CN102311097A - Method for extracting bromine from seawater by utilization of bipolar membrane - Google Patents
Method for extracting bromine from seawater by utilization of bipolar membrane Download PDFInfo
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- CN102311097A CN102311097A CN 201110224899 CN201110224899A CN102311097A CN 102311097 A CN102311097 A CN 102311097A CN 201110224899 CN201110224899 CN 201110224899 CN 201110224899 A CN201110224899 A CN 201110224899A CN 102311097 A CN102311097 A CN 102311097A
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Abstract
The invention relates to the field of ocean chemical engineering, specifically to a method for extracting bromine from seawater by the utilization of a bipolar membrane device. The method provided by the invention comprises the following steps of: preparing a macroporous highly basic anion exchange resin in advance, pretreating the resin for later use, clearing and filtering seawater, placing into an anode chamber of the bipolar membrane device, disposing a sodium chloride solution into a salt chamber of the bipolar membrane device, and effecting by current to generate acid and alkali; oxidizing related substances in seawater by the bipolar membrane device, allowing bromine to go through the resin and to be absorbed on the resin, finally washing out the above bromine absorbed on the resin, followed by regular distillation and rectification to obtain the finished product. By the adoption of the method provided by the invention, the high purity of the prepared product is high, the debromination effect from seawater is good, and there exist no environmental problems such as secondary pollution and the like. The method provided by the invention can be widely applied in coastal regions.
Description
Technical field
The invention belongs to the marine chemical industry field, specifically be meant a kind of method of utilizing the Bipolar Membrane device from seawater, to carry bromine.
Technical background
The bromine resource of China can be divided into four types: fld underground water bromine resource, salt lake brine bromine resource, sea salt field bittern water bromine resource and salt mining site bittern bromine resource.Wherein fld subsurface brine and salt lake brine are to contain the bittern bromine resource that bromine concentration is relatively the highest, quality is best; (water) saltern, sea bittern distribution of water resources is wide, quantity is big, is big promising bittern bromine resource; Salt mining site bittern bromine resource is the bittern bromine resource type that just grows up in recent years, and this bittern bromine resource means the bromine resource in the remaining bittern of natural bittern salt manufacturing mining site.In view of in the bittern salt manufacturing concentration process, bittern constantly concentrates, and bromine content constantly increases, and remaining bittern bromine content last after its salt manufacturing is high.
60,000 tons of China's bromine YO account for 1/10th of Gross World Product, and output occupies the third place in the world.Wherein 80% derive from the Shandong Province subsurface brine bromine resource; But because problems such as Technology cause the bromine resource utilization to be had only about 65%, caused a large amount of wastes of resource, also shortened resource longevity simultaneously; The brominated amount of subsurface brine is also in rapid decline, and China's bromine resource faces a crisis.For satisfying in the 21 century national economic development demand to bromine 3%-5% rate of increase; Face the situation that subsurface brine bromine resource lacks day by day; Need development and use to have the brominated resource-seawater or the concentrated seawater (the brominated 130mg/L of being) of strategic importance; Exploitation has the multiple seawater of independent intellectual property right and puies forward the bromine new technology, with the thorough resource problem that solves China's bromine industry Sustainable development.Thus, be necessary bromine characteristics of resources, digesting and assimilating on the basis of introducing external first system bromine technology and bromine deep process technology that exploitation adapts to the system bromine technology and the bromize product of China's bromine resources characteristic and the market requirement according to China.
Along with Chinese economic development, the bromine series product will have big demand in fields such as refrigeration, petroleum drilling, medicine, agricultural chemicals, fire-retardant, sterilization, printing and dyeing.It is predicted; Bromine is medicine intermediate two bromals, TMB, 2; 4,6-bromamide, Hydrogen bromide, dyestuffs industries with bromamine acid, disperse orchid, disperse grey, phenyl-monobromide all to have development prospect preferably around green onion ketone, dibromo-benzene green onion ketone, bromine flame retardant tetrabromo-bisphenol, decabromodiphenyl oxide, brominated agricultural chemicals RE-4355, bromobenzene eyeball, bromine cyanogen chrysanthemum vinegar, refrigeration agent lithiumbromide, drill in fluid Calcium Bromide, zinc bromide and the bromofenofos, sterilant dichlorophen etc. that are used for veterinary drug.
In a word, along with the continuous developing of development and national economy and bromine series product, the importance of bromine is more and more outstanding.According to the practical situation of the Economic development of present China and the market requirement, industrial unrestrained element should keep the optimum development impetus, makes every effort to digest voluntarily, makes great efforts to increase export.Take to introduce advanced foreign technology and the self-policy that combines of developing, the Development patterns and the experience of reference and learning overseas major company are improved production technology, improve automatic control degree.Pay attention to the increase of bromine deep processing transformation efficiency and kind, greatly develop bromine series product, strive making bromine of China and bromine produced in series to catch up with advanced world levels as early as possible with high added value.
As the important element of marine chemical resource development and use, bromine and bromine product play crucial effect in national economy.Modern age particularly,, the demand of bromine flame retardant is heightened along with the development of plastics industry and the projection of Highrise buildings.In addition, ban use of freon refrigerant in the world, therefore the demand with the lithium bromide refrigerating agent increases suddenly.Supply falls short of demand for the domestic old bromine mode of production, and seawater is put forward the bromine engineering and seemed severe and urgent.Bromine is as the main chemical compositions in the concentrated seawater, and its concentration is the nearly twice in the nature seawater.Therefore, extract the bromine resource in the concentrated seawater rationally, effectively, for reducing the sea water desaltination cost, reduce Marine Environmental Pollution, the fast development of promotion sea water desaltination industry and marine chemical industry industry etc. all has important practical significance.And concentrated seawater is proposed the development of bromine technology, and good promoter action is played in the comprehensive utilization of concentrated seawater chemical resource, also certain directive function is played in the extraction of chemical elements such as iodine, sodium and potassium in the concentrated seawater.
Desalting process is when making the main products desalination water, and also exporting sub product continuously is concentrated seawater.Contain number of chemical element and compound resource in the concentrated seawater than concentration is higher in the former seawater; Like non-metallic element chlorine, bromine, iodine; Metallic element sodium, potassium, magnesium, calcium, the heavy element uranium of nuclear fission reaction and the light element of nuclear fusion reaction, and the nuclear raw material heavy water etc.Wherein sodium, potassium, magnesium and bromine etc. are important basic chemical industry raw materials, and uranium, neon, neon and heavy water etc. then are few important energy source of land resources reserves and strategic materials.The processing and get from the solid that picks up from the land or liquid mineral reserve mostly of these materials, extraction is extremely rare from concentrated seawater.At present, the scarcely treated in line sea of going into of the concentrated seawater after the sea water desaltination.Valuable chemical resource is directly run off, and the sea life in certain zone are caused extinction, even formation " Dead Sea ".
At present, the domestic method of carrying bromine mainly contains air and blows out method, steam distillation, solvent extration, gaseous state embrane method, resin adsorption method etc.The common ground of these methods all is to extract after being oxidized to simple substance bromine to the bromide anion in the seawater in advance again, and the oxygenant that generally adopts is a chlorine.Before with chlorine oxidation, brominated raw material should be removed insolubles impurity earlier, regulates its pH value with acid then, and it is controlled between the 3-5.
Resin adsorption method is a purpose of utilizing ion exchange method to reach to carry bromine.Ion exchange process is a kind of stoichiometry distribution process that separated component takes place between the aqueous solution and solid ion exchanger; Have excellent separation selectivity and very high cycles of concentration; And easy to operate, in recovery, enrichment and the detached job in a lot of fields, brought into play remarkable technical functionality.At present; Ion exchange technique has obtained widespread use in fields such as chemical industry, medicine, food, water treatment, hydrometallurgy, environment protection and nuclear fuel reprocessing; Become after typical separate technology such as distillation, extraction, absorption the new chemical separation technology a kind of commonly used that emerges.
It is the ion exchange resin absorption method that seawater is put forward bromine method relatively more commonly used at present, and mainly comprise: seawater acidifying, chlorine oxidation, macroporous resin adsorption, pickling desorb, rectifying separation, cooling are collected.Raw material seawater or concentrated seawater elder generation clarification filtration are used hcl acidifying then, feed liquid chlorine and carry out oxidation.Seawater after the oxidation is through resin layer, and when contacting with resin, free bromine is attracted on the resin.After a certain amount of bromine of resin absorption, stop connecting the sea water, in resin column, feed hydrochloric acid soln again, carry out wash-out.What wash-out came out is to contain the higher solution of bromine concentration, and solution promptly obtains the finished product bromine after cooling off collection through rectifying separation.
There is the problem of safety and environmental protection in above various method for extracting bromine owing to used liquid chlorine.
Summary of the invention
The present invention utilizes the utmost point chamber of Bipolar Membrane that bromine is carried out oxidation, and to replace the oxidising process of former technology, the acid that Bipolar Membrane produces comes the resin of absorption bromine is carried out pickling, and last waste liquid neutralizes with the alkali that Bipolar Membrane produces.Need not add the acid that oxygenant, pickling such as chlorine are used in the whole technology in addition, not produce acid-bearing wastewater at last, make the whole bromine process of carrying need not to use liquid chlorine, also need not to add in addition acid comes the drip washing resin, does not also have advantages such as spent acid generation at last.
The raw water that the present invention carries bromine is seawater, can certainly be the dense water of desalination, subsurface brine of seawater etc.;
The present invention is achieved through following technical proposals:
A kind of method of utilizing Bipolar Membrane from seawater, to carry bromine is characterized in that comprising the steps:
(1) with pure water macroporous strong basic anionite-exchange resin was soaked more than 24 hours, wash to water outlet limpid then; The used typical resins of the present invention is the D201 resin;
(2) soak above-mentioned resin more than 2 hours with 1.0mol/LNaOH solution, washing is to neutral again;
(3) more than 3 hours, make resin fully transfer the Cl type to the above-mentioned resin of 2.0mol/L HCI solution soaking, use pure water subsequent use to pH2.0-3.0 again resin wash;
(4) carry out clarification filtration to seawater, it is 4.0～5.0 that the hydrochloric acid soln of use 2.0mol/L is acidified to the pH value;
(5) the anolyte compartment that places the Bipolar Membrane device through pretreated seawater, wherein anode is the plate electrode that titanium is coated with platinum or titanium ruthenium, and current density is 400-1200A/m
2, the polar board surface flow velocity is 4-15cm/s;
Feeding mass concentration in the salt chamber of Bipolar Membrane device is the sodium chloride concentrated liquid of 1.0-10.0%; Acid chamber and alkali chamber feed tap water or pure water respectively; Make the mass concentration of acid reach 2-15% through circulation, the mass concentration of alkali reaches 2-18%, and crossflow velocity is 3-9cm/s;
(6) seawater through oxidation passes through above-mentioned spare resin layer in the Bipolar Membrane device, and the seawater after the oxidation is through resin layer, and when contacting with resin, free bromine is attracted on the resin, and the linear flow speed during seawater process resin is 1-20cm/s;
(7), utilize acid that the Bipolar Membrane device produces that the bromine of resin absorption is carried out wash-out with the above-mentioned resin that adsorbs free bromine; To be distilled and rectifying by the elutriant process that discharge the resin column bottom, and promptly obtain the finished product bromine, wherein the linear flow of wash-out speed is 2-20cm/s.
Beneficial effect: the present invention improves on the basis of traditional ion exchange resin system bromine technology; Utilizing at present, more advanced Bipolar Membrane technology is optimized putting forward the bromine process; Thereby the safety of having avoided causing owing to use chlorine is with problem of environment pollution caused, and the basic non-pollutant discharge of whole process can really be accomplished environmental requirement; And the purity of preparation is high, and is effective to the debrominate of seawater.
Description of drawings
Seawater is carried the process flow diagram of bromine among Fig. 1 the present invention
Bromine oxide in the Bipolar Membrane device produces the soda acid synoptic diagram simultaneously among Fig. 2 the present invention
Bipolar Membrane device bromine oxide and with the schematic flow sheet of resin absorption among Fig. 3 the present invention
Embodiment
Specify in the face of enforcement of the present invention down:
Pressing Fig. 1, Fig. 2, flowage structure shown in Figure 3, reach schematic diagram, is raw water with the seawater, and its bromine content is 130mg/L; Used resin is the D201 resin, and carries out pre-treatment before use: soak more than 24 hours with pure water, make it abundant swelling; Wash to water outlet limpidly then, use the 1.0mol/LNaOH solution soaking more than 2 hours again, washing is to neutral; Use 2.0mol/L HCI solution soaking more than 3 hours afterwards; Make resin fully transfer the Cl type to, be washed till pH2.0-3.0 with pure water at last, subsequent use;
Seawater is carried out pre-treatment: get a certain amount of raw water, first clarification filtration is used the H of 2.0mol/L then
2SO
4It is about 4.5 that solution is acidified to the pH value;
Through pretreated raw water, utilize the anolyte compartment of Bipolar Membrane device that bromine is carried out oxidation.Anode is that titanium is coated with the platinum plate electrode, and current density is 800A/m
2, the polar board surface flow velocity is 12cm/s;
When the anolyte compartment carried out oxidation to raw water, the salt chamber of Bipolar Membrane device fed 5.0% sodium chloride concentrated liquid, and sour chamber and alkali chamber feed tap water respectively, made acid concentration reach 10% through circulation, and alkali concn reaches 12%, and crossflow velocity is 7cm/s;
Raw water after the oxidation is through resin layer, and when contacting with resin, free bromine is attracted on the resin.Linear flow speed during absorption is 10cm/s;
After a certain amount of bromine of resin absorption, stop logical bittern.The acid that utilizes Bipolar Membrane to produce comes the resin of absorption bromine is carried out wash-out.Wash-out by discharge the resin column bottom is accomplished liquid through distillation and rectifying, promptly obtains the finished product bromine, and wash-out linear flow speed is 15cm/s.
After this put forward the bromine process, the bromine content of raw water was 12mg/L, extraction rate reached 91%.Bromine concentration after the drip washing is 4250mg/L.
Concentrated seawater with sea water desaltination is a raw water, and its bromine content is 230mg/L; Used resin is the D201 resin.The pretreatment process of resin and raw water is an example 1;
Through pretreated raw water, utilize the anolyte compartment of Bipolar Membrane device that bromine is carried out oxidation.Anode is that titanium is coated with the ruthenium plate electrode, and current density is 700A/m
2, the polar board surface flow velocity is 10cm/s;
When the anolyte compartment carried out oxidation to raw water, the salt chamber of Bipolar Membrane device fed 4.0% sodium chloride concentrated liquid, and sour chamber and alkali chamber feed tap water respectively, made acid concentration reach 12% through circulation, and alkali concn reaches 14%, and crossflow velocity is 7cm/s;
Raw water after the oxidation is through resin layer, and when contacting with resin, free bromine is attracted on the resin.Linear flow speed during absorption is 8cm/s;
After a certain amount of bromine of resin absorption, stop logical bittern.The acid that utilizes Bipolar Membrane to produce comes the resin of absorption bromine is carried out wash-out.Wash-out by discharge the resin column bottom is accomplished liquid through distillation and rectifying, promptly obtains the finished product bromine, and wash-out linear flow speed is 12cm/s.
After this put forward the bromine process, the bromine content of raw water was 21mg/L, extraction rate reached 92%.Bromine concentration after the drip washing is 6250mg/L.
With the subsurface brine is raw water, and its bromine content is 830mg/L; Used resin is the D201 resin.The pretreatment process of resin and raw water is an example 1;
With 2.0mol/L hydrochloric acid seawater is carried out pre-treatment,, utilize the anolyte compartment of Bipolar Membrane device that bromine is carried out oxidation through pretreated raw water.Anode is that titanium is coated with the ruthenium plate electrode, and current density is 1200A/m
2, the polar board surface flow velocity is 6cm/s;
When the anolyte compartment carried out oxidation to raw water, the salt chamber of Bipolar Membrane device fed 6.0% sodium chloride concentrated liquid, and sour chamber and alkali chamber feed tap water respectively, made acid concentration reach 15% through circulation, and alkali concn reaches 18%, and crossflow velocity is 9cm/s;
Raw water after the oxidation is through resin layer, and when contacting with resin, free bromine is attracted on the resin.Linear flow speed during absorption is 6cm/s;
After a certain amount of bromine of resin absorption, stop logical bittern.The acid that utilizes Bipolar Membrane to produce comes the resin of absorption bromine is carried out wash-out.Wash-out by discharge the resin column bottom is accomplished liquid through distillation and rectifying, promptly obtains the finished product bromine, and wash-out linear flow speed is 15cm/s.
After this put forward the bromine process, the bromine content of raw water was 43mg/L, extraction rate reached 95%.Bromine concentration after the drip washing is 15530mg/L.
Claims (1)
1. a method of utilizing Bipolar Membrane from seawater, to carry bromine is characterized in that comprising the steps:
(1) with pure water macroporous strong basic anionite-exchange resin was soaked more than 24 hours, wash to water outlet limpid then;
(2) soak above-mentioned resin more than 2 hours with 1.0mol/LNaOH solution, washing is to neutral again;
(3) more than 3 hours, use pure water subsequent use to pH2.0-3.0 with the above-mentioned resin of 2.0mol/LHCI solution soaking again resin wash;
(4) carry out clarification filtration to seawater, it is 4.0～5.0 that the hydrochloric acid soln of use 2.0mol/L is acidified to the pH value;
(5) the anolyte compartment that places the Bipolar Membrane device through pretreated seawater, wherein anode is the plate electrode that titanium is coated with platinum or titanium ruthenium, and current density is 400-1200A/m
2, the polar board surface flow velocity is 4-15cm/s;
Feeding mass concentration in the salt chamber of Bipolar Membrane device is the sodium chloride concentrated liquid of 1.0-10.0%; Acid chamber and alkali chamber feed tap water or pure water respectively; Make the mass concentration of acid reach 2-15% through circulation, the mass concentration of alkali reaches 2-18%, and crossflow velocity is 3-9cm/s;
(6) seawater through oxidation passes through above-mentioned spare resin layer in the Bipolar Membrane device, and the linear flow speed during seawater process resin is 1-20cm/s;
(7), utilize acid that the Bipolar Membrane device produces that the bromine of resin absorption is carried out wash-out with the above-mentioned resin that adsorbs free bromine; To be distilled and rectifying by the elutriant process that discharge the resin column bottom, and promptly obtain the finished product bromine, wherein the linear flow of wash-out speed is 2-20cm/s.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102556972A (en) * | 2012-02-10 | 2012-07-11 | 淮北师范大学 | Method for extracting bromine by industrial wastewater rich in Br- |
| CN104176871A (en) * | 2014-09-04 | 2014-12-03 | 北京赛科康仑环保科技有限公司 | Recovery treatment method of acidic etching waste liquor |
| CN114875428A (en) * | 2022-06-15 | 2022-08-09 | 华东理工大学 | Method for extracting bromine and producing sodium bromide from potassium-extracting old bittern |
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| RU2007128380A (en) * | 2007-07-23 | 2009-01-27 | Институт химии и химической технологии СО РАН (ИХХТ СО РАН) (RU) | METHOD FOR EXTRACTION OF BROMINE FROM NATURAL CHLORIDE WATERS WITH PRODUCTION OF BROMIDE CONCENTRATE |
| CN101880028A (en) * | 2010-07-16 | 2010-11-10 | 国家海洋局天津海水淡化与综合利用研究所 | Method for extracting bromine from brine |
| CN102049195A (en) * | 2009-10-30 | 2011-05-11 | 中国石油化工股份有限公司 | Ion exchange method for solid substance containing exchangeable ions |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2007128380A (en) * | 2007-07-23 | 2009-01-27 | Институт химии и химической технологии СО РАН (ИХХТ СО РАН) (RU) | METHOD FOR EXTRACTION OF BROMINE FROM NATURAL CHLORIDE WATERS WITH PRODUCTION OF BROMIDE CONCENTRATE |
| CN102049195A (en) * | 2009-10-30 | 2011-05-11 | 中国石油化工股份有限公司 | Ion exchange method for solid substance containing exchangeable ions |
| CN101880028A (en) * | 2010-07-16 | 2010-11-10 | 国家海洋局天津海水淡化与综合利用研究所 | Method for extracting bromine from brine |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102556972A (en) * | 2012-02-10 | 2012-07-11 | 淮北师范大学 | Method for extracting bromine by industrial wastewater rich in Br- |
| CN104176871A (en) * | 2014-09-04 | 2014-12-03 | 北京赛科康仑环保科技有限公司 | Recovery treatment method of acidic etching waste liquor |
| CN104176871B (en) * | 2014-09-04 | 2016-05-18 | 北京赛科康仑环保科技有限公司 | A kind of recycling processing method for acidic etching waste liquid |
| CN114875428A (en) * | 2022-06-15 | 2022-08-09 | 华东理工大学 | Method for extracting bromine and producing sodium bromide from potassium-extracting old bittern |
| CN114875428B (en) * | 2022-06-15 | 2024-01-30 | 华东理工大学 | Method for extracting bromine from potassium-extracted old brine and producing sodium bromide |
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