulfuration system to carry out brine desulfuration, as follows including step,
Step one: will containing CaSO4、MgSO4Salt (NaCL290g/L, Ca Deng impurity2+0.85g/L,Mg2+0.02g/L；SO4 2-8g/L), in baffling groove, add the Na of NaOH and the 2.45g/L of 0.33g/L2CO3After pump in the first reaction container and react, remove the Ca in former halogen2+And Mg2+, by reacted salt after coarse filter filters, pump into the first inorganic ceramic film filter group and be filtered.
Step 2: salt (NaCL290g/L, the Ca after filtration2++Mg2+0.6mg/L；SO4 2-8g/L) entering nanofiltration membrane separation device after pretreatment system, inflow is 150m3/ h, the low glass gall (SO after separation4 2-0.08g/L, flow 130m3/ h), enter in the second reaction container, the high glass gall (SO after separation4 2-59.5g/L, flow 20m3/ h) pump into freezing and crystallizing device, the ten liquid glauber salt slurries crystallized out prepare without liquid glauber salt, the chilled brine (SO that freezing and crystallizing device produces after drying through pervaporation, thickener thickening, centrifuge dewatering and drying bed4 2-4g/L) enter in the second reaction container, the above-mentioned step that the preprocessed system of salt after filtering is processed includes carrying out static mixer and adds in mixed in hydrochloric acid 0.47g/L that concentration is 31%, acid-regulating tank and carry out adjusting pH value (7.0), and activated carbon tower carries out filtration of adsorbing and ensure public security.
Step 3: adding the barium chloride 1.22g/l that concentration is 22% in the second reaction container and react, reacted saline pumps into the second inorganic ceramic film filter group and is filtered, and obtains purification salt (NaCL290g/L, Ca2++Mg2+0.6mg/L；SO4 2-0.042g/L)。
The final anhydrous sodium sulfate prepared: product quality reaches GB (GB6009-2003) I class Grade A standard.
Sodium sulfate (Na2SO4) 99.6%, water-insoluble 0.01%, calcium and magnesium (in Mg) resultant 0.05%, chloride (in CL) 0.20%, ferrum (in Fe) 0.001%, moisture 0.008%, whiteness (R457) 88.
The detection of high-purity salt aquatic product quality is as follows:
NaCL290g/L；Ca2++Mg2+0.6mg/L；SO4 2-0.042g/L；SS0.5mg/L.
Embodiment 3
A kind of method adopting brine desulfuration system to carry out brine desulfuration, as follows including step,
Step one: will containing CaSO4、MgSO4Salt (NaCL300g/L, Ca Deng impurity2+0.4g/L,Mg2+0.04g/L；SO4 2-15g/L), in baffling groove, add the Na of NaOH and the 1.45g/L of 0.27g/L2CO3After pump in the first reaction container and react, remove the Ca in former halogen2+And Mg2+, by reacted salt after coarse filter filters, pump into the first inorganic ceramic film filter group and be filtered.
Step 2: salt (NaCL300g/L, the Ca after filtration2++Mg2+≤ 1mg/L；SO4 2-15g/L) entering nanofiltration membrane separation device after pretreatment system, inflow is 80m3/ h, the low glass gall (SO after separation4 2-0.2g/L, flow 65m3/ h), enter in the second reaction container, the high glass gall (SO after separation4 2-79g/L, flow 15m3/ h) pump into freezing and crystallizing device, the ten liquid glauber salt slurries crystallized out prepare without liquid glauber salt, the chilled brine (SO that freezing and crystallizing device produces after drying through pervaporation, thickener thickening, centrifuge dewatering and drying bed4 2-3.5g/L) enter in the second reaction container, the above-mentioned step that the preprocessed system of salt after filtering is processed includes carrying out static mixer and adds in mixed in hydrochloric acid 0.45g/l that concentration is 31%, acid-regulating tank and carry out adjusting pH value (6.0), and activated carbon tower carries out filtration of adsorbing and ensure public security.
Step 3: adding the barium chloride 1.68g/l that concentration is 22% in the second reaction container and react, reacted saline pumps into the second inorganic ceramic film filter group and is filtered, and obtains purification salt (NaCL300g/L, Ca2++Mg2+0.8mg/L；SO4 2-0.049g/L)。
The final anhydrous sodium sulfate prepared: product quality reaches GB (GB6009-2003) I class Grade A standard.
Sodium sulfate (Na2SO4) 99.5%, water-insoluble 0.04%, calcium and magnesium (in Mg) resultant 0.05%, chloride (in CL) 0.22%, ferrum (in Fe) 0.001%, moisture 0.009%, whiteness (R457) 87.
The detection of high-purity salt aquatic product quality is as follows:
NaCL300g/L；Ca2++Mg2+0.8mg/L；SO4 2-0.049g/L；SS0.5mg/L.
With the above-mentioned desirable embodiment according to the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not necessarily departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content in description, it is necessary to determine its technical scope according to right.
Claims (7)
1. one kind adopts the method that brine desulfuration system carries out brine desulfuration, it is characterised in that:
Tank, nanofiltration membrane separation device, the second reaction container and the second inorganic ceramic film filter group before baffling groove that described brine desulfuration system includes being sequentially connected with by pipeline, the first reaction container, coarse filter, the first inorganic ceramic film filter group, pretreatment system, film；
Described nanofiltration membrane separation utensil has two outlets, the respectively outlet of light phase and concentrated phase outlet, the mouth that fades out that described second retort is with described nanofiltration membrane separation device is connected, the concentrated phase outlet of described nanofiltration membrane separation device is connected to freezing and crystallizing device, described freezing and crystallizing utensil has crystallization outlet and brine outlet, described crystallization outlet is connected to dehydration by evaporation drying device, and described brine outlet is connected with described second reaction container；
Comprise the following steps that
Step one: pending salt is pumped in baffling groove, in baffling groove add concentration be 30% NaOH and concentration be the Na of 98%2CO3After pump in the first reaction container and react, by reacted salt after coarse filter filters, pump into the first inorganic ceramic film filter group and be filtered；
Step 2: the salt after filtration enters tank before film after pretreatment system, before film, pretreated salt is assigned in nanofiltration membrane separation device and carries out nanofiltration separation by tank, low glass gall after separation enters in the second reaction container, high glass gall after separation pumps into freezing and crystallizing device, and the ten liquid glauber salt slurries crystallized out prepare without liquid glauber salt after dehydration by evaporation drying device thickening dehydration；
Step 3: the chilled brine that freezing and crystallizing device produces is also in the second reaction container, and adding concentration in the second reaction container is that 22% barium chloride reacts, and reacted saline pumps into the second inorganic ceramic film filter group and is filtered, and obtains purification salt.
2. the method for brine desulfuration as claimed in claim 1, it is characterised in that: in step one, the dosage of NaOH is according to Mg2+Required mole calculates the amount of the NaOH needing consumption, after amount 0.1-0.3g/L；
Na2CO3Dosage be according to Ca2+Required mole conversion needs the Na consumed2CO3Amount, after amount 0.2-0.4g/L.
3. the method for brine desulfuration as claimed in claim 1, it is characterised in that: the dense slime water after the first inorganic ceramic film filter group filters in step one can be repeated filtering by circulating tank.
4. the method for brine desulfuration as claimed in claim 1, it is characterised in that: the step that the preprocessed system of the salt after filtering is processed in step 2 includes carrying out static mixer, and to add concentration be that to carry out adjusting pH value in 31% mixed in hydrochloric acid, acid-regulating tank be that 5-7, activated carbon tower adsorb and ensure public security filtration.
5. the method for brine desulfuration as claimed in claim 1, it is characterised in that: it is additionally provided with the dense slime water after the first inorganic ceramic film filter group can being filtered between described coarse filter and the first inorganic ceramic film filter group and iterates through the circulating tank of the first inorganic ceramic film filter group.
6. the method for the brine desulfuration as described in claim 1 or 5, it is characterised in that: described pretreatment system includes the static mixer, acid-regulating tank, activated carbon tower and the cartridge filter that are sequentially connected with by pipeline.
7. the method for brine desulfuration as claimed in claim 6, it is characterized in that: the first described purpose ceramic-film filter group includes three the first inorganic ceramic film filters being sequentially connected with, the first inorganic ceramic film filter foremost connects the outlet of circulating tank, first inorganic ceramic film filter of least significant end connects circulating tank entrance, and each first inorganic ceramic film filter is all connected with static mixer.
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| CN105645440B (en) * | 2015-12-30 | 2018-02-23 | 中国中轻国际工程有限公司 | A kind of mirabilite hydrate produces sodium sulphate technique |
| CN106082278A (en) * | 2016-06-20 | 2016-11-09 | 中盐金坛盐化有限责任公司 | A kind of Galuber's salt type brine removes the purification method of strontium element |
| CN105905927B (en) * | 2016-06-20 | 2017-10-31 | 中盐金坛盐化有限责任公司 | A kind of Galuber's salt type brine removes the bittern purifying device and method of strontium element |
| CN107879369A (en) * | 2016-09-29 | 2018-04-06 | 内蒙古乌海化工有限公司 | A kind of Waste Sulfuric Acid processing system and method |
| CN110759361B (en) * | 2018-07-25 | 2021-06-15 | 江苏省制盐工业研究所有限公司 | Method for poly-generation of potassium lithium nitrate by sodium sulfate type brine or mother liquor of potassium nitrate |
| CN112588008B (en) * | 2020-12-04 | 2022-09-13 | 安徽华塑股份有限公司 | Brine denitration and ammonium removal integrated treatment system for full-brine alkali preparation |
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| CL2008000676A1 (en) * | 2007-03-06 | 2008-10-10 | Tech Resources Pty Ltd | METHOD OF SEPARATION OF POTASSIUM CHLORIDE AND SODIUM CHLORIDE FROM A HEATED SOLUTION OF THESE SALTS THAT INCLUDES PASSING THE SOLUTION THROUGH A MEMBRANE SYSTEM, EXTRACTING THE WATER TO PRECIPITATE SODIUM CHLORIDE, SEPARATE THE PRECIPITATE, ENFORCEMENT |
| CN102432037A (en) * | 2011-12-05 | 2012-05-02 | 中盐金坛盐化有限责任公司 | Original halogen denitration production process and production equipment |
| CN202400919U (en) * | 2011-12-30 | 2012-08-29 | 青岛华轩环保科技有限公司 | Reusing and treating system for desalinizing high-concentration seawater through seawater membrane filtering |
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