CN1108616A - Control method for synthesis process of directly preparing lithium bromide - Google Patents
Control method for synthesis process of directly preparing lithium bromide Download PDFInfo
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- CN1108616A CN1108616A CN 94111269 CN94111269A CN1108616A CN 1108616 A CN1108616 A CN 1108616A CN 94111269 CN94111269 CN 94111269 CN 94111269 A CN94111269 A CN 94111269A CN 1108616 A CN1108616 A CN 1108616A
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- Prior art keywords
- lithium bromide
- reaction
- lithiumbromide
- ammonium
- liquid
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- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000008569 process Effects 0.000 title claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 title abstract description 6
- 238000003786 synthesis reaction Methods 0.000 title abstract description 6
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 11
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 229940059936 lithium bromide Drugs 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 230000002829 reductive effect Effects 0.000 claims description 11
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 34
- 239000002994 raw material Substances 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000033116 oxidation-reduction process Effects 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 5
- 239000007787 solid 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
- 239000000047 product Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 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
- 229910052794 bromium Inorganic materials 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000000463 material Substances 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
- 239000002826 coolant Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- IPLONMMJNGTUAI-UHFFFAOYSA-M lithium;bromide;hydrate Chemical compound [Li+].O.[Br-] IPLONMMJNGTUAI-UHFFFAOYSA-M 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 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
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 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
- 125000001246 bromo group Chemical class Br* 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000835 fiber 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
- 230000001939 inductive effect Effects 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
- 238000002156 mixing Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 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
- 238000004886 process control Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- -1 silt filters out Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 230000002557 soporific effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 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
- 230000009466 transformation Effects 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A control method for a synthesis process of lithium bromide prepared by a direct method relates to the technical field of preparation of lithium bromide. When liquid bromine, lithium carbonate and reducing agent containing ammonium are used for direct oxidation-reduction synthesis to prepare lithium bromide, the two-step synthesis method is adopted, namely, quantitative ammonium, reducing agent and liquid bromine are firstly used for pre-reaction, and then, the rest raw materials are gradually added under the condition of stirring to prepare qualified lithium bromide solution. The invention can shorten the reaction time, reduce the energy consumption, improve the production capacity and is suitable for using NH4OH、(NH4)2CO3、CO(NH4)2、NH3、NH4HCO3And controlling the synthesis process of preparing the lithium bromide by directly oxidizing and reducing the ammonium-containing compound or the mixture, the liquid bromine and the lithium carbonate.
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:
Suspension is at first made with Quilonum Retard when synthetic by this institute, adds reductive agent, and under continuous stirring state, add the liquid bromine and making by certain speed, filtering separation then, reaction solution promptly gets solid crystal LiBr product through evaporation concentration after crystallisation by cooling, separation, the drying.
Can find out that from chemical equation (1) in the lithiumbromide synthetic reaction process, the lithiumbromide of a mole of every generation just will generate 1/2 mole CO
2Nitrogen with 1/6 mole.Simultaneously, know a certain chemical reaction of process in the middle of it, its reaction equilibrium constant K=e from thermodynamics of reactions calculating
231, almost be infinitely great.In other words, this reaction is carried out very soon, and is very complete.The lithiumbromide of a fast like this mole of every generation is the CO of about 15 liters of corresponding generation
2And N
2Gas, because reaction is carried out very fiercely, the volume of reaction mass has increased many, often causes flash easily, and material is incurred loss, or improper because of controlling, and causes other danger.Also often, flash carries out not exclusively because of making reaction.
The present invention (contains NH with Quilonum Retard, liquid bromine and ammonia, ammonium salt reductive agent
+
4Ionic NH
4OH, (NH
4)
2CO
3, CO(NH
2)
2, NH
3, NH
4HCO
3Deng ammoniation all can) produce the method for lithium-bromide solution and lithiumbromide crystalline solid for raw material.
The present invention's purpose is exactly the defective that will overcome above-mentioned existence, control synthesising reacting speed and process.Controlling this synthesising reacting speed method has usually: (1) control reaction temperature; (2) rate of feeding of a kind of or two kinds of materials of control; (3) a certain material is repeatedly dropped into.Though more than three kinds of control methods played certain control action kou, prolonged the reaction times.For this reason, the technology of the present invention key is to have taked to divide for two steps finished chemical equation (1) in same reaction vessel, promptly produces pre-synthetic liquid earlier, is then obtained the synthetic method of lithiumbromide again with remaining raw material reaction by pre-synthetic liquid.Like this, entire reaction was both quick, and was steady again, and easy to control, and made whole synthesising reacting time almost shorten half.
Technical scheme of the present invention is to divide for two steps carried out direct synthetic reaction process, promptly earlier with an amount of ammonium reductive agent NH that contains as calculated
4OH, (NH
4)
2CO
3, CO(NH
4)
2, NH
3, NH
4HCO
3Deng in the compound a kind of or they mixture and the liquid bromine stir and normal temperature under in reactor, carry out pre-reaction, generation contains NH
4The pre-synthetic liquid of Br, progressively quantitative again constant speed adds remaining raw material such as Li under stirring state then
2CO
3Deng, make qualified LiBr solution.
Technical process block diagram of the present invention as shown in Figure 1.
The structural representation of Fig. 1-middle synthesizer is shown in figure two.
Fig. 1-in, in synthesizer, the LiBr solution that makes 35% qualified left and right sides concentration with 2 footworks is sent into first filtration unit, will remain Li
2CO
3, after solid impurity such as silt filters out, solution is sent into first concentrating unit and is concentrated to 50% left and right sides LiBr solution, solution is sent into refining plant then, removes NH in the solution
+
4Impurity etc. enter second filtration unit then, remove Ca
+, Mg
+, Ba
+Plasma makes and contains the qualified solution of LiBr concentration about 50%.This solution can be sold (as making cooling agent) with liquid LiBr product can.Also can further enter second concentrating unit, the Crystallization Separation device makes qualified LiBr crystalline solid product, as two water lithiumbromide crystal.
Synthesizer concrete structure synoptic diagram is shown in figure two, in Fig. 2 among Fig. 1: the 1-feed hopper; The 2-whipping appts; 3-container (as beaker); The 4-thermometer; 5-synthesizes liquid.
The present invention notices: (1) this chemical reaction is to carry out under the situation of solid, liquid, gas three-phase coexistence; (2) because speed of response is fast, power is big, and chemical reaction does not have inductive phase substantially, can be in normal temperature or more reaction rapidly under the low temperature; (3) in the reaction process along with the increase of viscosity of sludge, the CO that reaction generates
2, N
2It is very strong that gas is made the bubble effect; (4) the useful volume utilization coefficient of reaction vessel is very low; (5) how to make building-up reactions carry out not only rapidly but also steady, and easy to operate, want product yield height simultaneously, starting material transformation efficiency height is that redox control is crucial in the building-up process.In view of big, insensitive with the method controls reaction speed energy consumption of cooling water temperature; With the quantitative liquid feeding bromine, add the way controls reaction speed of reductive agent, though sensitive, the reaction times has prolonged many relatively, and needs metering accurately, if make mistakes slightly, react just uncontrollable, the reaction feed liquid is increased sharply, and just can cause flash or other danger.Therefore, the present invention has abandoned conventional control method, but certain intermediate reaction of decision synthesising reacting speed is carried out separately in advance, promptly the first step earlier quantitatively adds industrial liquid bromine or industrial ammonia and ammoniated compound through funnel 1 and makes reductive agent in same reaction vessel 3, stirs generation NH
4The synthetic in advance liquid of Br, second step was utilized above-mentioned pre-synthetic liquid and remaining raw material such as industrial Li again
2CO
3Reaction, promptly under whipping appts 2 stirred, quantitatively constant speed added Li
2CO
3Powder continues the LiBr solution that reaction obtains 35% qualified left and right sides concentration.Send into next step first filtration unit filtering and impurity removing, thereby realized that speed of response is fast, and steadily, easy to control, and the reaction times is than having shortened half with conventional control method.
Embodiment: adopt building-up reactions two step method of the present invention and with domestic certain institute with two kinds of methods of building-up reactions method, measure 212 milliliters of industrial liquid bromines, 208 milliliters of industrial ammonias and industrial lithium carbonate 308 grams respectively, carry out building-up reactions, reaction result: control with the inventive method, the building-up reactions method control of only spending 60 minutes and using with domestic certain institute has been spent 120～150 minutes.
Characteristics of the present invention:
1, energy consumption is low, and the building-up process energy consumption is reduced to original about 50%.
2, technological process speed is fast, steadily, and is easy to control, the used time only be originally half.
3, do not increasing under any investment situation, can improve nearly one times of synthesis capability.
4, do not increase schedule of operation.
5, economical rationality does not increase any investment.
The present invention is applicable to and uses NH
4OH, (NH
4)
2CO
3, CO(NH
4)
2, NH
3, NH
4HCO
3Produce the lithiumbromide process control Deng ammonium-containing compound and their mixture and bromine and Quilonum Retard direct oxidation reduction.
Claims (2)
1, a kind of direct method is produced the control method of lithiumbromide building-up process, it is characterized in that the lithiumbromide building-up process divide two the step carry out, at first will quantitatively contain the reductive agent of ammonium and liquid bromine stirs at normal temperatures and reacts, generation contains the pre-synthetic liquid of brometo de amonio, under stirring state, add quantitative Quilonum Retard pressed powder and make qualified lithium-bromide solution then.
2, method according to claim 1, the reductive agent that it is characterized in that containing ammonium are the liquid of a kind of in ammonia, ammoniacal liquor, volatile salt, bicarbonate of ammonia, the urea or their mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94111269A CN1041402C (en) | 1994-03-16 | 1994-03-16 | Control method for synthesis process of directly preparing lithium bromide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94111269A CN1041402C (en) | 1994-03-16 | 1994-03-16 | Control method for synthesis process of directly preparing lithium bromide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1108616A true CN1108616A (en) | 1995-09-20 |
| CN1041402C CN1041402C (en) | 1998-12-30 |
Family
ID=5035157
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94111269A Expired - Fee Related CN1041402C (en) | 1994-03-16 | 1994-03-16 | Control method for synthesis process of directly preparing lithium bromide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1041402C (en) |
Family Cites Families (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 CN94111269A patent/CN1041402C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1041402C (en) | 1998-12-30 |
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