CN105858687A - Method for preparing sodium bromide using waste hydrobromic acid - Google Patents
Method for preparing sodium bromide using waste hydrobromic acid Download PDFInfo
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- CN105858687A CN105858687A CN201610486509.0A CN201610486509A CN105858687A CN 105858687 A CN105858687 A CN 105858687A CN 201610486509 A CN201610486509 A CN 201610486509A CN 105858687 A CN105858687 A CN 105858687A
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- sodium bromide
- hydrobromic acid
- mixed liquor
- useless
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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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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for preparing sodium bromide using waste hydrobromic acid, comprising the following steps: 1), mixing sodium carbonate with water, and stirring well to obtain a first mixed liquid; 2), adding waste hydrobromic acid into the first mixed liquid obtained in step 1), and reacting under stirring to obtain a second mixed liquid, post-reaction PH being 2-7; 3), adding an adsorbing medium into the second mixed liquid, and heating to 60-130 DEG C to obtain a third mixed liquid; 4), adding sodium carbonate into the third mixed liquid obtained in step 3) to adjust pH to 3-8, heating at 75-140 DEG C, and filtering to obtain sodium bromide aqueous solution; 5), concentrating, centrifuging and drying the sodium bromide aqueous solution obtained in step 4) to obtain solid sodium bromide. Compared with the prior art, the method has the advantages of high production efficiency and low cost.
Description
Technical field
The present invention relates to a kind of method preparing sodium bromide, a kind of utilize useless hydrobromic acid to prepare sodium bromide
Method.
Background technology
Sodium bromide is white crystals or powder.There are saline taste or micro-strip bitterness.Moisture caking is absorbed but not deliquescence from air.
It is dissolved in water.Low toxicity, irritant.For microdetermination cadmium analytical chemistry, photomechanical production, pharmacy etc., overseas utilization sodium bromide is molten
It is huge that liquid makees oil drilling solution additive usage amount, extensive market.Physico-chemical property colourless cubic system crystal or white granular
Powder, odorless, taste alkali and micro-hardship.Relative density 3.203 (25 DEG C), fusing point 747 DEG C, there is hygroscopicity in atmosphere, soluble in water
(when 100 DEG C, dissolubility is 121g/100ml water), aqueous solution is neutrality, is slightly soluble in alcohol, separates out anhydrous bromination when 51 DEG C in solution
Sodium crystallizes, and then generates two water things less than 51 DEG C, and its bromide ion can be replaced by chlorine.
Sodium bromide preparation method can be divided into neutralisation, reducing process and ion exchange etc. several at present, wherein neutralisation work
Skill is simple, and obtained product quality is preferable, is therefore widely used in commercial production, particularly sodium carbonate and the hydrobromic acid system of reacting
The mode of standby sodium bromide.Owing to the usage amount of sodium bromide solution is very big, Production requirement amount is relatively big, and hydrobromic cost is raw in reality
Still significant proportion is accounted for during product.In industry actual production, the useless hydrobromic acid amount of generation is the most more, but can not get very well
Utilization, causing huge waste, if re-used by useless hydrobromic acid, the production cost of sodium bromide solution can be made again to drop
Low, create bigger interests for enterprise.Owing to useless hydrobromic acid existing the by-product acid of a lot of organic reaction, use existing sodium bromide
The preparation method of solution, it is impossible to realize the removing of the impurity such as Organic substance in useless hydrobromic acid, have a strong impact on product final mass.
Summary of the invention
The present invention proposes a kind of method utilizing useless hydrobromic acid to prepare sodium bromide.
The technical scheme is that and be achieved in that: a kind of method utilizing useless hydrobromic acid to prepare sodium bromide, including with
Lower step:
1) soda is mixed with water, and stir, prepare the first mixed liquor；
2) under conditions of heating, in the first mixed liquor of step 1) gained, add the reaction of useless hydrobromic acid, make the reacted PH be
2-7, prepares the second mixed liquor；Build suitable PH, to facilitate the removing of impurity in solution；
3) by step 2) the second mixed liquor of gained adds adsorbing medium and heats, heating-up temperature is 60-130 DEG C, prepares the
Three mixed liquors；At such a temperature, on the one hand will not affect impurity-eliminating effect because temperature is too low, on the other hand adsorbing medium can be made to protect
Hold optimal field of activity, impurity is had the strongest adsorption；
4) by the 3rd mixed liquor of step 3) gained adds soda regulation pH to 3-8, heat at temperature is 75-140 DEG C, then
Filter to obtain aqueous sodium bromide；
5) aqueous sodium bromide step 4) obtained is concentrated, centrifugal, be dried prepared sodium bromide solid.
As preferred technical scheme, in step 1), ratio for 1:1-1:2 in mass ratio mix soda with water, and stirring mixes
The conjunction time is 30min-90min.
As preferred technical scheme, step 2) in the first mixed liquor be 1:0.8-1:2 with useless hydrobromic mass ratio.
As preferred technical scheme, step 2) in the first mixed liquor be 20 ~ 70 DEG C with useless hydrobromic reaction temperature, instead
It is 40-90min between Ying Shi.
As preferred technical scheme, the heat time heating time in step 3) is 1-2h.
As preferred technical scheme, described useless hydrobromic acid mass concentration is 40%-41%.
As preferred technical scheme, the addition of described adsorbing medium is the 0.5%-1.5% of the second mixed liquor quality,
Described adsorbing medium be in activated carbon, active hargil, kieselguhr, attapulgite any one or a few.
As preferred technical scheme, the heat time heating time in step 4) is 0.5-1.5h.
As preferred technical scheme, step 4) adds the 0.1%-0.5% that amount is the 3rd mixed liquor quality of soda.
As preferred technical scheme, the baking temperature in step 5) is 100 DEG C-110 DEG C, containing of gained sodium bromide solid
Water yield ＜ 1%.
Owing to have employed technique scheme, the present invention has a beneficial effect highlighted below:
1, the present invention utilizes Industry Waste hydrobromic acid to react with sodium carbonate, produces sodium bromide solution, and in preparation process, regulation is suitable
Operating temperature, build suitable pH value working environment, the convenient impurity removing the more difficult separation such as Organic substance, coordinate absorption simultaneously
Medium adsorbs, and suitable operating temperature makes the field of activity that adsorbing medium holding is optimal, facilitates impurity to remove, with existing technique phase
Ratio, the present invention, without using refined hydrobromic acid to carry out sodium bromide production, saves great amount of cost, and can obtain stay-in-grade bromine
Changing sodium, preparation method efficiency is high.
2, good impurity removing effect, utilizes the sodium bromide solution that useless hydrobromic acid prepares, with the bromine prepared by refined hydrobromic acid
Change sodium to compare, the product quality indifference opposite sex of formation, form the product with grade, low cost, and useless hydrobromic acid is recycled,
Environmental protection.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under not making creative work premise, broadly falls into the model of present invention protection
Enclose.
Embodiment 1
A kind of method utilizing useless hydrobromic acid to prepare sodium bromide, comprises the following steps:
1) by soda and water, ratio for 1:1 in mass ratio mix, and stirs 30min to uniformly, prepared first mixed liquor；
2) in the first mixed liquor of step 1) gained add mass concentration be 40% give up hydrobromic acid reaction, be 20 DEG C of bars in temperature
Reacting 90min under part, the first mixed liquor is 1:0.8 with useless hydrobromic mass ratio, and making reacted PH is 7, prepares second and mixes
Close liquid；
3) by step 2) the second mixed liquor of gained adds the activated carbon of the second mixed liquor quality 0.5% and is heated to 60 DEG C,
Heating 2h, prepares the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the soda of the 3rd mixed liquor quality 0.5%, regulate pH to 8, in temperature
It is to heat at 75 DEG C, heats 1.5h, then filter to obtain aqueous sodium bromide；
5) aqueous sodium bromide step 4) obtained is concentrated, centrifugal, be dried prepared water content is 0.5% sodium bromide solid,
Baking temperature is 100 DEG C.
Embodiment 2
A kind of method utilizing useless hydrobromic acid to prepare sodium bromide, comprises the following steps:
1) by soda and water, ratio for 1:2 in mass ratio mix, and stirs 90min to uniformly, prepared first mixed liquor；
2) in the first mixed liquor of step 1) gained add mass concentration be 40% give up hydrobromic acid reaction, be 70 DEG C of bars in temperature
Reacting 40min under part, the first mixed liquor is 1:2 with useless hydrobromic mass ratio, and making reacted PH is 2, prepares the second mixing
Liquid；
3) by step 2) the second mixed liquor of gained adds the attapulgite of the second mixed liquor quality 1.5% and is heated to 130
DEG C, heat 1h, prepare the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the soda of the 3rd mixed liquor quality 0.1%, regulate pH to 3, in temperature
It is to heat at 140 DEG C, heats 0.5h, then filter to obtain aqueous sodium bromide；
5) aqueous sodium bromide step 4) obtained is concentrated, centrifugal, be dried prepared water content is 0.5% sodium bromide solid,
Baking temperature is 110 DEG C.
Embodiment 3
A kind of method utilizing useless hydrobromic acid to prepare sodium bromide, comprises the following steps:
1) by soda and water, ratio for 1:1.5 in mass ratio mix, and stirs 60min to uniformly, prepared first mixed liquor；
2) in the first mixed liquor of step 1) gained add mass concentration be 41% give up hydrobromic acid reaction, be 50 DEG C of bars in temperature
Reacting 60min under part, the first mixed liquor is 1:1.5 with useless hydrobromic mass ratio, and making reacted PH is 5, prepares second and mixes
Close liquid；
3) by step 2) the second mixed liquor of gained adds the kieselguhr of the second mixed liquor quality 1% and is heated to 100 DEG C, add
Hot 1.5h, prepares the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the soda of the 3rd mixed liquor quality 0.3%, regulate pH to 6, in temperature
It is to heat at 100 DEG C, heats 1h, then filter to obtain aqueous sodium bromide；
5) aqueous sodium bromide step 4) obtained is concentrated, centrifugal, be dried prepared water content is 0.5% sodium bromide solid,
Baking temperature is 105 DEG C.
Reference examples 1
A kind of method utilizing useless hydrobromic acid to prepare sodium bromide, comprises the following steps:
1) by soda and water, ratio for 1:1.5 in mass ratio mix, and stirs 60min to uniformly, prepared first mixed liquor；
2) in the first mixed liquor of step 1) gained add mass concentration be 41% give up hydrobromic acid reaction, be 50 DEG C of bars in temperature
Reacting 60min under part, making reacted PH is 9, prepares the second mixed liquor；
3) by step 2) the second mixed liquor of gained adds the kieselguhr of the second mixed liquor quality 1% and is heated to 100 DEG C, add
Hot 1.5h, prepares the 3rd mixed liquor；
4) by the 3rd mixed liquor regulation pH to 6 of step 3) gained, heat at temperature is 100 DEG C, heat 1h, then filter
Aqueous sodium bromide；
5) aqueous sodium bromide step 4) obtained is concentrated, centrifugal, be dried prepared water content is 0.5% sodium bromide solid,
Baking temperature is 105 DEG C.
Reference examples 2
A kind of method utilizing useless hydrobromic acid to prepare sodium bromide, comprises the following steps:
1) by soda and water, ratio for 1:1.5 in mass ratio mix, and stirs 60min to uniformly, prepared first mixed liquor；
2) in the first mixed liquor of step 1) gained add mass concentration be 41% give up hydrobromic acid reaction, be 50 DEG C of bars in temperature
Reacting 60min under part, the first mixed liquor is 1:1.5 with useless hydrobromic mass ratio, and making reacted PH is 5, prepares second and mixes
Close liquid；
3) by step 2) the second mixed liquor of gained adds the kieselguhr of the second mixed liquor quality 1% and is heated to 140 DEG C, add
Hot 1.5h, prepares the 3rd mixed liquor；
4) by the 3rd mixed liquor of step 3) gained adds the 3rd mixed liquor quality 0.3% soda, regulate pH to 6, in temperature
Degree is to heat at 100 DEG C, heats 1h, then filters to obtain aqueous sodium bromide；
5) aqueous sodium bromide step 4) obtained is concentrated, centrifugal, be dried prepared water content is 0.5% sodium bromide solid,
Baking temperature is 105 DEG C.
Reference examples 3
A kind of method utilizing useless hydrobromic acid to prepare sodium bromide, comprises the following steps:
1) by soda and water, ratio for 1:1.5 in mass ratio mix, and stirs 60min to uniformly, prepared first mixed liquor；
2) in the first mixed liquor of step 1) gained add mass concentration be 41% give up hydrobromic acid reaction, be 50 DEG C of bars in temperature
Reacting 60min under part, the first mixed liquor is 1:1.5 with useless hydrobromic mass ratio, and making reacted PH is 5, prepares second and mixes
Close liquid；
3) by step 2) the second mixed liquor of gained adds the kieselguhr of the second mixed liquor quality 1% and is heated to 100 DEG C, add
Hot 1.5h, prepares the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add soda, regulate pH to 9, heat at temperature is 100 DEG C, heat 1h,
Then aqueous sodium bromide is filtered to obtain；
5) aqueous sodium bromide step 4) obtained is concentrated, centrifugal, be dried prepared water content is 0.5% sodium bromide solid,
Baking temperature is 105 DEG C.
Being chemically examined by the sodium bromide product of the embodiment of the present invention and reference examples gained, result is as shown in the table:
As seen from the above table, the product quality prepared by embodiment of the present invention 1-3 meets required standard, and reference examples 1-3 change side
Temperature parameter in method, PH parameter, all can produce impact to this product quality.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (10)
1. one kind utilizes the method that useless hydrobromic acid prepares sodium bromide, it is characterised in that comprise the following steps:
1) soda is mixed with water, and stir, prepare the first mixed liquor；
2) under conditions of heating, in step 1) the first mixed liquor of gained adds useless hydrobromic acid reaction, make reacted PH
For 2-7, prepare the second mixed liquor；
3) by step 2) the second mixed liquor of gained adds adsorbing medium and heats, heating-up temperature is 60-130 DEG C, prepares the
Three mixed liquors；
4) by step 3) the 3rd mixed liquor of gained adds soda regulation pH to 3-8, heat at temperature is 75-140 DEG C, then
Filter to obtain aqueous sodium bromide；
5) by step 4) aqueous sodium bromide that obtains is concentrated, centrifugal, be dried and prepare sodium bromide solid.
2. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: step 1) in
Soda is that the ratio of 1:1-1:2 mixes in mass ratio with water, and stirring incorporation time is 30min-90min.
3. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: step 2) in
First mixed liquor is 1:0.8-1:2 with useless hydrobromic mass ratio.
4. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: step 2) in
First mixed liquor is 20～70 DEG C with useless hydrobromic reaction temperature, and the response time is 40-90min.
5. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: step 3) in
Heat time heating time be 1-2h.
6. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: described useless hydrogen
Bromic acid mass concentration is 40%-41%.
7. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: described absorption
The addition of medium is the 0.5%-1.5% of the second mixed liquor quality, and described adsorbing medium is activated carbon, active hargil, diatom
Soil, in attapulgite any one or a few.
8. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: step 4) in
Heat time heating time be 0.5-1.5h.
9. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: step 4) in
Add the 0.1%-0.5% that amount is the 3rd mixed liquor quality of soda.
10. according to a kind of method utilizing useless hydrobromic acid to prepare sodium bromide described in claim 1, it is characterised in that: step 5)
In baking temperature be 100 DEG C-110 DEG C, water content ＜ 1% of gained sodium bromide solid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610486509.0A CN105858687A (en) | 2016-06-26 | 2016-06-26 | Method for preparing sodium bromide using waste hydrobromic acid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610486509.0A CN105858687A (en) | 2016-06-26 | 2016-06-26 | Method for preparing sodium bromide using waste hydrobromic acid |
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| CN201610486509.0A Pending CN105858687A (en) | 2016-06-26 | 2016-06-26 | Method for preparing sodium bromide using waste hydrobromic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047807A (en) * | 2020-08-24 | 2020-12-08 | 临海市建新化工有限公司 | Impurity removal process for methyl bromide by adopting weak base |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616352A (en) * | 2003-11-12 | 2005-05-18 | 李茂山 | Process for extracting sodium bromide |
| CN104649300A (en) * | 2013-11-19 | 2015-05-27 | 湖南省湘中制药有限公司 | Method for recovering and refining sodium bromide from dipropyl cyanoacetate mixture |
-
2016
- 2016-06-26 CN CN201610486509.0A patent/CN105858687A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616352A (en) * | 2003-11-12 | 2005-05-18 | 李茂山 | Process for extracting sodium bromide |
| CN104649300A (en) * | 2013-11-19 | 2015-05-27 | 湖南省湘中制药有限公司 | Method for recovering and refining sodium bromide from dipropyl cyanoacetate mixture |
Non-Patent Citations (1)
| Title |
|---|
| 沈艳等: ""溴化钠的制备工艺综述"", 《江西化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112047807A (en) * | 2020-08-24 | 2020-12-08 | 临海市建新化工有限公司 | Impurity removal process for methyl bromide by adopting weak base |
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Application publication date: 20160817 |
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