CN106587090A - Method for synthesizing disodium octaborate tetrahydrate by utilizing liquid boron ore - Google Patents
Method for synthesizing disodium octaborate tetrahydrate by utilizing liquid boron ore Download PDFInfo
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- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
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Abstract
The invention belongs to the technical field chemical, and relates to a method for synthesizing disodium octaborate tetrahydrate by utilizing liquid boron ore. The method comprises the following steps: performing acidizing and boron extracting on the liquid boron ore to obtain acidized boron extracting liquid, extracting boracic acid from the acidized boron extracting liquid by adopting an alcohol extraction agent at a normal temperature, performing an esterification reaction on an extracting agent and the boracic acid to obtain a boron-rich organic phase, washing the boron-rich organic phase by adopting an acidic solution with the acidity of 0 to 12 M to remove the impurities, such as calcium, magnesium and iron, mixing the impurities-removed boron-rich organic phase and sodium hydroxide solution, performing back extraction with stirring to obtain a back extraction solution, controlling the concentration and the flow ratio of the sodium hydroxide solution so that a hydrolysis reaction process of boron-rich organic phase borate is coupled with a synthesis reaction process of the disodium octaborate tetrahydrate to directly obtain disodium octaborate tetrahydrate solution, and drying and pulverizing to obtain the disodium octaborate tetrahydrate with low impurity content. According to the method, a preparation process of the disodium octaborate tetrahydrate is simplified; the method has the characteristics that the raw materials are low in cost and are easily obtained, the product quality is high, the energy consumption is reduced, and the method is suitable for industrial application.
Description
Technical field
The present invention relates to chemical technology field, more particularly to a kind of side of utilization liquid boron rock synthesis four water eight borate two sodium
Method.
Background technology
Four water eight borate two sodium is one of important fine boride, and boron content is high, boron element theoretical content 20.967%,
Actual content 20%～21.5%.Which is highly soluble in water, is 4.2g/100ml water at 0 DEG C, is 41g/100ml water when 50 DEG C, and 100
DEG C when be 74g/100ml water.Four water eight borate two sodium has a wide range of applications in agricultural and industrial aspect, agricultural aspect, due to
Boron is one of element necessary to plant growing, has very important effect in growth and development of plants, agriculturally commonly uses and sprays
The method of fertilizer carrys out boron make-up, and four water eight borate two sodium can be with as boron content height, good water solubility, aqueous solution are in weakly acidic pH, almost
With all pestsides synthesis, therefore using extensive in agricultural production.Industrial aspect, due to four water eight borate two sodium have insect prevention and
Antibacterial effect, can be used as environmental friendly, anti-corrosive agent.
The method of production four water eight borate two sodium is mainly Borax, boric acid polymerization, and other also have sodium-hydroxide method.For
The borax decahydrate of production four water eight borate two sodium, higher to purity requirement, domestic borax decahydrate is using relatively difficult at present.Boron
Acid also has higher requirements to purity for the production of four water eight borate two sodium, and the boric acid of current China's One-step production is difficult to completely
Sufficient technique needs.Chinese invention patent CN201410634611 discloses a kind of using one-step method boric acid synthesis four water, eight boric acid two
The method of sodium, one-step method boric acid, chemicals containing sodium, cleaner are placed in reactor, are heated with stirring to 60～120 DEG C, insulation
Under the conditions of continue 0.5～2h of heating, obtained product filtered, filtrate is dried at 90～200 DEG C, make powder after obtain low
The four water eight borate two sodium of impurity content, the cleaner be hydrogen peroxide, strong aqua ammonia, ammonium carbonate, ammonium hydrogen carbonate, one in activated carbon
Plant or two or more mixing.Chinese invention patent CN201410253286.4 discloses a kind of synthesis of four water eight borate two sodium
Method, method are characterized in that the mixing that technological process is raw material, heating for dissolving, filter and remove residue obtain mother solution, crystallisation by cooling, centrifugation point
From, cold drying eliminating water, be dried eliminating water, crush and screen to obtain eight operations compositions of product, it is raw materials used be mixed into boric acid and other
Borax decahydrate, borax pentahydrate, borax anhydrouss, any one in four kinds of raw materials of sodium hydroxide carry out dispensing.Above-mentioned production four
The method of eight boric acid disodium of water needs to use the higher boric acid of purity, Borax and makees raw material, and cost of material is high, or in building-up process
Cleaner is added, reagent cost is increased and is easily introduced impurity, technological process is complicated, product quality is difficult to control to.
Solvent extraction technology is the effective technology of the separation and Extraction object element from solution, with separation efficiency height, technique
, operation serialization simple with equipment, the advantages of automatically controlling is easily achieved, researcher is to solvent extraction technology from liquid boron rock
Extracting separating boron has carried out substantial amounts of research.Chinese invention patent CN201210105542.6 is disclosed using salt lake lithium liquor
The method for producing high borosilicate glass industry and boric acid, its basic working procedure are, after concentration is shone on salt lake lithium liquor salt pan beach, to enter
Cross pressure-filtering deslagging, sulphuric acid acidifying, the acidifying solution dense rear filter pressing that cools obtain thick boric acid, acidifying analysis boron mother solution carry out extraction and
Three-level back extraction, extractant consist of "+50% aerial kerosene (volume ratio) of+25% isoamyl alcohol of 25% isooctanol ", strippant
For the deionized water that pH value is 1.5, cold crystallization after the thick boric acid of strip liquor thermosol, finally it is centrifuged, washs dry packing
Obtain final product boric acid finished product.Document " mixed alcohol extractant puies forward boron experimentation from salt lake bittern " with 2- ethyls -1,3 hexanediol with it is different
Capryl alcohol is diluent from boron extraction in salt lake bittern, development by certain volume ratio composition mixed extractant, sulfonated kerosene
The concentration of extractant, brine ph, organic faciess and water phase volume ratio, extraction time, extraction series, saturation loading capacity, back extraction
The condition experiments such as agent concentration, research show, from sodium hydroxide solution as back washing agent, as salt content of magnesium is higher, select
Just easily there is emulsifying in the sodium hydroxide solution (being more than 0.25mol/l) of larger concentration, test from the concentration of sodium hydroxide is
0.01mol/l～0.25mol/l.Chinese invention patent CN201210231099.7 discloses one kind and extracts from lake bittern containing magnesium salt
Take the method for carrying boron, it is proposed that with lake bittern containing magnesium salt as material liquid, with containing aryl 1,3-binary aliphatic alcohol is extracted to carry boron
Agent, by mixed solution that boron extractant and diluent constitute is carried as extraction organic faciess, extraction organic faciess carry out many with material liquid
Stage countercurrent is extracted, and obtains the extraction phase containing boric acid, with aqueous alkali as back washing agent, by back washing agent and the extraction phase containing boric acid
Multi-stage countercurrent back extraction is carried out, boracic aqueous solution is obtained.1,3-binary aliphatic alcohol of the class containing aryl be the invention provides for height
Effect carries boron extractant, and the boric acid being extracted in organic faciess can be straight by the routine chemical separation technology such as back extraction operation and evaporative crystallization
Connect and obtain tincal product.Existing employing extraction puies forward boron technique from liquid boron rock, and the boron-rich organic faciess being obtained by extraction directly are entered instead
Extraction, back washing agent adopt Low acid deionized water or low-concentration alkali liquor, and strip liquor final product is boric acid or Borax, due to boric acid or
In Borax water at normal temperature, dissolubility is low, and in causing strip liquor, Boron contents are low, subsequent evaporation crystallization process high energy consumption, and due to boron-rich
It is not scrubbed before organic faciess back extraction, cause the impurity content such as magnesium in strip liquor high, four water, eight boric acid such as prepared by high added value
Disodium product, needs further deep processing, high energy consumption and long flow path.
The content of the invention
Present invention aims to the deficiencies in the prior art, there is provided one kind can reduce process energy consumption and cost and technique
Flow process is simply controllable, it is easy to which the utilization liquid boron rock of Project Realization synthesizes the method for four water eight borate two sodium.
The present invention provides a kind of method that utilization liquid boron rock synthesizes four water eight borate two sodium, and its technological process is：
The acidifying of liquid boron rock carries boron and obtains acidifying and carries boron liquid, alcohol kind of extractants and diluent are mixed to get extract it is organic
Phase, acidifying carry boron liquid and carry out multi-stage counter current extraction with extraction organic faciess at normal temperatures, by the esterification of alcohol kind of extractants and boric acid
Reaction obtains boron-rich organic faciess, and boron-rich organic faciess remove the impurity such as calcium, magnesium, ferrum using the washing of 0～12M of acidity acidity solutions, wash
Wash away it is miscellaneous after boron-rich organic faciess mix with back washing agent sodium hydroxide solution, back extraction is carried out under stirring and obtains strip liquor, by control
Concentration of sodium hydroxide solution processed and flow ratio, make the hydrolysis reaction of boron-rich organic faciess borate and the conjunction of four water eight borate two sodium
Couple into course of reaction, directly obtain four water eight borate two sodium solution, drying is obtained the low impurity content after making powder
Four water eight borate two sodium.
Preferably, the preparation method that described acidifying carries boron liquid is：To in liquid boron rock add inorganic acid solution react to
PH value≤2 of solution, filtration obtain final product.
Wherein, the liquid boron rock is boracic salt lake bittern, and its mesoboric acid total concentration is 1g/l～60g/l, and magnesium ion is dense
Spend for 60g/l～120g/l.
Wherein, the alcohol kind of extractants is unitary fatty alcohol, binary aliphatic alcohol, aromatic alcohol or its combination.
Wherein, the diluent be No. 200 industrial napthas, kerosene, benzene,toluene,xylenes or derivatives thereof one kind or
It is various, it is preferred that the diluent is sulfonated kerosene.
Wherein, 0～12M of acidity acidity solutions are that the preparation of mineral acid and pure water is obtained, it is preferable that the mineral acid is
Hydrochloric acid.
Wherein, in the boron-rich organic faciess after the washing impurity-removing, impurity element total amount is less than with host element boron mass ratio
0.01:1, described impurity element includes but is not limited to calcium constituent, magnesium elements, ferrum element.
Wherein, the back washing agent concentration of sodium hydroxide solution is 0.1～10mol/l, stripping process organic faciess and back washing agent
Flow ratio is 1:1～30:1, back extraction temperature is 10～100 DEG C.
Wherein, it is preferred that the back washing agent concentration of sodium hydroxide solution is 0.5～2mol/l.
Wherein, it is preferred that 20～50 DEG C of the back extraction temperature
Wherein, in the strip liquor, boron sodium element mass ratio is 1.85～1.9.
Wherein, it is preferred that 20～80g/l of boron element mass concentration in the strip liquor.
Compared to prior art, the invention has the beneficial effects as follows：Washing impurity-removing is carried out to boron-rich organic faciess so that washing is removed
In boron-rich organic faciess after miscellaneous, the impurity element total amount such as calcium, magnesium, ferrum and host element boron mass ratio are less than 0.01:1, can directly obtain
The strip liquor of low impurity content, and due to washing impurity-removing after boron-rich organic faciess in the impurity element such as calcium, magnesium, ferrum it is very low, can adopt
Emulsifying is not produced as back washing agent with the sodium hydroxide solution of high concentration, it is easy to by controlling concentration of sodium hydroxide solution and stream
Than making the boron-rich hydrolysis reaction of organic faciess borate couple with the synthetic reaction process of four water eight borate two sodium, directly obtaining
Four water eight borate two sodium solution is obtained, drying is obtained the four water eight borate two sodium of the low impurity content after making powder.The present invention
Method simplifies the preparation process of four water eight borate two sodium, with raw material is cheap and easy to get, superior product quality, energy consumption decline, are suitable to
The characteristics of commercial Application.
Description of the drawings
Fig. 1 is the schematic flow sheet that the embodiment of the present invention synthesizes four water eight borate two sodium using liquid boron rock.
Specific embodiment
The present invention is described in detail below by way of concrete and infinite embodiment, so that advantages and features of the invention energy
It is easier to be readily appreciated by one skilled in the art.
Following examples adopt technique as shown in Figure 1.
Described technique specifically includes following step：
1) acidifying proposes the preparation of boron liquid：To in liquid boron rock, inorganic acid solution is added to react to pH value≤2 of solution, filtration is
Must be acidified and carry boron liquid；
2) extract organic faciess to prepare：Alcohol kind of extractants and diluent are mixed in proportion and obtain extracting organic faciess；
3) extract：Acidifying carries boron liquid and carries out multi-stage counter current extraction with extraction organic faciess at normal temperatures, by alcohol kind of extractants
Boron-rich organic faciess are obtained with the esterification of boric acid；
4) washing impurity-removing：Boron-rich organic faciess remove the impurity such as calcium, magnesium, ferrum using the washing of 0～12M of acidity acidity solutions.
5) back extraction：Back extraction is carried out to boron-rich organic faciess using 0.1～10mol/l sodium hydroxide solutions so that boron-rich organic
Phase mesoboric acid ester hydrolysis reaction process is coupled with the synthetic reaction process of four water eight borate two sodium, obtains four water eight borate two sodium molten
Liquid, solution drying soap powder are obtained four water eight borate two sodium.
The composition of the liquid boron rock used in the following embodiments of the present invention is as shown in table 1.
The composition of table 1 certain liquid boron rock
| Composition | Li+ | Mg2+ | Ca2+ | Fe2+ | Cl- | B2O3 |
| Content (g/l) | 0.5～10 | 80～130 | 0～5 | 0～5 | ≥200 | 1～50 |
Specific embodiment 1
Alcohol kind of extractants selects isooctanol, diluent to have in extraction from sulfonated kerosene composition extraction organic faciess, isooctanol
Volume ratio 20%～50% is accounted in machine phase.
6mol/l hydrochloric acid solutions are added in 1 part of liquid boron rock, is reacted to solution ph≤2, above-mentioned solution is filtered
Boric acid solid and acidifying carry boron liquid, and the flow ratio that extraction organic faciess agent carries boron liquid with acidifying is 1：1～1.5, carry out in 25 DEG C 4 grades it is inverse
Stream extraction, obtains boron-rich organic faciess after split-phase, with 1mol/l hydrochloric acid as detergent, boron-rich organic faciess are 1 with detergent flow ratio:20
～30,3 stage countercurrent washings are carried out in 25 DEG C, the boron-rich organic faciess after washing impurity-removing is obtained after split-phase, with 0.5～1mol/l hydrogen-oxygens
Change sodium solution is back washing agent, and the boron-rich organic faciess after washing impurity-removing are 5～10 with back washing agent flow ratio:1, carry out reacting in 25 DEG C
To four water eight borate two sodium solution, wherein 20～40g/l of boron element mass concentration, boron sodium element mass ratio is 1.85～1.9, on
State four water eight borate two sodium solution be dried at 140 DEG C, make powder after obtain four water eight borate two sodium, in product, boron content exists
20%～20.5%, the impurity metal ion content such as ferrum is in below 10ppm.
Specific embodiment 2
Alcohol kind of extractants is constituted from sulfonated kerosene from isooctanol and 2- ethyls -1,3 hexanediol compound systems, diluent
Extraction organic faciess, isooctanol account for volume ratio 10%～50% in extraction organic faciess, and 2- ethyls -1,3 hexanediol are organic in extraction
Volume ratio 10%～50% is accounted in phase, sulfonated kerosene accounts for volume ratio 50%～70% in extraction organic faciess.
3mol/l sulfuric acid solutions are added in 1 part of liquid boron rock, is reacted to solution ph≤2, above-mentioned solution is filtered
Boric acid solid and acidifying carry boron liquid, and the flow ratio that extraction organic faciess agent carries boron liquid with acidifying is 1：1～2,3 stage countercurrents are carried out in 25 DEG C
Extraction, obtains boron-rich organic faciess after split-phase, with 3mol/l hydrochloric acid as detergent, boron-rich organic faciess are 1 with detergent flow ratio:20～
30,3 stage countercurrent washings are carried out in 25 DEG C, the boron-rich organic faciess after washing impurity-removing is obtained after split-phase, with 0.5～1mol/l hydroxides
Sodium solution is back washing agent, and the boron-rich organic faciess after washing impurity-removing are 3～5 with back washing agent flow ratio:1, reaction is carried out in 25 DEG C obtain
Four water eight borate two sodium solution, wherein 20～40g/l of boron element mass concentration, boron sodium element mass ratio are 1.85～1.9, above-mentioned
Four water eight borate two sodium solution is dried at 140 DEG C, make powder after obtain four water eight borate two sodium, in product, boron content exists
20%～20.5%, the impurity metal ion content such as ferrum is in below 10ppm.
Specific embodiment 3
Alcohol kind of extractants selects isooctanol, diluent to have in extraction from sulfonated kerosene composition extraction organic faciess, isooctanol
Volume ratio 20%～50% is accounted in machine phase.
6mol/l hydrochloric acid solutions are added in 1 part of liquid boron rock, is reacted to solution ph≤2, above-mentioned solution is filtered
Boric acid solid and acidifying carry boron liquid, and the flow ratio that extraction organic faciess agent carries boron liquid with acidifying is 1：1～1.5, carry out in 25 DEG C 4 grades it is inverse
Stream extraction, obtains boron-rich organic faciess after split-phase, with 1mol/l hydrochloric acid as detergent, boron-rich organic faciess are 1 with detergent flow ratio:20
～30,3 stage countercurrent washings are carried out in 25 DEG C, the boron-rich organic faciess after washing impurity-removing is obtained after split-phase, with 1.5～2mol/l hydrogen-oxygens
Change sodium solution is back washing agent, and the boron-rich organic faciess after washing impurity-removing are 10～20 with back washing agent flow ratio:1, reacted in 50 DEG C
Four water eight borate two sodium solution, wherein 40～80g/l of boron element mass concentration are obtained, boron sodium element mass ratio is 1.85～1.9,
Above-mentioned four water eight borate two sodium solution is dried at 140 DEG C, make powder after obtain four water eight borate two sodium, boron content in product
20%～20.5%, the impurity metal ion content such as ferrum is in below 10ppm.
Claims (10)
1. a kind of method that utilization liquid boron rock synthesizes four water eight borate two sodium, it is characterised in that described synthetic method includes
Following steps：
The acidifying of liquid boron rock carries boron and obtains acidifying and carries boron liquid, and alcohol kind of extractants and diluent are mixed to get extraction organic faciess, acid
Change carries boron liquid and carries out multi-stage counter current extraction with extraction organic faciess at normal temperatures, obtains richness by esterification of the extractant with boric acid
Boron organic faciess, boron-rich organic faciess adopt acidity 0～12M acidity solution washing impurity-removings, the boron-rich organic faciess after washing impurity-removing with it is anti-
Extraction agent sodium hydroxide solution mixing, carries out back extraction, by controlling concentration of sodium hydroxide solution and flow ratio, makes boron-rich organic under stirring
The hydrolysis reaction of phase borate is coupled with the synthetic reaction process of four water eight borate two sodium, directly obtains strip liquor, and Jing does
It is dry to make i.e. prepared four water eight borate two sodium after powder.
2. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 1, it is characterised in that the liquid
Body boron rock is boracic salt lake bittern, and boric acid total concentration is 1g/l～60g/l, and magnesium ion concentration is 60g/l～120g/l.
3. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 1, it is characterised in that the alcohol
Kind of extractants is unitary fatty alcohol, binary aliphatic alcohol, aromatic alcohol or its combination.
4. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 1, it is characterised in that described dilute
It is one or more in No. 200 industrial napthas, kerosene, benzene,toluene,xylenes or derivatives thereof to release agent.
5. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 4, it is characterised in that described dilute
Agent is released for sulfonated kerosene.
6. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 1, it is characterised in that the acid
0～12M of degree acidity solutions are that mineral acid is prepared with pure water.
7. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 6, it is characterised in that the nothing
Machine acid is hydrochloric acid.
8. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 1, it is characterised in that described
Acidifying puies forward the preparation method of boron liquid：To in liquid boron rock, inorganic acid solution is added to react to pH value≤2 of solution, filtration is
.
9. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 1, it is characterised in that described anti-
Extraction agent concentration of sodium hydroxide solution is 0.1～10mol/l, and stripping process organic faciess are 1 with back washing agent flow ratio:1～30:1, back extraction
10～100 DEG C of temperature.
10. the method for synthesizing four water eight borate two sodium using liquid boron rock according to claim 9, it is characterised in that described
Back washing agent concentration of sodium hydroxide solution is 0.5～2mol/l, and stripping process organic faciess are 1 with back washing agent flow ratio:1～30:1, instead
20～50 DEG C of temperature of extraction, in the strip liquor, boron sodium element mass ratio is 1.85～1.9, and in the strip liquor, boron element quality is dense
20～80g/l of degree.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113454025A (en) * | 2019-02-15 | 2021-09-28 | 雅宝公司 | Method for extracting boron from organic solutions |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113454025A (en) * | 2019-02-15 | 2021-09-28 | 雅宝公司 | Method for extracting boron from organic solutions |
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| CN106587090B (en) | 2018-11-13 |
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