CN109437245A - The method of organic solvent Isolating chlorinated sodium and sodium bromide - Google Patents
The method of organic solvent Isolating chlorinated sodium and sodium bromide Download PDFInfo
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- CN109437245A CN109437245A CN201811529856.2A CN201811529856A CN109437245A CN 109437245 A CN109437245 A CN 109437245A CN 201811529856 A CN201811529856 A CN 201811529856A CN 109437245 A CN109437245 A CN 109437245A
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- sodium
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- methanol
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
- C01D3/18—Purification with selective solvents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/10—Bromides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the separation technology field of halogen element salt, the method for being specifically related to a kind of organic solvent Isolating chlorinated sodium and sodium bromide.In dry sodium chloride and sodium bromide salt-mixture, organic solvent, stirring at normal temperature dissolution is added；Filtering, filters out undissolved salt；Filtrate heating evaporation steams methanol, decrease temperature crystalline；Filtering, filters out the salt of crystallization, and bromination sodium content reaches 90wt% or more in the salt；Continue filtrate heating evaporation steaming remaining methanol, cooling filtering obtains finished product bromination sodium salt；The methanol set of all evapn recycling uses next group dissolving salt.The method of organic solvent Isolating chlorinated sodium and sodium bromide of the present invention, separation equipment is simple, and operating cost is low, rational technology, it is easy to accomplish, the rate of recovery is high, and no waste water generates, no environmental protection pressure, it is easy to accomplish industrialization.
Description
Technical field
The invention belongs to the separation technology field of halogen element salt, it is specifically related to a kind of Isolating chlorinated sodium of organic solvent and bromine
Change the method for sodium.
Background technique
Halogen element salt is that the particularly important raw material of industry, especially sodium chloride and sodium bromide purposes are even more extensive, sodium chloride
It is used as manufacture chlorine, hydrogen, hydrochloric acid, soda ash, caustic soda, chlorate, the raw material of bleaching powder, refrigeration system in inorganic and organic industry
Refrigerant, the raw material of organic synthesis and saltout medicament, steel and iron industry is used as heat treatment agent, and leather industry is used for tan leather,
Soapmaking industry is for soap production of saltouing；In life is the essential daily necessities of the mankind；Medically, the exquisite chlorine of height
Changing sodium more may be utilized in fabricating physiological saline etc., be widely used in clinical treatment and Physiological Experiment.Sodium bromide is for manufacturing photographic film
Emulsion is also used for synthetic material and synthesis in medical industry for producing pharmaceutical intermediate, such as diuretics, sedative etc.
Dyestuff makees bromating agent.
In industrial production, due to the needs of production, the largely waste water containing sodium chloride and sodium bromide can be generated, and this two
Kind salt is very close in nature, it is desirable to which two kinds of salt, which are separated, also becomes extremely difficult.Traditionally use is crystallized or is recrystallized
Method is separated using the different solubility of salt at different temperatures.This method hardly results in sterling, needs back and forth to tie again
It is brilliant repeatedly can, and yield is lower, and energy consumption is higher in separation process.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of Isolating chlorinated sodium of organic solvent and sodium bromide
Method.This method separation equipment is simple, and operating cost is low, rational technology, it is easy to accomplish, the rate of recovery is high, and no waste water generates, acyclic
Packing pressure.
The method of organic solvent Isolating chlorinated sodium and sodium bromide of the present invention, specifically includes the following steps:
(1) in dry sodium chloride and sodium bromide salt-mixture, organic solvent, stirring at normal temperature dissolution is added；
(2) it filters, filters out undissolved salt；
(3) filtrate heating evaporation steams methanol, decrease temperature crystalline；
(4) it filters, filters out the salt of crystallization, which reaches 90wt% or more；
(5) continue filtrate heating evaporation steaming remaining methanol, cooling filtering obtains finished product bromination sodium salt；
(6) salt filtered out in step (2) and (4) repeats above step, and the methanol set of all evapn recycling uses next group
Dissolving salt.
Wherein:
The salt-mixture of sodium chloride used in step (1) and sodium bromide must be it is dry, it is anhydrous, be not the water of the salt
Solution.
It is that dry sodium chloride and sodium bromide mixed salt are directly dissolved with methanol in step (1), rather than in mixed salt aqueous solution
In plus methanol crystallization.
Organic solvent described in step (1) is anhydrous methanol, and purity is 99% or more, it is necessary to ensure that water content in methanol
Less than 1%, prevents the water in methanol from dissolving a large amount of sodium chloride, influence the separating effect in later period.
In the sodium chloride and sodium bromide salt-mixture of drying described in step (1), sodium bromide account for the 70wt% of mixed salt amount with
On, that is to say, that the mass ratio of sodium chloride and sodium bromide is less than 3:7, Within this range, it is desirable to which the organic solvent of addition is without water beetle
The quality of alcohol is 4~6 times for mixing salt quality.
Mixing time described in step (1) is 1.5-3h.
Solution temperature is at 70~80 DEG C in reaction kettle when filtrate heating evaporation described in step (3), and top temperature is 60~64
DEG C, principal security methanol smoothly steams.
Methanol is steamed described in step (3), decrease temperature crystalline is the methanol for steaming the total methanol 20-30wt% of Zhan, is cooled to
20~25 DEG C of crystallizations.
The filtering of cooling described in step (5), is specifically cooled to 20~25 DEG C of filterings.
Finished product bromination sodium salt content described in step (5) is 98.5% or more, and chloride ion content is less than 0.3%.
It needs first to steam the methanol of part in step (3), part mixed salt is precipitated, make being improved for sodium bromide in filtrate
98.5% or so.
The salt filtered out in step (2) and (4) is able to secondary purification, the total recovery of the sodium bromide made reach 75% with
On.All methanol recovery always, does not generate waste liquid, no environmental protection pressure in separation process.
As a preferred technical solution, the method for organic solvent Isolating chlorinated sodium and sodium bromide of the present invention,
Specifically includes the following steps:
(1) in dry sodium chloride and sodium bromide salt-mixture, quantitative organic solvent methanol is added, (amount of methanol with
The variation of the ratio of two kinds of salt and change), stirring at normal temperature dissolution；
(2) it filters, filters out undissolved salt, be mainly sodium chloride in the salt；
(3) filtrate heating evaporation steams 30% methanol, decrease temperature crystalline；
(4) it filters, filters out the salt of crystallization, the salt bromination sodium content is up to 90% or more；
(5) continue filtrate heating evaporation steaming remaining methanol, 98.5% or more content can be obtained in cooling filtering
Bromination sodium salt, the salt meet national Grade A standard；
(6) salt filtered out in step (2) and (4) repeats above step, and the methanol set of all evapn recycling uses next group
Dissolving salt.
It as organic solvent is because by a large amount of lab scale, having separately verified first why the present invention, which selects anhydrous methanol,
Solubility of the common solvents such as alcohol, ethyl alcohol, DMF, acetone, methylene chloride, chloroform, isopropanol and acetonitrile to sodium chloride and sodium bromide
Influence, by experiment, solubility of the sodium bromide in anhydrous methanol is 17 grams under room temperature, and the solubility of sodium chloride is less than 1
Gram, illustrate that anhydrous methanol is larger to the dissolubility difference of sodium bromide and sodium chloride, can be used as separation sodium bromide and sodium chloride
Medium.
Part methanol is first steamed when distillation, mainly considers still to dissolve a small amount of sodium chloride in methanol solution, in technique first
Part methanol is steamed, a small amount of sodium bromide sodium chloride can be separated out, the sodium chloride content in methanol solution is reduced, improves bromination
Sodium content steams the methanol of 20~30wt% by experimental verification, can sodium chloride largely be separated out, be unlikely to shadow
The purity of later period sodium bromide is rung, and sodium bromide can be reduced as far as possible and be largely precipitated, guarantees the rate of recovery of sodium bromide.
Compared with the prior art, the present invention has the following beneficial effects:
The method of organic solvent Isolating chlorinated sodium and sodium bromide of the present invention, separation equipment is simple, and operating cost is low,
Rational technology, it is easy to accomplish, the rate of recovery is high, and no waste water generates, no environmental protection pressure, it is easy to accomplish industrialization.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
(1) analytical reagents sodium chloride and sodium bromide salt-mixture are taken, sodium bromide accounts for the 70% of mixing salt quality, is added 4 times
Anhydrous methanol, stirring at normal temperature 2 hours, filtering, filter out insoluble solids, which installs spare；
(2) filtrate in step (1) is squeezed into evaporating kettle, heating is evaporated, and solution temperature is 75 DEG C in evaporating kettle, and top temperature exists
62℃；
(3) methanol for steaming 20% or so, is cooled to 20 DEG C, and filtering filters out crystal salt, which packages spare；
(4) filtrate in step (3) is squeezed into evaporating kettle, continues heating evaporation；
(5) methanol for steaming 80% or so is cooled to 20 DEG C, and filtering obtains finished product sodium bromide, and filtrate set uses next group
In the filtrate of secondary step (3)；
(6) salt that filters out in step (1) and (3) is repeated into above step；
(7) the Methanol Recovery set steamed is for dissolving salt-mixture in next group step (1)；
(8) finished product sodium bromide obtained in step (5) is dried, packaging；Bromination sodium content is detected 99.0%, chloride ion
It is 0.2%, surplus is impurity；Sodium bromide yield is 78%.
Embodiment 2
(1) company's cyclization abraum salt, mainly sodium chloride and sodium bromide are taken, a small amount of sodium carbonate and sodium sulphate, bromine are also contained
Change sodium accounts for mixing salt quality 80%, is added 5 times of methanol, stirring at normal temperature 2 hours；Filtering, filters out insoluble solids, the solid bag
It installs spare；
(2) filtrate in step (1) is squeezed into evaporating kettle, heating is evaporated, and solution temperature is 80 DEG C in evaporating kettle, and top temperature exists
64℃；
(3) methanol for steaming 30% or so, is cooled to 20 DEG C, and filtering filters out crystal salt, which packages spare；
(4) filtrate in step (3) is squeezed into evaporating kettle, continues heating evaporation；
(5) methanol for steaming 70% or so is cooled to 20 DEG C, and filtering obtains finished product sodium bromide, and filtrate set uses next group
In the filtrate of secondary step (3)；
(6) salt that filters out in step (1) and (3) is repeated into above step；
(7) the Methanol Recovery set steamed is for dissolving salt-mixture in next group step (1)；
(8) finished product sodium bromide obtained in step (5) is dried, packaging；Bromination sodium content is detected 98.7%, chloride ion
0.4%, surplus is impurity；Sodium bromide yield is 75%.
Embodiment 3
(1) analytical reagents sodium chloride and sodium bromide salt-mixture are taken, sodium bromide accounts for the 75% of mixing salt quality, is added 4.5
Anhydrous methanol again, stirring at normal temperature 2 hours, filtering filtered out insoluble solids, which installs spare；
(2) filtrate in step (1) is squeezed into evaporating kettle, heating is evaporated, and solution temperature is 70 DEG C in evaporating kettle, and top temperature exists
60℃；
(3) methanol for steaming 20% or so, is cooled to 20 DEG C, and filtering filters out crystal salt, which packages spare；
(4) filtrate in step (3) is squeezed into evaporating kettle, continues heating evaporation；
(5) methanol for steaming 80% or so is cooled to 20 DEG C, and filtering obtains finished product sodium bromide, and filtrate set uses next group
In the filtrate of secondary step (3)；
(6) salt that filters out in step (1) and (3) is repeated into above step；
(7) the Methanol Recovery set steamed is for dissolving salt-mixture in next group step (1)；
(8) finished product sodium bromide obtained in step (5) is dried, packaging；Bromination sodium content is detected 98.9%, chloride ion
0.3%, surplus is impurity；Sodium bromide yield is 78%.
Claims (8)
1. a kind of method of organic solvent Isolating chlorinated sodium and sodium bromide, it is characterised in that: specifically includes the following steps:
(1) in dry sodium chloride and sodium bromide salt-mixture, organic solvent, stirring at normal temperature dissolution is added；
(2) it filters, filters out undissolved salt；
(3) filtrate heating evaporation steams organic solvent, decrease temperature crystalline；
(4) it filters, filters out the salt of crystallization, bromination sodium content reaches 90wt% or more in the salt；
(5) continue filtrate heating evaporation steaming remaining methanol, cooling filtering obtains finished product bromination sodium salt；
(6) salt filtered out in step (2) and (4) repeats above step, and the methanol set of all evapn recycling uses next group dissolution
Salt.
2. the method for organic solvent Isolating chlorinated sodium and sodium bromide according to claim 1, it is characterised in that: step (1)
Described in organic solvent be anhydrous methanol, purity is 99% or more, it is necessary to ensure that water content is less than 1% in methanol.
3. the method for organic solvent Isolating chlorinated sodium and sodium bromide according to claim 1, it is characterised in that: step (1)
Described in drying sodium chloride and sodium bromide salt-mixture in, sodium bromide accounts for the 70wt% or more of mixed salt amount, within this range, need
The quality of organic solvent to be added is 4~6 times for mixing salt quality.
4. the method for organic solvent Isolating chlorinated sodium and sodium bromide according to claim 1, it is characterised in that: step (1)
Described in mixing time be 1.5-3h.
5. the method for organic solvent Isolating chlorinated sodium and sodium bromide according to claim 1, it is characterised in that: step (3)
Described in filtrate heating evaporation when reaction kettle in solution temperature at 70~80 DEG C, top temperature at 60~64 DEG C.
6. the method for organic solvent Isolating chlorinated sodium and sodium bromide according to claim 1, it is characterised in that: step (3)
Described in steam methanol, decrease temperature crystalline is the methanol for steaming the total methanol 20-30wt% of Zhan, is cooled to 20~25 DEG C of crystallizations.
7. the method for organic solvent Isolating chlorinated sodium and sodium bromide according to claim 1, it is characterised in that: step (5)
Described in cooling filtering, be specifically cooled to 20~25 DEG C of filterings.
8. the method for organic solvent Isolating chlorinated sodium and sodium bromide according to claim 1, it is characterised in that: step (5)
Described in finished product bromination sodium salt content 98.5% or more, chloride ion content is less than 0.3%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110950360A (en) * | 2019-12-09 | 2020-04-03 | 广东飞南资源利用股份有限公司 | Separation method of sodium bromide and sodium chloride and recovery method of sodium bromide in solid bromine roasting slag |
| CN112028091A (en) * | 2020-09-16 | 2020-12-04 | 兰州大学 | Preparation method of nano-salt template |
| CN112279273A (en) * | 2019-07-24 | 2021-01-29 | 中国科学院过程工程研究所 | Treatment method for removing COD (chemical oxygen demand) of industrial byproduct salt |
| CN112441600A (en) * | 2019-08-30 | 2021-03-05 | 联化科技(盐城)有限公司 | Separation method of industrial mixed potassium salt |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112279273A (en) * | 2019-07-24 | 2021-01-29 | 中国科学院过程工程研究所 | Treatment method for removing COD (chemical oxygen demand) of industrial byproduct salt |
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| CN112028091A (en) * | 2020-09-16 | 2020-12-04 | 兰州大学 | Preparation method of nano-salt template |
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