CN101659418B - Method for preparing boric acid in boracic sodium chloride and potassium chloride saturated bittern solution containing boron - Google Patents
Method for preparing boric acid in boracic sodium chloride and potassium chloride saturated bittern solution containing boron Download PDFInfo
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- CN101659418B CN101659418B CN 200910164353 CN200910164353A CN101659418B CN 101659418 B CN101659418 B CN 101659418B CN 200910164353 CN200910164353 CN 200910164353 CN 200910164353 A CN200910164353 A CN 200910164353A CN 101659418 B CN101659418 B CN 101659418B
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- sodium chloride
- potassium chloride
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Abstract
The invention relates to a method for preparing boric acid in boracic sodium chloride and potassium chloride saturated bittern solution containing boron. The boracic sodium chloride and potassium chloride saturated bittern solution containing boron is processed by the working procedure of calcium and magnesium removal, evaporation concentration, acidification for extracting boron, hot-melt cold crystallization and washing, so that the boric acid can be obtained. The method has the advantages of low product cost and energy consumption, zero emission, less impurities, high recovery rate and purity and the like, and is better in economic benefits.
Description
(1) technical field
The invention belongs to the salt chemical engineering technical field, relate in particular to a kind of method that in the sodium chloride and potassium chloride saturated bittern solution of boracic, prepares boric acid.
(2) background technology
The raw material that China is used for producing boric acid at present has magnesium borate ore and earth's surface salt lake brine, and is day by day ripe with the method for these two kinds of raw material production boric acid.Now explore out these novel liquid mineral products of DEEP MARINE potassium-rich brine, be rich in the multiple elements such as potassium, sodium, lithium, boron, bromine, iodine, and this bittern is state of saturation at concentration extraction sodium-chlor post chlorization sodium Repone K.Carrying boron in the DEEP MARINE potassium-rich brine is a kind of new boric acid production method.
(3) summary of the invention
The objective of the invention is the method that boron is produced boric acid of putting forward for this New Type of Deep subsurface brine design of DEEP MARINE potassium-rich brine.
The technical scheme that realizes the object of the invention is:
The sodium chloride and potassium chloride saturated bittern solution of boracic is carried boron, thermosol cold crystallization, washing procedure through calcium-magnesium removing, evaporation concentration, acidifying and is made boric acid.
The calcium-magnesium removing operation is to add milk of lime in the sodium chloride and potassium chloride saturated bittern solution with boracic, treats pH value of solution=10～12 o'clock precipitated magnesium hydroxide, then adds the yellow soda ash precipitated chalk, solid-liquid separation, the concentration＜0.01g/L of calcium magnesium in the solution;
The evaporation concentration operation is the process of enrichment boron, and the bittern solution that namely obtains after with the calcium-magnesium removing operation adds sodium hydroxide solution, behind pH＞7, it is concentrated into B
2O
3Filter behind＞the 20g/L, remove the sodium chloride and potassium chloride mixed salt, the filtrate temperature is answered＞60 ℃;
It is the process that generates thick boric acid that the boron operation is put forward in acidifying, namely in the solution that the evaporation concentration operation obtains, add acid and make pH value of solution＜7, and cooling, solid-liquid separation obtains thick boric acid or boric acid and borate mixture;
Thermosol cold crystallization operation is thick boric acid that the boron operation obtains or boric acid and borate mixture to be carried in acidifying add water and ℃ be dissolved near saturated in temperature＞80, and cooling solution is to temperature＜30 ℃, and solid-liquid separation obtains the thick boric acid of recrystallization;
Washing procedure is to wash the boric acid that thermosol cold crystallization operation obtains with water, removes the impurity that boric acid is carried secretly, and solid-liquid separation and drying obtain the boric acid product;
As preferably:
In the calcium-magnesium removing operation, remove after magnesium hydroxide and the precipitation of calcium carbonate and remove calcium magnesium with the chelating resin special degree of depth of absorption calcium, magnesium again.
In the evaporation concentration operation, add sodium hydroxide solution, to pH value of solution=9.5～10.5.
In the evaporation concentration operation, be concentrated into B
2O
3＞150g/L.
Carry in the boron operation in acidifying, add acid and make pH value of solution=1～3.
In thermosol cold crystallization operation, the thick boric acid of recrystallization that obtains is operated once to get smart boric acid again according to thermosol cold crystallization operation again, filtrate returning made recrystallization water of thick boric acid.
In thermosol cold crystallization operation, the filtrate after the solid-liquid separation is returned the evaporation concentration operation and is continued to use.
In washing procedure, washing lotion is returned and is made thick boric acid secondary recrystallization water.
The method for preparing boric acid from the sodium chloride and potassium chloride saturated bittern solution of boracic has that product cost is low, energy consumption is little, zero release, impurity is few, the rate of recovery is high, the purity advantages of higher, and preferably economic benefit is arranged.
(4) description of drawings
Fig. 1 is technological process block-diagram of the present invention
(5) embodiment
Embodiment 1
In the sodium chloride and potassium chloride saturated bittern solution of boracic, add milk of lime, treat that pH value of solution=10.4 sink magnesium, then add the heavy calcium of yellow soda ash, solid-liquid separation, remove calcium magnesium with the chelating resin special degree of depth of absorption calcium, magnesium again after removing magnesium hydroxide and precipitation of calcium carbonate, the concentration=0.009g/L of calcium magnesium in the solution adds sodium hydroxide solution with the solution behind the calcium-magnesium removing, behind pH=10, it is concentrated into B
2O
3Filter behind=the 160g/L, remove the sodium chloride and potassium chloride mixed salt, the filtrate temperature is 70 ℃, enter hydrochloric acid in the solution behind separating potassium sodium mixed salt and make pH value of solution=2.5, cooling, boron is separated out in a large number with the boric acid form, solid-liquid separation obtains thick boric acid, and gained filtrate is returned enrichment process.Thick boric acid is added water to be dissolved near saturated 90 ℃ of temperature, cooling solution to 20 ℃, solid-liquid separation gets the thick boric acid of recrystallization one time, the thick boric acid of recrystallization is got smart boric acid by the aforesaid operations secondary recrystallization again, a recrystallization filtrate returns the evaporation concentration operation to be continued to use, and secondary recrystallization filtrate is returned and made a recrystallization water.With pure water detergent boric acid, solid-liquid separation and the dry boric acid product that gets, the washing water behind the detergent boric acid return makes thick boric acid secondary recrystallization water.
Embodiment 2
In the sodium chloride and potassium chloride saturated bittern solution of boracic, add milk of lime, treat that pH value of solution=11 sink magnesium, then add the heavy calcium of yellow soda ash, solid-liquid separation, remove calcium magnesium with the chelating resin special degree of depth of absorption calcium, magnesium again after removing magnesium hydroxide and precipitation of calcium carbonate, the concentration=0.007g/L of calcium magnesium in the solution adds sodium hydroxide solution with the solution behind the calcium-magnesium removing, behind pH=9, it is concentrated into B
2O
3Filter behind=the 80g/L, remove the sodium chloride and potassium chloride mixed salt, the filtrate temperature is 80 ℃, enter sulfuric acid in the solution behind separating potassium sodium mixed salt and make pH value of solution=4, and cooling, boron is separated out in a large number with the boric acid form, and solid-liquid separation obtains thick boric acid, and gained filtrate is returned enrichment process.Thick boric acid is added water to be dissolved near saturated 80 ℃ of temperature, cooling solution to 30 ℃, solid-liquid separation gets the thick boric acid of recrystallization one time, the thick boric acid of recrystallization is got smart boric acid by the aforesaid operations secondary recrystallization again, a recrystallization filtrate returns the evaporation concentration operation to be continued to use, and secondary recrystallization filtrate is returned and made a recrystallization water.With pure water detergent boric acid, solid-liquid separation and the dry boric acid product that gets, the washing water behind the detergent boric acid return makes thick boric acid secondary recrystallization water.
Claims (8)
1. method that in the sodium chloride and potassium chloride saturated bittern solution of boracic, prepares boric acid, it is characterized in that: the sodium chloride and potassium chloride saturated bittern solution of boracic is carried boron, thermosol cold crystallization, washing procedure through calcium-magnesium removing, evaporation concentration, acidifying and is made boric acid, wherein the calcium-magnesium removing operation is to add milk of lime in the sodium chloride and potassium chloride saturated bittern solution with boracic, treat pH value of solution=10～12 o'clock precipitated magnesium hydroxide, then add the yellow soda ash precipitated chalk, solid-liquid separation, the concentration＜0.01g/L of calcium magnesium in the solution; The evaporation concentration operation is the process of enrichment boron, and the bittern solution that namely obtains after with the calcium-magnesium removing operation adds sodium hydroxide solution, behind pH＞7, it is concentrated into B
2O
3Filter behind＞the 20g/L, remove the sodium chloride and potassium chloride mixed salt, the filtrate temperature is answered＞60 ℃; It is the process that generates thick boric acid that the boron operation is put forward in acidifying, namely in the solution that the evaporation concentration operation obtains, add acid and make pH value of solution＜7, and cooling, solid-liquid separation obtains thick boric acid or boric acid and borate mixture; Thermosol cold crystallization operation is thick boric acid that the boron operation obtains or boric acid and borate mixture to be carried in acidifying add water and ℃ be dissolved near saturated in temperature＞80, and cooling solution is to temperature＜30 ℃, and solid-liquid separation obtains the thick boric acid of recrystallization; Washing procedure is to wash the boric acid that thermosol cold crystallization operation obtains with water, removes the impurity that boric acid is carried secretly, and solid-liquid separation and drying obtain the boric acid product.
2. a kind of method that in the sodium chloride and potassium chloride saturated bittern solution of boracic, prepares boric acid according to claim 1, it is characterized in that: in the calcium-magnesium removing operation, remove after magnesium hydroxide and the precipitation of calcium carbonate and remove calcium magnesium with the chelating resin special degree of depth of absorption calcium, magnesium again.
3. a kind of method for preparing boric acid in the sodium chloride and potassium chloride saturated bittern solution of boracic according to claim 1 is characterized in that: in the evaporation concentration operation, add sodium hydroxide solution, to pH value of solution=9.5～10.5.
4. a kind of method for preparing boric acid in the sodium chloride and potassium chloride saturated bittern solution of boracic according to claim 1 is characterized in that: in the evaporation concentration operation, be concentrated into B
2O
3＞150g/L.
5. a kind of method for preparing boric acid in the sodium chloride and potassium chloride saturated bittern solution of boracic according to claim 1 is characterized in that: carry in the boron operation in acidifying, add acid and make pH value of solution=1～3.
6. a kind of method that in the sodium chloride and potassium chloride saturated bittern solution of boracic, prepares boric acid according to claim 1, it is characterized in that: in thermosol cold crystallization operation, the thick boric acid of recrystallization that obtains is operated once to get smart boric acid again according to thermosol cold crystallization operation again, and filtrate returning made recrystallization water of thick boric acid.
7. a kind of method for preparing boric acid in the sodium chloride and potassium chloride saturated bittern solution of boracic according to claim 1 is characterized in that: in thermosol cold crystallization operation, the filtrate after the solid-liquid separation is returned the evaporation concentration operation and is continued to use.
8. a kind of method for preparing boric acid in the sodium chloride and potassium chloride saturated bittern solution of boracic according to claim 6, it is characterized in that: in washing procedure, washing lotion is returned and is made thick boric acid secondary recrystallization water.
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| CN 200910164353 CN101659418B (en) | 2009-09-02 | 2009-09-02 | Method for preparing boric acid in boracic sodium chloride and potassium chloride saturated bittern solution containing boron |
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| CN101659418B true CN101659418B (en) | 2013-03-06 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105217644B (en) * | 2015-10-28 | 2018-05-08 | 中国科学院青海盐湖研究所 | A kind of method that magnesium-based hydrotalcite coproduction boric acid is prepared using salt lake brine with high magnesium-lithium ratio |
| CN109970073B (en) * | 2019-04-03 | 2020-10-09 | 无锡中天固废处置有限公司 | Method for preparing boric acid and potassium chloride by recycling polarizing plate waste liquid |
| CN110255577B (en) * | 2019-06-05 | 2021-10-22 | 核工业北京化工冶金研究院 | Preparation process of nuclear pure grade boric acid standard substance |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5676916A (en) * | 1995-05-12 | 1997-10-14 | Sociedad Minera Salar De Atacama S.A. | Process for extracting the boron content in the brine of natural or industrial salt mines |
| CN1736864A (en) * | 2005-07-17 | 2006-02-22 | 青海中信国安科技发展有限公司 | Production process of boric acid from boron-containing bischofite satured solution |
| CN101024502A (en) * | 2007-01-30 | 2007-08-29 | 西部矿业集团有限公司 | Method for combined extracting boron, magnesium and lithium from salt lake bittern |
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2009
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5676916A (en) * | 1995-05-12 | 1997-10-14 | Sociedad Minera Salar De Atacama S.A. | Process for extracting the boron content in the brine of natural or industrial salt mines |
| CN1736864A (en) * | 2005-07-17 | 2006-02-22 | 青海中信国安科技发展有限公司 | Production process of boric acid from boron-containing bischofite satured solution |
| CN101024502A (en) * | 2007-01-30 | 2007-08-29 | 西部矿业集团有限公司 | Method for combined extracting boron, magnesium and lithium from salt lake bittern |
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