CN100460326C - Method of refining salt by membrane filtration - Google Patents
Method of refining salt by membrane filtration Download PDFInfo
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- CN100460326C CN100460326C CNB2006100388686A CN200610038868A CN100460326C CN 100460326 C CN100460326 C CN 100460326C CN B2006100388686 A CNB2006100388686 A CN B2006100388686A CN 200610038868 A CN200610038868 A CN 200610038868A CN 100460326 C CN100460326 C CN 100460326C
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Abstract
A membrane filter process for refining saline includes such steps as dissolving salt to obtain saturated solution, adding sodium hydroxide, sodium carbonate and barium chloride, reaction to generate magnesium hydroxide, calcium carbonate and barium sulfate, adding coagulating precipitant and oxidant for pre-treating, adsorbing and depositing to remove magnesium hydroxide colloid and part of particles, cross-flow filtering by inorganic membrane, and ion exchange.
Description
Technical field
The present invention relates to a kind of chlorine industry salt refining method, relate in particular to a kind of with mineral membrane cross flow filter technology salt refining method.
Background technology
Electrolysis process mainly contains diaphragm process, mercury process, ion exchange membrane in the chloralkali process.Wherein mercury process is gradually eliminated for generally acknowledged toxic substance because of mercury, what application was more now is diaphragm process and ion exchange membrane, ion exchange membrane because of its less investment, energy consumption is low, working cost is little, pollution-free gaining great popularity, adopted by increasing chlor-alkali plant.Ionic membrane is the core that ion film caustic soda is produced, though it does not participate in electrochemical reaction directly, influences physical processes such as mass transfer, conduction, the Ca in its operation medium salt solution
2+, Mg
2+In electrolytic process with from cathode compartment, permeate the OH of coming Deng impurity
-Reaction forms insolubles and is deposited on the ionic membrane, causes the destruction of ionic membrane physicals, causes the reduction of ionic membrane current efficiency, power consumption increase, side reaction aggravation, quality product to descend.More and more cause the attention of enterprise so go into groove brinish quality, with regard to traditional flocculating settling technology, calcium, magnesium insolubles are removed and are not full of a subject matter that influences electric groove operating index.
Existing refining general tradition " barrel type reactor+Dao Er settling tank+sand-bed filter " technology that adopts of primary brine of domestic chlor-alkali enterprise is with NaOH and Na
2CO
3For finishing agent, TXY (sodium polyacrylate) are that settling agent, hydrochloric acid are the neutralizing agent refined brine; Beginning in 1999, to raise agricultural chemical industry group company, begin to adopt the filtering technique of U.S. Ge Er company, chlor-alkali producer such as the positive chemical industry in Binhua Group Co., Ltd., Shandong, Yanhua Co., Ltd., Yunnan and Chongqing three company limited successively introduces this filtering technique; Secondary brine rectification process adopts carbon pipe filter to filter mostly, through neutralization, heating, gets secondary refining salt solution through chelate resin tower absorption again, uses for each factory's ion-membrane electrolysis device.
The traditional technology idiographic flow is: bittern and the next impurity salt solution that is rich in of evaporation section through refinement treatment enter storage tank for salt dissolving water, enter salt dissolving tank through changing brinepump; Become saturated crude brine after changing salt water dissolution crude salt, overflow from salt dissolving tank top; After being metered into finishing agent NaOH, saturated crude brine enters medial launder, is pumped into reactor by crude brine, adds finishing agent Na again
2CO
3, after cohesion settling agent TXY (sodium polyacrylate), flow into settling tank certainly; The clear liquid that settling tank comes out enters sand-bed filter, enters the sand filtration clarified brine storage tank after sand-bed filter filters; The sand filtration refined brine is after the pressurization of sand filtration refined salt water pump enters the filtration of PE (polyethylene) pipe filter, and its clear liquid enters clarified brine storage tank No. one time, enters carbon pipe filter through the pressurization of refined salt water pump; Enter resin tower at last, after ion exchange tower is refining, enter the anolyte circulation groove, use in electrolysis.This technology main drawback has: be subjected to salt quality influence big, brine quality is unstable, filter that suspended solid (SS) in the salt solution of back exceeds standard and strainer easily stops up and comes off etc.
Gore film method refined brine technology (Z100127853) is specially: the backflow saltwater is replenished clear water add from changing the salt trench bottom, by salt deposit, change salt to saturated, be spilled over to reactive tank from changing salt bath top, be metered into finishing agent NaOH and BaCl
2After, enter medial launder.Crude brine is pumped into the pressure air-dissolving jar by crude brine, after decompression, enters air flotation slot after being metered into oxygenant, and clear liquid goes out from the overflow of air flotation slot top, is metered into finishing agent Na
2CO
3After enter reactive tank, fully reaction back overflow enters the filtrate groove, enters the gore film strainer after the pressurization of Ge Er fresh feed pump, filtrate overflows from the top of gore film strainer, enters the clarified brine storage tank use in electrolysis No. one time after being metered into hydrochloric acid.This kind technology used the composite tube filter membrane of PTEE film/PP have following problem: the combined strength bination of (1) two kind of material is low; (2) filter membrane lap-joint easily breaks; (3) in the salt solution free chlorine, oxymuriate to the PP material corrosion; (4) be subjected to the influence of pretreating effect, filtration capacity changes too greatly.Show as in production application that filter membrane is easy to crack, damaged, the life-span is short etc., makes this technology management difficulty aborning strengthen.
Though the HVM film of the full PTEE material of Singapore Hyflux can remedy the defective that the composite tube filter membrane of existing PTEE film/PP exists, adopted by units such as shore, China Shandong grouping of the world economy factories, but it uses membrane filtration technique the same with the gore film method, all is that terminal type filters.As shown in Figure 8, end-filtration is because feedstock direction is vertical with face, gather filter cake at face easily, cause flux to descend rapidly, filtration resistance increases, and recoils and has brought very big pressure to film strength for keeping high frequency that flux carries out, it also is the easy disruptive reason of gore film filter membrane lap-joint, though the HVM film has improved film toughness, still exist filter cake to gather rapidly, the flux shortcoming faster that descends.The cross flow filter technology has then overcome above-mentioned shortcoming, and as shown in Figure 9, its feedstock direction is parallel to face, and face is had good souring, can effectively reduce the filter cake deposition, significantly improves membrane flux, reduces the cleaning interval (as the recoil frequency) of film.Main solid particle is CaCO in China's refined brine process
3And Mg (OH)
2Practice shows CaCO
3Form the filter cake porous and easily come off, filtration resistance is advanced the speed low, and the backwash ratio is easier to, and Mg (OH)
2Be colloid, recoil filter cake difficult drop-off, sedimentation.Existing end-filtration salt refining method adopts usually with CaCO
3And Mg (OH)
2The isolating method of substep has increased processing step, and floor space is bigger.
Summary of the invention
The salt refining method that the purpose of this invention is to provide a kind of novelty, this method use the mineral membrane cross-flow filter of special construction to realize solid-liquid separation, simplify existing technology, can disposablely obtain qualified high-quality refined brine.
Technical scheme of the present invention comprises step:
A kind of method of membrane filtration technique refined brine, its step comprises:
A) bittern and the next salt solution that is rich in impurity of evaporation section through refinement treatment enters storage tank for salt dissolving water, enters salt dissolving tank through changing brinepump, becomes saturated crude brine behind the change salt water dissolution crude salt, is spilled over to reactive tank from salt dissolving tank top;
B) disposable finishing agent sodium hydroxide, yellow soda ash and the bariumchloride chemical agent of being metered into generates magnesium hydroxide colloid, lime carbonate and barium sulfate solid matter with the reaction of the foreign ion in the salt solution;
C) add cohesion settling agent and oxygenant and carry out pre-treatment, remove magnesium hydroxide colloid and other part solid particulate by absorption and co-precipitation;
D) salt solution enters the mineral membrane cross-flow filter through pump and filters, the penetrating fluid that sees through mineral membrane enters into ion exchange resin, obtain refined brine after treatment, the salt solution that is rich in impurity that does not see through film returns pre-treatment step and adsorbs once more and co-precipitation, enters the mineral membrane cross-flow filter then and filters.
Wherein salt solution is controlled transmembrane pressure 0.05MPa-0.5MPa, crossflow velocity 0.5m/s-3m/s among the step D when pump enters the mineral membrane cross-flow filter.NaOH and Na among the step C
2CO
3Add volumetric molar concentration respectively greater than Ca
2+With Mg
2+Volumetric molar concentration 1-5%, BaCl
2Add volumetric molar concentration less than SO
4 2-Volumetric molar concentration 1-5%.
Wherein said cohesion settling agent is sodium polyacrylate, polyacrylamide or causticization starch; Described oxygenant is clorox, hydrogen peroxide or chlorinated lime.
Wherein the mineral membrane cross-flow filter comprises housing 3, film filtering element 4, upper face plate 5 and lower face plate 10, crude salt water cavity 2 and is rich in the salt water cavity 6 of impurity, fix several film filtering elements 4 according to required treatment capacity between upper face plate 5 and the lower face plate 10, be separated to form the salt water cavity 6 that is rich in impurity between upper face plate 5 and the housing, be separated to form crude salt water cavity 2 between lower face plate 10 and the housing.
The mineral membrane cross-flow filter is equipped with recoiling device interface 9, when membrane flux drops to the 40-50% of initial flux, adopt refined brine interval backflushing membrane separation apparatus automatically, will come off attached to the filter cake on the face, be deposited to the bottom of separator, thereby prevent that effectively film from polluting; Perhaps use the method for matting (as pickling), membrane flux is recovered substantially.The salt slurry process press filtration or the suction filtration that produce in pre-treatment and the membrane filtration processes, returning of the salt solution salt section of acquisition, solid slag is then worked as waste disposal.
Wherein the separatory membrane in the film filtering element is the tubular type mineral membrane, and it is the symmetry or the asymmetric membrane of pottery, metal or its matrix material formation of 0.1-10 μ m that mineral membrane adopts mean pore size, and the diameter of membrane channel 12 is 4-10mm, and single tube or hyperchannel all can.The present invention is big with the design of membrane channel diameter, mainly is that solid impurity is more in the treating process according to China's salt solution characteristics, even guarantee that the face filter cake deposits under the more situation in filtration procedure, also is unlikely to take place membrane channel and stops up.
The inventive method is for increasing the face cross flow effects, turbulence promoter (Fig. 2 can be installed in membrane channel, a is a column type, and b is spiral, and c is a wound form), turbulence promoter can improve the face velocity of shear, take away the particle of film surface deposition, reduce film and pollute, and can improve membrane flux, as shown in Figure 3, salt solution is mainly by 14 transmission of the annular channel between turbulence promoter 13 and membrane channel.Fig. 4 is the single channel architecture synoptic diagram of tubular type mineral membrane in the inventive method, and turbulence promoter is directly installed in the middle of the membrane channel, the kind of turbulence promoter, can select with the distance of face, motion morphology etc.
Beneficial effect
1, with Fig. 5 among the technical process of traditional refined brine and Fig. 6 the technical process of gore film method refined brine compare, membrane filtration processes is except that producing clear liquid in the inventive method 6, produce the salt solution that is rich in impurity in addition, by it being returned the settled repeatedly operation of pretreater, more salt slurries are stayed outside the film filter, reduce the processing load of membrane separation apparatus, guaranteed the high permeating flux and the processing efficiency of membrane separation apparatus.
2, compare with the technical process of traditional refined brine among Fig. 5, the inventive method Fig. 7 will be because of generating Mg (OH) with the mineral membrane cross-flow filter
2, CaCO
3With BaSO
4One step of reaction Deng solid matter finishes, and has reduced operation steps; Finish the work of sand-bed filter and carbon pipe filter, technical process is obviously shortened.Compare with the technical process of Fig. 6 gore film method refined brine, the inventive method because of the use filtering technique separates various form solid matters all can keep higher flux, so need not generate Mg (OH) earlier
2Regeneration CaCO
3Precipitation.
3, the gore film method is used end-filtration, the face filter cake gathers comparatively fast, the flux decay in order to keep working efficiency, must frequently use high-frequency impulse to clean film rapidly, make the film damage of breaking easily, and the present invention reduces the face deposition of filter cake by the face cross flow effects of cross flow filter, can significantly reduce the recoil wash number, increase work efficiency, cut down the consumption of energy;
4, adopt the inventive method refined brine can obtain calcium contents, magnesium total content less than 3mg/L, sulfate radical content is less than 10mg/L, and SS content is less than the salt solution of 1mg/L.
Description of drawings
Fig. 1 is a mineral membrane cross-flow filter structural representation of the present invention;
Fig. 2 is the turbulence promoter of the used reinforcement cross flow filter of the present invention effect;
Fig. 3 is the end face structure synoptic diagram of the used tubular type mineral membrane of the present invention;
Fig. 4 is equipped with the channel architecture synoptic diagram of turbulence promoter for the used tubular type mineral membrane of the present invention.
1-crude brine import among the figure, 2-crude salt water cavity, 3-housing, 4-film filtering element, 5-upper face plate, 6-are rich in the impurity salt water cavity, 7-is rich in impurity salt water out, the outlet of 8-refined brine, 9-recoiling device interface, 10-lower face plate, 11-slag notch, 12-membrane channel, 13-turbulence promoter, 14-annular channel;
D-crude brine, E-be rich in salt solution, F-refined brine, G-backwash liquid, the H-filter residue of impurity
Fig. 5 is the process flow sheet of traditional refined brine.
Fig. 6 is the process flow sheet of gore film method refined brine.
Fig. 7 is the process flow sheet of refined brine of the present invention.
Fig. 8 is the end-filtration synoptic diagram.
Fig. 9 is the cross flow filter synoptic diagram.
Embodiment
Embodiment 1
The present invention will be described in detail below in conjunction with width of cloth figure
A) bittern and the next salt solution that is rich in impurity of evaporation section through refinement treatment enters storage tank for salt dissolving water, enters salt dissolving tank through changing brinepump, becomes saturated crude brine behind the change salt water dissolution crude salt, is spilled over to reactive tank from salt dissolving tank top;
B) in reactive tank, be metered into finishing agent NaOH, Na
2CO
3, BaCl
2Make Ca in the salt solution Deng chemical agent
2+, Mg
2+, SO
4 2-Generate Mg (OH) Deng reaction
2, CaCO
3With BaSO
4Deng solid matter, wherein NaOH and Na
2CO
3Add concentration respectively greater than Ca
2+With Mg
2+Concentration 1-5%, BaCl
2Adding concentration less than SO
4 2-Concentration 1-5%;
C) above-mentioned salt solution enters pretreater, adds cohesion settling agent sodium polyacrylate, polyacrylamide or causticization starch; Remove Mg (OH) by absorption and co-precipitation
2And other part solid particulate, add oxygenant clorox, hydrogen peroxide or chlorinated lime simultaneously to remove organic impurity, enter the inorganic membrane filtration device then;
D) as shown in Figure 1, salt solution enters film filter through import 1 and arrives crude salt water cavity 2 in the inventive method, enters then in the tubular type inorganic ceramic film 4, the penetrating fluid direction flows to perpendicular to crude brine, discharge through exporting 8, enter ion exchange resin, after exchange, obtain high-quality refined brine.The salt solution of holding back that is rich in impurity is then through exporting 7 discharge filters, turn back in the pretreater with above-mentioned steps B) in the salt solution that produces carry out precipitating action once more, so that more solid matter is removed, thereby reduce the solid matter that enters film filter in this step, reduce film and pollute.When the mineral membrane cross-flow filter significantly was reduced to set(ting)value when flux, back-purge system started automatically, carried out counterflush through 9 pairs of separatory membranes of backwash liquid import, and filter cake is come off, and was deposited to the bottom of separator.Also can use matting (as pickling), membrane flux is recovered substantially.When running up to a certain degree, the filter cake amount can discharge filter residue automatically through slag-drip opening 11.Salt slurry in pretreater and the film filter is after press filtration, and liquid returns steps A), the solid filter residue is then when the waste residue processing.
Embodiment 2
Calcium contents 754.2mg/L in the crude brine after the change salt, Mg content 83.21mg/L, sulfate radical content 7.6g/L, SS content 3589.33mg/L.This saturated brine is sent in the reactive tank, add sodium hydroxide 0.4g/L, yellow soda ash 1.6g/L and bariumchloride 12.5g/L and react, enter pretreater after reaction finishes, add polyacrylamide 50mg/L and hydrogen peroxide 30mg/L, behind adsorption coprecipitation, be pumped into the mineral membrane cross-flow filter, adopting the aperture is the ceramic membrane of 0.02 μ m, 19 passages, passage internal diameter 4mm (turbulence promoter is not installed in the passage), cross-flow velocity 1m/s, working pressure 0.4MPa, membrane permeation flux 0.5m
3M
-2H
-1, experiment is carried out 5h and be need not film is recoiled.With ICP (plasma emission spectrum) salt solution after filtering is measured, calcium, magnesium and SS all do not detect, and sulfate radical content 5.1mg/L meets high-quality refined brine standard fully.
Embodiment 3
Embodiment 1 identical saturated brine is sent in the reactive tank, add sodium hydroxide 0.4g/L, yellow soda ash 1.6g/L and react with bariumchloride 12.5g/L, enter pretreater after reaction finishes, adding sodium polyacrylate 60mg/L and hypochlorous acid are received 40mg/L, behind adsorption coprecipitation, be pumped into the mineral membrane cross-flow filter, adopting the aperture is the ceramic membrane of 0.02 μ m, 7 passages, passage internal diameter 6mm, cross-flow velocity 2m/s, working pressure 0.3MPa, membrane permeation flux 0.6m
3M
-2H
-1, experiment is carried out 10h and be need not film is recoiled.With ICP (plasma emission spectrum) salt solution after filtering is measured, calcium, magnesium and SS all do not detect, and sulfate radical content 5.0mg/L meets high-quality refined brine standard fully.
Embodiment 4
Embodiment 1 identical saturated brine is sent in the reactive tank, adding sodium hydroxide 0.4g/L, yellow soda ash 1.6g/L and bariumchloride 12.5g/L reacts, after finishing, reaction enters pretreater, add sodium polyacrylate 600mg/L and chlorinated lime 50mg/L, behind adsorption coprecipitation, be pumped into the mineral membrane cross-flow filter, adopting the aperture is the ceramic membrane of 0.2 μ m, 19 passages, passage internal diameter 6mm (turbulence promoter is installed in the passage), cross-flow velocity 0.5m/s, working pressure 0.3MPa, membrane permeation flux 2.0m
3M
-2H
-1, experiment is carried out 10h and be need not film is recoiled.With ICP (plasma emission spectrum) salt solution after filtering is measured, calcium contents does not detect, Mg content 2.0mg/L, and SS content 0.2mg/L, sulfate radical content 8.3mg/L meets high-quality refined brine standard fully.
Claims (9)
1. the method for a refining salt by membrane filtration, its step comprises:
A) bittern and the next salt solution that is rich in impurity of evaporation section through refinement treatment enters storage tank for salt dissolving water, enters salt dissolving tank through changing brinepump, becomes saturated crude brine behind the change salt water dissolution crude salt, is spilled over to reactive tank from salt dissolving tank top;
B) disposable finishing agent sodium hydroxide, yellow soda ash and the bariumchloride chemical agent of being metered into generates magnesium hydroxide colloid, lime carbonate and barium sulfate solid matter with the reaction of the foreign ion in the salt solution;
C) add cohesion settling agent and oxygenant and carry out pre-treatment, remove magnesium hydroxide colloid and other part solid particulate by absorption and co-precipitation;
D) salt solution enters the mineral membrane cross-flow filter through pump and filters, the penetrating fluid that sees through mineral membrane enters into ion exchange resin, obtain refined brine after treatment, the salt solution that is rich in impurity that does not see through film returns pre-treatment step and adsorbs once more and co-precipitation, entering the mineral membrane cross-flow filter then filters, wherein salt solution is controlled transmembrane pressure 0.05MPa-0.5MPa, crossflow velocity 0.5m/s-3m/s when pump enters the mineral membrane cross-flow filter; It is the symmetry or the asymmetric membrane of pottery, metal or its matrix material formation of 0.1-10 μ m that mineral membrane adopts mean pore size.
2. the method for claim 1, its feature is NaOH and Na in step C
2CO
3Add volumetric molar concentration respectively greater than Ca
2+With Mg
2+Volumetric molar concentration 1-5%, BaCl
2Add volumetric molar concentration less than SO
4 2-Volumetric molar concentration 1-5%.
3. the method for claim 1, it is characterized in that condensing settling agent is sodium polyacrylate, polyacrylamide or causticization starch.
4. the method for claim 1 is characterized in that oxygenant is clorox, hydrogen peroxide or chlorinated lime.
5. the method for claim 1, it is characterized in that the mineral membrane cross-flow filter comprises housing (3), film filtering element (4), upper face plate (5) and lower face plate (10), crude salt water cavity (2) and is rich in the salt water cavity (6) of impurity, fix several film filtering elements (4) according to required treatment capacity between upper face plate (5) and the lower face plate (10), be separated to form the salt water cavity (6) that is rich in impurity between upper face plate (5) and the housing, be separated to form crude salt water cavity (2) between lower face plate (10) and the housing.
6. method as claimed in claim 5, it is characterized in that the mineral membrane cross-flow filter is equipped with recoiling device interface (9), when membrane flux drops to the 40-50% of initial flux, automatically adopt refined brine interval backflushing membrane separation apparatus, to come off attached to the filter cake on the face, be deposited to the bottom of separator, thereby prevent that effectively film from polluting; Perhaps use the method for matting, membrane flux is recovered substantially.
7. method as claimed in claim 5 is characterized in that the separatory membrane in the film filtering element is the tubular type mineral membrane, and the diameter of membrane channel (12) is 4-10mm, and single tube or hyperchannel all can.
8. method as claimed in claim 7 wherein can be installed turbulence promoter in the tubular type mineral membrane passage.
9. the method for claim 1, the salt slurry that produces in pre-treatment and the membrane filtration processes be through press filtration or suction filtration, returning of the salt solution salt section of acquisition, and solid slag is then worked as waste disposal.
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| CN1868878A (en) | 2006-11-29 |
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