CN1041403C - Purification process for directly preparing lithium bromide - Google Patents
Purification process for directly preparing lithium bromide Download PDFInfo
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- CN1041403C CN1041403C CN94111270A CN94111270A CN1041403C CN 1041403 C CN1041403 C CN 1041403C CN 94111270 A CN94111270 A CN 94111270A CN 94111270 A CN94111270 A CN 94111270A CN 1041403 C CN1041403 C CN 1041403C
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- Prior art keywords
- lithium bromide
- solution
- lithium
- libr
- lithiumbromide
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- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 title claims abstract description 118
- 238000000746 purification Methods 0.000 title abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 229940059936 lithium bromide Drugs 0.000 claims description 23
- 239000012141 concentrate Substances 0.000 claims description 6
- 230000002829 reductive effect Effects 0.000 claims description 5
- 230000002000 scavenging effect Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 1
- 229910052788 barium Inorganic materials 0.000 claims 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 229910052749 magnesium Inorganic materials 0.000 claims 1
- 239000011777 magnesium Substances 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 14
- 239000007787 solid Substances 0.000 abstract description 8
- 238000001914 filtration Methods 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052736 halogen Inorganic materials 0.000 abstract description 4
- 150000002367 halogens Chemical class 0.000 abstract description 4
- 238000006386 neutralization reaction Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract description 3
- 239000007800 oxidant agent Substances 0.000 abstract description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract 1
- 230000033116 oxidation-reduction process Effects 0.000 abstract 1
- 150000002926 oxygen Chemical class 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000002826 coolant Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000031709 bromination Effects 0.000 description 1
- 238000005893 bromination reaction Methods 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- IPLONMMJNGTUAI-UHFFFAOYSA-M lithium;bromide;hydrate Chemical compound [Li+].O.[Br-] IPLONMMJNGTUAI-UHFFFAOYSA-M 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000002557 soporific effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229940125725 tranquilizer Drugs 0.000 description 1
- 239000003204 tranquilizing agent Substances 0.000 description 1
- 230000002936 tranquilizing effect Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Removal Of Specific Substances (AREA)
Abstract
A purification process method for preparing lithium bromide by a direct method relates to the technical field of preparation of lithium bromide. When liquid bromine, lithium carbonate and ammonia water are used for preparing lithium bromide by direct oxidation-reduction synthesis, the impurities in the solution after the synthesis reaction are many, except for the common filtering method, the key point of the invention is to add a purification process, namely, using halogen elements or oxygen acids or salts of the halogen elements and other oxidants to remove NH which is extremely difficult to remove in the solution4 +And the like. The invention can simultaneously obtain two products of liquid lithium bromide and solid lithium bromide which meet the product quality standard, has low energy consumption and removes NH4 +High efficiency, simple process, short time and low cost. The method is suitable for the occasions that the product quality is influenced due to the pollution of ammonia in the process of preparing the lithium bromide by a direct synthesis method or a neutralization method.
Description
The invention belongs to inorganic chemistry, basic metal class, relate to the bromide preparing technical field of lithium.
The lithiumbromide molecular formula is LiBr, and molecular weight is 86.845, and density (25 ℃) is 3464Kg/m
3, 547 ℃ of fusing points, 1265 ℃ of boiling points.Anhydrous lithium bromide be white in color cubic system or granular powder, nontoxic nothing is smelt, and salty bitter taste is arranged, deliquescence very easily, soluble in water, ethanol and ether dissolve in the organic solvents such as methyl alcohol, acetone, ethylene glycol.According to different crystallization conditions, lithiumbromide can form a water lithiumbromide, two water lithiumbromides, three water lithiumbromides and composition thereof respectively with water.
Lithiumbromide is a kind of efficient water vapor absorption agent and air humidity conditioning agent, and the absorption agent that the lithiumbromide mixing solutions of 50～55% concentration is used as refrigerator is a cooling agent.In organic chemistry, lithiumbromide is as removing hydrogen chloride agent, the swelling agent of organic fibre (as wool, hair).In medicine industry, be used as soporific and tranquilizer, also can be used for the ionogen and the chemical reagent of some advanced battery (as lithium cell).
The preparation of lithiumbromide is according to " Lithium Products March " (production method of lithium compound) magazine report in 1992, and abroad, industrial lithiumbromide mainly is to use neutralisation, promptly uses in the HBr acid and LiOH, Li
2CO
3Obtain.At home, the main method of producing LiBr is still based on above-mentioned neutralisation, and also having with iron filings, bromine, Quilonum Retard is the bromination iron processes report of feedstock production lithiumbromide, but above-mentioned two methods cost an arm and a leg.But occurred the redox direct synthesis technique in the recent period, useful urea is made reductive agent; Useful hydrogen peroxide (Urumchi, Xinjiang lithium salts institute) is made reductive agent; Also useful ammonia and compound (Qinghai Yanhu Inst., Chinese Academy of Sciences) thereof are made reductive agent.
Qinghai Yanhu Inst., Chinese Academy of Sciences had once finished " lithiumbromide new preparation process research (small test research report) " and " the lithiumbromide new preparation process is studied (expanding test report) " respectively in 1987 and 1991, be to be that raw material is produced lithiumbromide crystalline solid method with Quilonum Retard, liquid bromine and ammoniacal liquor.Having built up the expansion trial assembly puts.
Its chemical reaction general equation formula is:
………(1)
Its technical process is:
Use Br
2, Li
2CO
3, NH
4After the OH building-up reactions makes the synthetic liquid of LiBr, the filtering separation removal of impurities, synthetic then liquid is through evaporation concentration, and crystallisation by cooling separates drying and makes LiBr solid crystal product.
From above-mentioned chemical reaction general equation formula (1) as can be known, in the lithiumbromide building-up reactions at the end, during forming, synthetic liquid, a spot of Li is arranged still except based on the LiBr
2CO
3With the Rr that is dissolved in the solution
2, NH
4 +, CO
2, HCO
3 -, Ca
+, Mg
+, Ba
+And the silt foreign material etc., for reaching standard compliant qualified LiBr product, must remove above-mentioned foreign material.
The present invention's purpose has been set up a scavenging process in order to remove foreign material in the above-mentioned solution exactly, adopt twice filtration, twice concentration technology, primary purification, simultaneously, because foreign material are removed, can not only produce qualified LiBr crystalline solid product, and can direct production go out the qualified liquid product that contains 50% left and right sides LiBr.
Technical process block diagram of the present invention is shown in figure one.
In the drawings, at synthesis procedure Br2、Li
2CO
3, the reducing agent synthetic reaction that the contains ammonium synthetic liquid that makes 35%LiBr sends into the first filter progress removal of impurities, then enter the first enrichment process solution is concentrated into LiBr to 50% left and right sides concentration, then enter the further removal of contamination of cleaning procedure, and then enter the second filter progress and filter to get the qualifying liquid of 50% left and right sides LiBr, this liquid can directly be done export trade after the product can, also can enter successively the second enrichment process, Crystallization Procedure, separation circuit again and obtain qualified solid LiBr crystalline product.
Technical scheme of the present invention is to adopt secondary filtration, secondary concentration, primary purification technology, and each process in the CONTROL PROCESS flow process, various impurity is disposed, that is: respectively
1, removes by filter remaining Li in the synthetic liquid first time behind end of synthesis
2CO
3, solid matter such as silt foreign material.
2, in first time concentration process, utilize heating and vacuumize, remove the CO in the LiBr solution
2
3, in scavenging process, mainly adopt oxygenant to remove NH in the LiBr solution
4 +Ion, NH before and after it is removed
4 +Concentration is respectively 1500ppm and below the 10ppm.
4, in second time filtration procedure, remove by Li
2CO
3The Ca that brings in the solid
+, Mg
+, Ba
+Plasma.
Key problem in technology of the present invention is to remove NH in the LiBr solution in scavenging process
4 +Ion.NH
4 +Ion exists in LiBr cooling agent, and evaporating in refrigeration processes influences works better; NH
4 +Ion exists in the LiBr solid crystal also influences quality product.Therefore, must remove.And NH
4 +Ion is not easy to remove, because NH
3Mineral compound all are soluble substances, remove NH with generating sedimentary method in other words
4 +Be not all right, though so with physical method promptly heat, concentrate, the crystalline method is feasible, need to concentrate repeatedly.And concentrate repeatedly, crystallization, separation, dissolving, concentrate, recrystallize, energy expenditure be too big, uneconomical, unreliable, particularly for the occasion of making cooling agent with 50%LiBr concentration solution, LiBr crystalline solid can only be dissolved in the past again and made.Extremely uneconomical economically.For this reason, key problem in technology of the present invention is that the LiBr solution of 50% concentration after concentrating first is cooled to below 80 ℃, under stirring state, adds quantitative oxygenant, promptly adds the salt of the oxygen acid of the oxygen acid of haloid element or haloid element or haloid element.The amount that adds is according to NH in the LiBr solution
4 +Concentration comes to determine as calculated, is generally 3/1000ths～four of pending LiBr solution gross weight.By the NH in the product after the purifying treatment
4 +Ion content can reach ammonia (NH in the lithiumbromide target level of product quality
4) % is less than or equal to 0.001 index, i.e. NH in the LiBr solution
4 +Concentration is lower than 16.7ppm.
The embodiment of the invention: the haloid element add 3/1000ths to four in first filtration, the first spissated 50%LiBr of the containing solution after stirring, draws as table one and removes NH
4 +Data.Table one
| Test piece number (Test pc No.) | Ammonium concentration ppm in the solution before purifying | Purify ammonium concentration ppm in the solution of |
| 1 # 2 # 3 # | 1430 1000 850 | 8.7 3.1 10.0 |
Characteristics of the present invention are:
1, energy resource consumption is low, need only with the waste heat of concentrate, just can satisfy halogen and oxidant and the NH such as halogen family oxyacid and salt4 +Reaction condition, need not add heat.
2, technical process time weak point, the purification time only is 10～15 minutes.
3, except NH4 +Efficient is high, can make NH4 +Concentration is down to below the 10ppm from 1500ppm.
4, cost is low, because used oxidant content only is 3/1000ths～four of the LiBr solution total amount that purifies.
5, use the inventive method, product is not only LiBr crystalline solid product, also 50%LiBr fluid product.
6, so overall economic efficiency of the present invention is more much higher than adopting the repeated crystallization purification method, because adopt repeated crystallization to purify NH4 +Energy consumption is high, and process cycle is long, except NH4 +Efficient is subjected to NH4 +Concentration affects is large, such as primary crystallization, and NH in the product4 +Concentration 〉=50ppm then must repeat crystallization.
The present invention is applicable to: (1) direct method is synthesized in the lithiumbromide process because of having added NH
3, NH
4OH, (NH
4)
2CO
3, NH
4HCO
3, CO (NH
2)
2, NH
4Br, (NH
4)
2SO
4, NH
4 +Reductive agents such as Cl and NH in the lithium-bromide solution that causes
4 +Concentration is higher, required purifying treatment of carrying out.(2) lithium-bromide solution of neutralisation production need carry out purifying treatment because of the pollution of ammonia.Be specially adapted to produce liquid LiBr and be used to do the cooling agent occasion.
Claims (1)
1, a kind of direct method is produced the technological process for purifying of lithiumbromide, it is characterized in that it comprises following successively technological process: filter for the first time, remove impurity such as remaining lithiumbromide, silt in the synthetic liquid; Concentrate, in heating with vacuumize under the condition and lithium-bromide solution to be concentrated to 50% concentration; Scavenging process is cooled to lithium-bromide solution below 80 ℃, adds the haloid element oxygenant of pending lithium-bromide solution gross weight thousand molecules three to thousand molecules four under stirring state, makes NH in the solution
4 +Ionic concn is reduced to below the 10ppm by the 1500ppm before removing; Filter for the second time, remove calcium, magnesium, barium plasma in the solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94111270A CN1041403C (en) | 1994-03-16 | 1994-03-16 | Purification process for directly preparing lithium bromide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94111270A CN1041403C (en) | 1994-03-16 | 1994-03-16 | Purification process for directly preparing lithium bromide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1108617A CN1108617A (en) | 1995-09-20 |
| CN1041403C true CN1041403C (en) | 1998-12-30 |
Family
ID=5035158
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94111270A Expired - Fee Related CN1041403C (en) | 1994-03-16 | 1994-03-16 | Purification process for directly preparing lithium bromide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1041403C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553085A (en) * | 2013-09-28 | 2014-02-05 | 昆山市周市溴化锂溶液厂 | Method for eliminating calcium and magnesium ions in lithium bromide solution |
| CN103508471A (en) * | 2013-09-28 | 2014-01-15 | 昆山市周市溴化锂溶液厂 | Method for refining anhydrous lithium bromide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1038282A1 (en) * | 1980-05-22 | 1983-08-30 | Matyushenko Evgeniya | Process for producing lithium bromide |
-
1994
- 1994-03-16 CN CN94111270A patent/CN1041403C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1038282A1 (en) * | 1980-05-22 | 1983-08-30 | Matyushenko Evgeniya | Process for producing lithium bromide |
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| Publication number | Publication date |
|---|---|
| CN1108617A (en) | 1995-09-20 |
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