CN109110775A - A method of the preparing boracic acid from boron rock - Google Patents
A method of the preparing boracic acid from boron rock Download PDFInfo
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- CN109110775A CN109110775A CN201811344855.0A CN201811344855A CN109110775A CN 109110775 A CN109110775 A CN 109110775A CN 201811344855 A CN201811344855 A CN 201811344855A CN 109110775 A CN109110775 A CN 109110775A
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- acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01B35/1045—Oxyacids
- C01B35/1054—Orthoboric acid
- C01B35/1063—Preparation from boron ores or borates using acids or salts
Abstract
The method of the invention discloses a kind of from boron rock preparing boracic acid, include the steps that being followed successively by ore crushing, acidolysis, it filters for the first time, first order purification, second of filtering, concentration, crystallization, it is centrifuged for the first time, FLOTATION SEPARATION, second of centrifugation, freeze-drying, boric acid product is made, it is characterized in that, it is filtered at second and increases second level purification between concentration, the second level purification uses organic complexing agent chelated iron ion and aluminium ion, the organic complexing agent is for precipitating iron ion and aluminium ion, form iron-organic complex sediment and aluminium-organic complex sediment.This method can effectively remove iron ion, eliminate influence of the iron ion to boric acid finished product gloss, simple process, strong operability, the cyclic utilization rate of filtrate are high, at low cost, boric acid recovery rate is high.
Description
Technical field
The present invention relates to boric acid extractive technique field, in particular to a kind of method of the preparing boracic acid from boron rock.
Background technique
The method of domestic preparing boracic acid mainly uses sulfuric acid process to decompose magnesium mine production boric acid, and technical process is boron magnesium
Miberal powder is broken → and miberal powder adds sulfuric acid and water acidification → filtering removal filter residue → crystallisation by cooling → centrifuge separation discharge mother liquor, receives to obtain wet boron
Acid → with water washing, boric acid product is made in → centrifugation dries → after drying.Mother liquor is finally discharged away, may be contained in mother liquor
The impurity such as heavy metal, concentrated acid, direct emission will cause environmental pollution, and will cause being largely lost for boron, reduce boric acid
Recovery rate.
It is most of to generate phase after containing the impurity, with effect of sulfuric acid such as iron, aluminium in boron rock in boric acid producing process
The salt answered, is finally present in finished product with boric acid together.The especially presence and accumulation of iron ion, can seriously affect product
Appearance and inherent quality.Can make to generate when iron is exceeded boric acid color is gloomy, purity is low.The presence of iron ion can make boric acid
And Adlerika is in reddish yellow or bronzing, it not only influences boric acid and the color of sulfuric acid magnesium products can also be to boric acid and sulfuric acid
Magnesium crystallization has very big obstruction.
CN200910058548.0 discloses a kind of industrial waste adsorbent for the cerium sulphate crystal of boric acid production and brightens
Control method uses acticarbon to adsorb iron ion, but the at high cost of active carbon adsorption decoloration, dosage are big, and not
It can be recycled, operability is not strong, is restricted industrial applications.
Summary of the invention
The technical problem to be solved by the present invention is overcoming the deficiencies of the prior art and provide one kind preparing boracic acid from boron rock
Method, this method can effectively remove iron ion, and simple process, strong operability, the cyclic utilization rate of filtrate be high, cost
Low, boric acid recovery rate height.
The technical solution adopted by the present invention to solve the technical problems is: a method of the preparing boracic acid from boron rock, it should
Method include the steps that being followed successively by ore crushing, acidolysis, filtering for the first time, first order purification, second of filtering, concentration, crystallization,
FLOTATION SEPARATION, second of centrifugation, freeze-drying, boric acid product is made in centrifugation for the first time, filters at second and increases between concentration
Second level purification is added, the second level purification uses organic complexing agent chelated iron ion and aluminium ion, the organic complexing agent
For precipitating iron ion and aluminium ion, iron-organic complex sediment and aluminium-organic complex sediment are formed.
Preferably, the degree of grinding that ore crushes is 200-300 mesh, makes miberal powder sufficiently and sulfuric acid contact, increases miberal powder and sulphur
The contact area of acid, improves the recovery rate of boric acid.
Further, third time filtering is carried out after second of purification, the filtered filter residue of third time is stripped using hydrochloric acid
The iron-organic complex sediment and aluminium-organic complex sediment are taken, organic complexing agent is entered the after separating in sediment
Secondary purification process cycles use.By back extraction iron-organic complex sediment and aluminium-organic complex sediment, keep iron-organic
Complex precipitate and iron ion in aluminium-organic complex sediment and aluminium ion are separated with organic complexing agent, and extraction stands liquid separation,
Organic complexing agent after liquid separation is returned into chelated iron ion and aluminium ion in first order purification again, obtains organic complexing agent
It is recycled, reduces the extraction cost of boric acid.
Further, the organic complexing agent is mixed by volume for 1:1 by four sodium of iminodisuccinic acid with 8-hydroxyquinoline
Conjunction is prepared.
Further, the concentration of four sodium of iminodisuccinic acid and 8-hydroxyquinoline be 20-30%, the organic complexing agent with
Second of filtered filtrate volume ratio is 1:20-30, and the reaction time of the complexing is 3-5min, reaction temperature 30-40
℃。
Further, the step of acidolysis: being that sulfuric acid, side is added in 1:2-3 at room temperature by the solid-liquid ratio of miberal powder and sulfuric acid
Stirring side adds sulfuric acid, then increases temperature, is 90-100 DEG C of acidolysis 1-2h in temperature, the pH of acidolysis is 4-5.
Filtering after acidolysis by first time can remove Ca2+, it is rinsed with water filter residue, makes to be attached to the boron of precipitation surface in filter residue
Acid is rinsed into flushing liquor, then flushing liquor is returned to acidolysis process, further extracts, the recovery rate of boric acid can be improved.
Further, the step of first order purifies are as follows: by filtered filtrate for the first time and hydrogen peroxide, vulcanized sodium
Volume ratio is that hydrogen peroxide and vulcanized sodium is added in 1:2-3, reacts 10-15min at being 90-100 DEG C in temperature, the vulcanized sodium
Concentration is 30-40%.It is purified by the first order and removes the heavy metal ion such as manganese, arsenic.
Contain manganese sulfide, arsenones and part iron hydroxide, aluminium hydroxide, sediment in second of filtered filter residue,
It is rinsed with water filter residue again, the boric acid for being attached to precipitation surface can be made to be flushed into flushing liquor, then flushing liquor is returned to acidolysis process,
It further extracts, the recovery rate of boric acid can be improved.
Further, the temperature of the concentration is 60-80 DEG C, and the volume after concentration is the 1/2-1/3 of original volume.
Further, the time of the crystallization is 3-16h, and crystallization temperature is 10-20 DEG C.
Further, the FLOTATION SEPARATION is passed through air flotation using flotation device, and the revolving speed of the flotation device is 2000-
2300r/s, the content of air are 8L/min~10L/min, and the flotation time is 10-15min.
Boric acid crystal after FLOTATION SEPARATION is rinsed with water, make the uncrystallized boric acid for being attached to boric acid plane of crystal rinse to
In flushing liquor, then eluent returned into acidolysis process, further extracts, the recovery rate of boric acid can be improved.
The MgSO obtained after FLOTATION SEPARATION4Crystal carries out third time centrifugation, makes to be attached to MgSO4Uncrystallized boron on crystal
Acid is transferred in centrifugate, then centrifugate is returned to concentration, crystallization processes, after being centrifuged by first time centrifugation and second from
Heart liquid also all returns to concentration, crystallization processes, further crystallizes, to improve the recovery rate of boric acid.
Further, the temperature of the freeze-drying is 20-30 DEG C.
A kind of method of the preparing boracic acid from boron rock of the present invention the utility model has the advantages that the present invention by acidolysis, purification for the first time,
Purify, be filtered for multiple times and be centrifuged for the second time, be concentrated, crystallizing, freeze-drying prepares boric acid, iron ions are gone using organic complexing agent
And aluminium ion, and organic complexing agent repetitive cycling is used, the extraction cost of boric acid is reduced, the gloss of boric acid product is improved
And quality, flushing liquor throughout the extraction process have carried out repeating to extract again, improve the recovery rate of boric acid, and reach
Zero emission standards, it is free from environmental pollution.
Detailed description of the invention
Fig. 1-is a kind of method flow diagram of the preparing boracic acid from boron rock of the present invention.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and embodiments, but these specific embodiments are not with any side
Formula limits the scope of the invention.
Embodiment 1
A method of the preparing boracic acid from boron rock, include the following:
(1) ore crushes: use mineral breaker that ore is crushed to degree of grinding as 300 mesh, according to solid-liquid ratio for 1:3 to
70% sulfuric acid is added in miberal powder, sulfuric acid is added while stirring, increases temperature, acidolysis 1.5h at being 90 DEG C in temperature, the pH of acidolysis are
4；First time filtering is carried out after acidolysis, filtered filtrate enters in subsequent processing for the first time, what filter residue was formed after being rinsed with water
Flushing liquor returns to further acidolysis in acid hydrolysis solution；
(2) first order purifies: being separately added into the hydrogen peroxide and concentration of 2 times of volumes into step (1) filtrate as 30% vulcanization
Sodium reacts 12min at being 90 DEG C in temperature, is deposited manganese, arsenic and part aluminium ion and iron ion in filtrate；The first order is net
It carries out filtering for second after change, second of filtered filtrate enters in subsequent processing, the flushing that filter residue is formed after being rinsed with water
Liquid returns to further acidolysis in acid hydrolysis solution；
(3) second level purifies: four sodium of iminodisuccinic acid and 8-hydroxyquinoline that concentration is 20% has been respectively configured, according to body
Product is 1:20 addition by the volume ratio of organic complexing agent and step (2) filtrate than being that organic complexing agent is made in 1:1 after mixing
5min is complexed at being 30 DEG C in temperature in organic complexing agent, makes iron ion and aluminium ion and organic complexing agent complexing at the organic network of iron-
Close sediment and aluminium-organic complex sediment；Third time filtering is carried out after complexing, the filtered filtrate of third time enters next
Process, filter hydrochloric acid for dreg back extraction iron-organic complex sediment and aluminium-organic complex sediment, make iron ion and aluminium ion with
Organic complexing agent separation, stands liquid separation after extraction, and isolated organic complexing agent is put back in the purification of the second level, network can be recycled
Close iron ion and aluminium ion；
(4) it is concentrated, crystallizes: being concentrated by evaporation at being 80 DEG C in temperature by the filtrate in step (3) to the 1/3 of original volume, then will be dense
10h is crystallized at 10 DEG C after the cooling of contracting liquid, obtains the crystallization of boron magnesium and boric acid magma.After being centrifuged using first time, by what is obtained
Centrifugate returns to further concentration, and the boron magnesium crystallization after centrifugation is entered in subsequent processing；
(5) FLOTATION SEPARATION: carrying out FLOTATION SEPARATION with flotation device for obtained boron magnesium crystallization, is 2300r/s, sky in flotation device revolving speed
Gas content is flotation 10min under 10L/min, makes boric acid crystallization and magnesium sulfate Crystallization Separation, obtained antifungin is crystallized and is carried out
Third time is centrifuged, and centrifugate is returned to further concentration；
(6) it is centrifuged for second: boric acid crystallization being rinsed with water after forming flushing liquor, flushing liquor standing and returned it into acidolysis into one
Acidolysis is walked, then a small amount of flushing liquor boric acid crystallization will be contained and carry out second of centrifugation, centrifugate is returned into further concentration；
(7) be freeze-dried: freeze-drying is at the boric acid crystallization that centrifugation is obtained is 20 DEG C in temperature to get boric acid finished product.
Embodiment 2
A method of the preparing boracic acid from boron rock, include the following:
(1) ore crushes: using mineral breaker that ore is crushed to degree of grinding as 200 mesh, is 1:2 to miberal powder according to solid-liquid ratio
Sulfuric acid is added in 80% sulfuric acid of middle addition while stirring, increases temperature, and acidolysis 1h at being 100 DEG C in temperature, the pH of acidolysis are 5；Acid
First time filtering is carried out after solution, filtered filtrate enters in subsequent processing for the first time, the flushing that filter residue is formed after being rinsed with water
Liquid returns to further acidolysis in acid hydrolysis solution；
(2) first order purifies: being separately added into the hydrogen peroxide and concentration of 3 times of volumes into step (1) filtrate as 40% vulcanization
Sodium reacts 10min at being 100 DEG C in temperature, is deposited manganese, arsenic and part aluminium ion and iron ion in filtrate；The first order
It carries out filtering for second after purification, second of filtered filtrate enters in subsequent processing, and what filter residue was formed after being rinsed with water rushes
Washing lotion returns to further acidolysis in acid hydrolysis solution；
(3) second level purifies: four sodium of iminodisuccinic acid and 8-hydroxyquinoline that concentration is 30% has been respectively configured, according to body
Product is 1:30 addition by the volume ratio of organic complexing agent and step (2) filtrate than being that organic complexing agent is made in 1:1 after mixing
3min is complexed at being 40 DEG C in temperature in organic complexing agent, makes iron ion and aluminium ion and organic complexing agent complexing at the organic network of iron-
Close sediment and aluminium-organic complex sediment；Third time filtering is carried out after complexing, the filtered filtrate of third time enters next
Process, filter hydrochloric acid for dreg back extraction iron-organic complex sediment and aluminium-organic complex sediment, make iron ion and aluminium ion with
Organic complexing agent separation, stands liquid separation after extraction, and isolated organic complexing agent is put back in the purification of the second level, benefit is recycled
With chelated iron ion and aluminium ion；
(4) it is concentrated, crystallizes: being concentrated by evaporation at being 60 DEG C in temperature by the filtrate in step (3) to the 1/2 of original volume, then will be dense
16h is crystallized at 20 DEG C after the cooling of contracting liquid, obtains the crystallization of boron magnesium and boric acid magma.After being centrifuged using first time, by what is obtained
Centrifugate returns to further concentration, and the boron magnesium crystallization after centrifugation is entered in subsequent processing；
(5) FLOTATION SEPARATION: carrying out FLOTATION SEPARATION with flotation device for obtained boron magnesium crystallization, is 2000r/s, sky in flotation device revolving speed
Gas content is flotation 15min under 8L/min, makes boric acid crystallization and magnesium sulfate Crystallization Separation, and the crystallization of obtained antifungin is carried out the
It is centrifuged three times, centrifugate is returned into further concentration；
(6) it is centrifuged for second: boric acid crystallization being rinsed with water after forming flushing liquor, flushing liquor standing and returned it into acidolysis into one
Acidolysis is walked, then a small amount of flushing liquor boric acid crystallization will be contained and carry out second of centrifugation, centrifugate is returned into further concentration；
(7) be freeze-dried: freeze-drying is at the boric acid crystallization that centrifugation is obtained is 30 DEG C in temperature to get boric acid finished product.
Embodiment 3
A method of the preparing boracic acid from boron rock, include the following:
(1) ore crushes: using mineral breaker that ore is crushed to degree of grinding as 250 mesh, is 1:3 to miberal powder according to solid-liquid ratio
Sulfuric acid is added in 75% sulfuric acid of middle addition while stirring, increases temperature, and acidolysis 1h at being 95 DEG C in temperature, the pH of acidolysis are 4；Acidolysis
First time filtering is carried out afterwards, and filtered filtrate enters in subsequent processing for the first time, the flushing liquor that filter residue is formed after being rinsed with water
Return to further acidolysis in acid hydrolysis solution；
(2) first order purifies: being separately added into the hydrogen peroxide and concentration of 2 times of volumes into step (1) filtrate as 35% vulcanization
Sodium reacts 10min at being 95 DEG C in temperature, is deposited manganese, arsenic and part aluminium ion and iron ion in filtrate；The first order is net
It carries out filtering for second after change, second of filtered filtrate enters in subsequent processing, the flushing that filter residue is formed after being rinsed with water
Liquid returns to further acidolysis in acid hydrolysis solution；
(3) second level purifies: four sodium of iminodisuccinic acid and 8-hydroxyquinoline that concentration is 25% has been respectively configured, according to body
Product is 1:25 addition by the volume ratio of organic complexing agent and step (2) filtrate than being that organic complexing agent is made in 1:1 after mixing
3min is complexed at being 35 DEG C in temperature in organic complexing agent, makes iron ion and aluminium ion and organic complexing agent complexing at the organic network of iron-
Close sediment and aluminium-organic complex sediment；Third time filtering is carried out after complexing, the filtered filtrate of third time enters next
Process, filter hydrochloric acid for dreg back extraction iron-organic complex sediment and aluminium-organic complex sediment, make iron ion and aluminium ion with
Organic complexing agent separation, stands liquid separation after extraction, and isolated organic complexing agent is put back in the purification of the second level, network can be recycled
Close iron ion and aluminium ion；
(4) it is concentrated, crystallizes: being concentrated by evaporation at being 70 DEG C in temperature by the filtrate in step (3) to the 1/3 of original volume, then will be dense
12h is crystallized at 15 DEG C after the cooling of contracting liquid, obtains the crystallization of boron magnesium and boric acid magma.After being centrifuged using first time, by what is obtained
Centrifugate returns to further concentration, and the boron magnesium crystallization after centrifugation is entered in subsequent processing；
(5) FLOTATION SEPARATION: carrying out FLOTATION SEPARATION with flotation device for obtained boron magnesium crystallization, is 2200r/s, sky in flotation device revolving speed
Gas content is flotation 10min under 9/min, makes boric acid crystallization and magnesium sulfate Crystallization Separation, and the crystallization of obtained antifungin is carried out the
It is centrifuged three times, centrifugate is returned into further concentration；
(6) it is centrifuged for second: boric acid crystallization being rinsed with water after forming flushing liquor, flushing liquor standing and returned it into acidolysis into one
Acidolysis is walked, then a small amount of flushing liquor boric acid crystallization will be contained and carry out second of centrifugation, centrifugate is returned into further concentration；
(7) be freeze-dried: freeze-drying is at the boric acid crystallization that centrifugation is obtained is 25 DEG C in temperature to get boric acid finished product.
The present invention is measured the boric acid recovery rate in embodiment 1-3, and measurement result is as shown in the table:
The result of 1 boric acid recovery rate of table
As seen from the above table, reach 80% using the recovery rate that method of the invention extracts boric acid, recovery rate with higher.
Claims (10)
1. a kind of method of the preparing boracic acid from boron rock, include the steps that being followed successively by ore crushing, acidolysis, for the first time filtering, the
Second of filtering, concentration, crystallization, centrifugation for the first time, FLOTATION SEPARATION, second of centrifugation, freeze-drying, boron is made in first class purification
Acid product, which is characterized in that second level purification is increased between concentration filtering for the second time, the second level purification, which uses, to be had
Machine complexing agent chelated iron ion and aluminium ion, the organic complexing agent form the organic network of iron-for precipitating iron ion and aluminium ion
Close sediment and aluminium-organic complex sediment.
2. a kind of method of the preparing boracic acid from boron rock as described in claim 1, which is characterized in that it is described purify for the second time it is laggard
Row third time filters, and the filtered filter residue of third time is stripped the iron-organic complex sediment and the organic network of aluminium-using hydrochloric acid
Sediment is closed, organic complexing agent is entered to second level purification process after separating in sediment and is recycled.
3. a kind of method of the preparing boracic acid from boron rock as described in claim 1, which is characterized in that the organic complexing agent is by Asia
Four sodium of amino disuccinic acid is that 1:1 is mixed with 8-hydroxyquinoline by volume.
4. a kind of method of the preparing boracic acid from boron rock as claimed in claim 3, which is characterized in that the iminodisuccinic acid
The concentration of four sodium and 8-hydroxyquinoline is 20-30%, and the organic complexing agent is 1 with second of filtered filtrate volume ratio:
20-30, the reaction time of the complexing are 3-5min, and reaction temperature is 30-40 DEG C.
5. a kind of method of the preparing boracic acid from boron rock as described in claim 1, which is characterized in that the step of the acidolysis: pressing
The solid-liquid ratio of miberal powder and sulfuric acid is that sulfuric acid is added in 1:2-3 at room temperature, while stirring plus sulfuric acid, then increases temperature, is in temperature
90-100 DEG C of acidolysis 1-2h, the pH of acidolysis are 4-5.
6. a kind of method of the preparing boracic acid from boron rock as described in claim 1, which is characterized in that the step of the first order purification
Suddenly are as follows: the volume ratio by filtered filtrate for the first time and hydrogen peroxide, vulcanized sodium is that hydrogen peroxide and vulcanization is added in 1:2-3
Sodium, reacts 10-15min at being 90-100 DEG C in temperature, the concentration of the vulcanized sodium is 30-40%.
7. a kind of method of the preparing boracic acid from boron rock as described in claim 1, which is characterized in that the temperature of the concentration is
60-80 DEG C, the volume after concentration is the 1/2-1/3 of original volume.
8. a kind of method of the preparing boracic acid from boron rock as described in claim 1, which is characterized in that the time of the crystallization is 3-
16h, crystallization temperature are 10-20 DEG C.
9. a kind of method of the preparing boracic acid from boron rock as described in claim 1, which is characterized in that the FLOTATION SEPARATION is using floating
Machine is selected to be passed through air flotation, the revolving speed of the flotation device is 2000-2300r/s, and the content of air is 8L/min~10L/min,
The flotation time is 10-15min.
10. a kind of method of the preparing boracic acid from boron rock as described in claim any one of 1-9, which is characterized in that the freezing
Dry temperature is 20-30 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112268414A (en) * | 2020-10-21 | 2021-01-26 | 衡阳市大宇锌业有限公司 | Prepare boric acid from boron ore and use freeze-drying device |
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| CN101575100A (en) * | 2009-06-18 | 2009-11-11 | 大连理工大学 | Method for removing metallic impurities in boric acid by complex crystallizing method |
| CN102963948A (en) * | 2012-12-14 | 2013-03-13 | 中国环境科学研究院 | Method for treating adamantanamined waste water through extraction method |
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| CN1130595A (en) * | 1995-03-03 | 1996-09-11 | 大连理工大学 | Comprehensive utilization method for decomposition of B-Mg-Fe ore with sulfuric acid |
| CN101209844A (en) * | 2006-12-31 | 2008-07-02 | 肖莹 | Technique for preparing high quality boric acid from salt lake type boron ore by one-step method |
| CN101575100A (en) * | 2009-06-18 | 2009-11-11 | 大连理工大学 | Method for removing metallic impurities in boric acid by complex crystallizing method |
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| CN112268414A (en) * | 2020-10-21 | 2021-01-26 | 衡阳市大宇锌业有限公司 | Prepare boric acid from boron ore and use freeze-drying device |
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