CN102139897A - Method for removing bromine impurities from alkali metal or alkali earth metal chloride - Google Patents
Method for removing bromine impurities from alkali metal or alkali earth metal chloride Download PDFInfo
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- CN102139897A CN102139897A CN 201110046219 CN201110046219A CN102139897A CN 102139897 A CN102139897 A CN 102139897A CN 201110046219 CN201110046219 CN 201110046219 CN 201110046219 A CN201110046219 A CN 201110046219A CN 102139897 A CN102139897 A CN 102139897A
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- Prior art keywords
- chloride
- earth metal
- alkali
- alkaline earth
- metal
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- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 title claims abstract description 20
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052794 bromium Inorganic materials 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000012535 impurity Substances 0.000 title claims abstract description 12
- 229910052783 alkali metal Inorganic materials 0.000 title claims abstract description 8
- 150000001340 alkali metals Chemical class 0.000 title claims abstract description 8
- 229910052784 alkaline earth metal Inorganic materials 0.000 title claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 20
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims abstract description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 13
- 229910001617 alkaline earth metal chloride Inorganic materials 0.000 claims description 13
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 11
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical group [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 10
- 229910052728 basic metal Inorganic materials 0.000 claims description 10
- 150000003818 basic metals Chemical class 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 5
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims description 4
- 230000003750 conditioning effect Effects 0.000 claims description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical group [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 4
- -1 alkaline earth metal chlorate Chemical class 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 2
- 229910001626 barium chloride Inorganic materials 0.000 claims description 2
- 229940045511 barium chloride Drugs 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 2
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000010992 reflux Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000012286 potassium permanganate Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- 241000024287 Areas Species 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000002934 diuretic Substances 0.000 description 1
- 230000001882 diuretic effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WALYXZANOBBHCI-UHFFFAOYSA-K magnesium sodium trichloride hydrate Chemical compound O.[Cl-].[Na+].[Mg+2].[Cl-].[Cl-] WALYXZANOBBHCI-UHFFFAOYSA-K 0.000 description 1
- NNNSKJSUQWKSAM-UHFFFAOYSA-L magnesium;dichlorate Chemical compound [Mg+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O NNNSKJSUQWKSAM-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for rapidly removing bromine impurities from alkali metal or alkali earth metal chloride. The method disclosed by the invention comprises the following steps of: firstly, dissolving alkali metal or alkali earth metal chloride into water to form an aqueous solution, adding hydrochloric acid to adjust the pH value of the solution to be 2.5 to 5.5, and adding corresponding alkali metal or alkali earth metal chlorate or perchlorate; secondly, heating to boil and reflux for 1-5 hours, condensing and crystallizing to obtain alkali metal or alkali earth metal chloride products. The content of the bromide in industrial alkali metal or alkali earth metal is reduced from 0.1% to below 5 ppm and no new impurities are introduced to the system.
Description
Technical field
The present invention relates to the method for purification of material, specifically is a kind of method of removing bromide impurity from alkali metal chloride.
Background technology
Alkali metal chloride such as Repone K or sodium-chlor have purposes widely in a lot of fields as the staple product of salt chemical engineering industry.Industrial, Repone K, sodium-chlor are mainly used in produces other Chemicals, as the oxyhydroxide of potassium, sodium, carbonate, oxymuriate, hypochlorite etc., also is widely used in petroleum industry, rubber industry and electroplating industry.On medical and health, Repone K, sodium-chlor are that medicine is regulated in clinical electrolyte balance commonly used, also can be used as diuretic(s), for the salt agent.
But in many Application Areass, the bromide foreign matter content in Repone K, the sodium-chlor is excessive, is a bigger restriction to the quality of product.Effective elimination bromide impurity is one of key of restriction China industrial potassium chloride, sodium-chlor quality from Repone K, sodium-chlor.
To removing the technology of bromine in the muriate, document (Li Fenglan, the discussion that medicinal Repone K is removed bromine technology are arranged, sea lake salt and chemical industry) report, in acidic solution, utilize potassium permanganate to make oxygenant bromide is oxidized to bromine simple substance, heating makes bromine simple substance be the gaseous state effusion then.Though this method can obtain certain bromine effect of removing, after having reacted, potassium permanganate is reduced into Mn
2+, combine formation Mn (OH) with the KOH that adds
2Precipitation needs to increase a step filter operation and just can remove, and has increased the loaded down with trivial details property of technological process.And, also can introduce new impurity if the potassium permanganate that adds is excessive slightly.
Patent DE-2118623A has described a kind of bromine method of removing of magnesium chloride brine, and this method is to feed the content that chlorine reduces bromide in solution.DE-261328A has described a kind of preparation method of high density chlorination magnesium solution, and the debrominate method of document record is also undertaken by chlorine.But for the purpose of safety, using chlorine to remove bromine has very big restrictedly, and corresponding method and experimental program also have very high requirement to equipment.
Summary of the invention
The object of the present invention is to provide a kind of method of from basic metal or alkaline earth metal chloride, removing bromide fast.
The water-soluble formation aqueous solution of basic metal of the present invention or alkaline earth metal chloride, add hydrochloric acid conditioning solution pH value to 2.5 ~ 5.5, add corresponding alkali metal or alkaline earth metal chlorate or perchlorate, heated and boiled refluxed 1 ~ 5 hour, the reconcentration crystallization obtains basic metal or alkaline earth metal chloride product.
Among the present invention, alkali metal chloride can be lithium chloride, sodium-chlor or Repone K, and alkaline earth metal chloride can be magnesium chloride, calcium chloride, strontium chloride or bariumchloride.
The pH value preferable range of hydrochloric acid conditioning solution is 2.5 ~ 3.
The present invention can be in basic metal or alkaline earth metal chloride purification Production Flow Chart, increase the present invention and remove bromine technology, perhaps change original bromine technology of removing, realize fast, simply and effectively removing the bromine effect, bromide content in industrial soda metal or the alkaline earth metal chloride is dropped to below the 5ppm from 0.1%, and in system, do not introduce new impurity.
Embodiment
Embodiment 1.
Get 400 g bromide content and be 0.1% Repone K raw material, be dissolved in the 700 mL pure water, stir down heated and boiled to dissolving fully.
In above-mentioned solution, add weight content 30% hydrochloric acid, transfer to pH value of solution value=2.5 ~ 3.
Add 0.5 g Potcrate, heated and boiled 2 hours.During this time, constantly monitor the pH value of solution value,, then add appropriate hydrochloric acid, make the pH value of solution value maintain 2.5 ~ 3 if the pH value is higher than 3.
After removing bromine and finishing, with the solution concentration crystallization, centrifuge dripping, the Repone K product after dry must the purification.
The Repone K product sampling and detecting, bromide content is reduced to 3ppm as a result.
Embodiment 2.
Get 400 g bromide content and be 0.1% sodium-chlor raw material and be dissolved in the 700 mL pure water, stir down heated and boiled to dissolving fully.
In above-mentioned solution, add weight content 30% hydrochloric acid, transfer to pH value=2.5 ~ 3.
Add 0.5 g sodium perchlorate, heated and boiled 2 hours.During this time, constantly monitor the pH value of solution value,, then add appropriate hydrochloric acid, make the pH value of solution value maintain 2.5 ~ 3 if the pH value is higher than 3.
After removing bromine and finishing, with the solution concentration crystallization, centrifuge dripping, the sodium-chlor product after dry must the purification.
The sodium-chlor product sampling and detecting, bromide content is reduced to 4ppm as a result.
Embodiment 3.
Get 400 g bromide content and be 0.1% magnesium chloride raw material and be dissolved in the 700 mL pure water, stir down heated and boiled to dissolving fully.
In above-mentioned solution, add weight content 30% hydrochloric acid, transfer to pH value=2.5 ~ 3.
Add 0.5 g magnesium chlorate, heated and boiled 2 hours.During this time, constantly monitor the pH value of solution value,, then add appropriate hydrochloric acid, make the pH value of solution value maintain 2.5 ~ 3 if the pH value is higher than 3.
After removing bromine and finishing, with the solution concentration crystallization, centrifuge dripping, the magnesium chloride product after dry must the purification.
The magnesium chloride product inspection by sampling, bromide content is reduced to 2ppm as a result.
Claims (4)
1. the method for removing bromine impurity in basic metal or the alkaline earth metal chloride, it is characterized in that: with the basic metal or the water-soluble formation aqueous solution of alkaline earth metal chloride, add hydrochloric acid conditioning solution pH value to 2.5 ~ 5.5, add corresponding alkali metal or alkaline earth metal chlorate or perchlorate, heated and boiled 1 ~ 5 hour, the reconcentration crystallization obtains chloride product.
2. according to the method for removing bromine impurity in described basic metal of claim 1 or the alkaline earth metal chloride, it is characterized in that described alkali metal chloride is lithium chloride, sodium-chlor or Repone K.
3. according to the method for removing bromine impurity in described basic metal of claim 1 or the alkaline earth metal chloride, it is characterized in that described alkaline earth metal chloride is magnesium chloride, calcium chloride, strontium chloride or bariumchloride.
4. according to the method for removing bromine impurity in described basic metal of claim 1 or the alkaline earth metal chloride, it is characterized in that described hydrochloric acid conditioning solution pH value to 2.5 ~ 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110046219 CN102139897A (en) | 2011-02-26 | 2011-02-26 | Method for removing bromine impurities from alkali metal or alkali earth metal chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110046219 CN102139897A (en) | 2011-02-26 | 2011-02-26 | Method for removing bromine impurities from alkali metal or alkali earth metal chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102139897A true CN102139897A (en) | 2011-08-03 |
Family
ID=44407721
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110046219 Pending CN102139897A (en) | 2011-02-26 | 2011-02-26 | Method for removing bromine impurities from alkali metal or alkali earth metal chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102139897A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3174828A (en) * | 1960-08-31 | 1965-03-23 | Du Pont | Sorption of bromine on anion exchange resins in the presence of excess chlorine |
| JPS5730944A (en) * | 1980-07-31 | 1982-02-19 | Sumitomo Chem Co Ltd | Separation of analysis of ammonia nitrogen and urea nitrogen in water |
| EP0779880B1 (en) * | 1994-09-08 | 1998-12-02 | Solvay Umweltchemie GmbH | Method of removing chlorate and bromate compounds from water by catalytic reduction |
| WO2001005716A1 (en) * | 1999-07-14 | 2001-01-25 | Akzo Nobel N.V. | Microbiological removal of bromine salts from fluid streams |
| WO2004113239A1 (en) * | 2003-05-20 | 2004-12-29 | Nederlandse Organisatie Voor Toegepast- Natuurwetenschappelijk Onderzoek Tno | Method for removing a pollutant from an aqueous medium using a membrane |
| CN101683989A (en) * | 2008-09-26 | 2010-03-31 | 天津市黎虹化工有限公司 | Process for producing edible grade magnesium chloride |
-
2011
- 2011-02-26 CN CN 201110046219 patent/CN102139897A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3174828A (en) * | 1960-08-31 | 1965-03-23 | Du Pont | Sorption of bromine on anion exchange resins in the presence of excess chlorine |
| JPS5730944A (en) * | 1980-07-31 | 1982-02-19 | Sumitomo Chem Co Ltd | Separation of analysis of ammonia nitrogen and urea nitrogen in water |
| EP0779880B1 (en) * | 1994-09-08 | 1998-12-02 | Solvay Umweltchemie GmbH | Method of removing chlorate and bromate compounds from water by catalytic reduction |
| WO2001005716A1 (en) * | 1999-07-14 | 2001-01-25 | Akzo Nobel N.V. | Microbiological removal of bromine salts from fluid streams |
| WO2004113239A1 (en) * | 2003-05-20 | 2004-12-29 | Nederlandse Organisatie Voor Toegepast- Natuurwetenschappelijk Onderzoek Tno | Method for removing a pollutant from an aqueous medium using a membrane |
| CN101683989A (en) * | 2008-09-26 | 2010-03-31 | 天津市黎虹化工有限公司 | Process for producing edible grade magnesium chloride |
Non-Patent Citations (1)
| Title |
|---|
| 《无机盐工业》 19830131 谭秉彝 氯酸盐电解液除溴 1-4 , 第01期 2 * |
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| PB01 | Publication | ||
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Application publication date: 20110803 |