CN106698372A - Wet-process phosphoric acid defluorination method - Google Patents
Wet-process phosphoric acid defluorination method Download PDFInfo
- Publication number
- CN106698372A CN106698372A CN201510784981.8A CN201510784981A CN106698372A CN 106698372 A CN106698372 A CN 106698372A CN 201510784981 A CN201510784981 A CN 201510784981A CN 106698372 A CN106698372 A CN 106698372A
- Authority
- CN
- China
- Prior art keywords
- phosphoric acid
- wet process
- defluorination
- parts
- defluorination method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a wet-process phosphoric acid defluorination method. Under the temperature of 30-40 DEG C, a defluorination agent is added to wet-process phosphoric acid, stirring is performed for 1.5-2.5 hours, then a settlement agent is added, settlement is performed for 10-15 hours, and filtration is performed. The wet-process phosphoric acid defluorination method is high in defluorination efficiency, the highest defluorination efficiency can be up to 92%, the fluorine content in the phosphoric acid is low, the lowest fluorine content is 0.24 g/L, a defluorination effect is good, the solid content of obtained phosphoric acid supernatant is low, the lowest solid content is 0.25%, the fluorine removal rate is as high as 92%, and the process is simple.
Description
Technical field
The present invention relates to a kind of method of phosphoric acid defluorinate, particularly a kind of wet defluorination of phosphoric acid method of defluorinate efficiency high.
Technical background
Wet method phosphoric acid manufacture process be with inorganic acid (mainly sulfuric acid) decomposing phosphate rock manufacture phosphoric acid process, i.e., with sulfuric acid with
Phosphorus ore reacts, and generates crystal of calcium sulfate and phosphoric acid solution, then carries out solid-liquor separation, and isolated phosphoric acid solution is referred to as wet method
Phosphoric acid.Mainly there are two water laws, half water law, hemi-dihydrate process in the source of phosphoric acid by wet process.Due to there is part fluorine-containing in phosphoric acid by wet process
Harmful substance (generally below 2%), it is impossible to phosphoric acid by wet process is directly made into deep processing production, therefore phosphoric acid by wet process must be carried out
Defluorinate is processed, and defluorinate treatment can obtain the relatively low purifying phosphoric acid of harmful substance and available fluorine-containing byproduct.
The method of country's wet defluorination of phosphoric acid purification and separation method generally filtering at present, can be because phosphoric acid viscosity when this method is separated
Greatly, solid particle is tiny and cause intensity filter to be greatly reduced in acid, causes filtration difficulty or cannot filter, and gained phosphoric acid
Middle Oil repellent is high, and generally higher than 0.5%, Oil repellent is also higher in phosphoric acid, generally higher than 2.0g/L, and defluorinate efficiency is low, fluorine removing
Rate is usually no more than 65%, and defluorination effect is poor.
The content of the invention：
It is an object of the present invention to provide a kind of method of wet defluorination of phosphoric acid.The inventive method defluorinate efficiency high, reaches as high as
92%, Oil repellent is low in phosphoric acid, and minimum 0.24g/L, defluorination effect is good, and the solid content of gained phosphoric acid clear liquid is low, minimum
0.25%, fluorine removal efficiency is up to 92%, and process is simple.
In order to solve the above technical problems, the present invention uses following technical scheme reality：A kind of defluorination method of phosphoric acid by wet process, at 30-40 DEG C
Under, to defluorinating agent is added in phosphoric acid by wet process, 1.5-2.5h is stirred, sedimentation agent is added, 10-15h is settled, filtering is obtained final product.
In the defluorination method of foregoing phosphoric acid by wet process, the mass fraction of contained phosphorus pentoxide is 30-40% in the phosphoric acid by wet process.
In the defluorination method of foregoing phosphoric acid by wet process, the mass fraction of the phosphorus pentoxide is 35%.
In the defluorination method of foregoing phosphoric acid by wet process, the addition of the defluorinating agent is 2-3 times of fluorine ion in phosphoric acid.
In the defluorination method of foregoing phosphoric acid by wet process, the addition of the defluorinating agent is 2.5 times of fluorine ion in phosphoric acid.
In the defluorination method of foregoing phosphoric acid by wet process, defluorinating agent component by weight is calculated, containing sodium carbonate 1-1.5 parts, carbonic acid
Calcium 1.2-1.8 parts and silica 1 .5-2 parts.
In the defluorination method of foregoing phosphoric acid by wet process, defluorinating agent component by weight is calculated, 1.3 parts of containing sodium carbonate, calcium carbonate
1.5 parts and silica 1 .7 parts.
In the defluorination method of foregoing phosphoric acid by wet process, the sedimentation agent parts by weights calculates by flocculant in non-ion type 1-5 parts and cloudy
The ionic surface active agent 30-40 parts of concentration being configured to is the aqueous solution of 5-8%；The addition of the sedimentation agent is phosphoric acid by wet process body
Long-pending 0.5-0.9%.
In the defluorination method of foregoing phosphoric acid by wet process, the flocculant in non-ion type is polyoxyethylene, polyvinyl alcohol or polyacrylamide
Amine.
In the defluorination method of foregoing phosphoric acid by wet process, the anion surfactant be polyacrylate, carboxymethylcellulose calcium or
Dodecyl sodium sulfate.
Applicant has carried out substantial amounts of research to the method for wet defluorination of phosphoric acid, it is found by the applicant that adding surfactant, it is possible to decrease
The viscosity of raw phosphoric acid, allows flocculant fully to adsorb sludge particles, reaches the purpose of abundant sedimentation.Lived in selective flocculant and surface
Property agent collocation when, it is contemplated that raw phosphoric acid impurity is more, and viscosity is big and flocculant and the mutual influence factor of surfactant,
Selected in flocculant in non-ion type and anion surfactant, applicant previously select starch, tannin, cellulose,
Sodium Alginate, jar (unit of capacitance) glue and animal glue and gelatin, polyacrylamide and its derivative, carboxymethyl cellulose is used as flocculant, Shen
Ask someone to find, performance sedimentation is incomplete during these flocculants are used in phosphoric acid sedimentation, bottom liquid excessive height, it is impossible to the phosphorus clarified
Acid.Applicant has found by substantial amounts of experimental study, from polyoxyethylene, polyvinyl alcohol or polyacrylamide as flocculant；
From polyacrylate, carboxymethylcellulose calcium or dodecyl sodium sulfate as surfactant, flocculant and surface-active are controlled
The quality proportioning of agent is 1-5：30-40, be made into mass concentration for 5%~8% aqueous solution as sedimentation agent, for being taken off
During fluorine, defluorinate efficiency high reaches as high as 90%, and defluorination effect is good, and the prodan purity of production is high, up to 80%.
Applicant carried out following experiments, the provable present invention has effective effect；
Experimental example：Defluorinate rate is investigated
Defluorination process 1：Defluorinate is carried out as described in Example 1.
Defluorination process 2：Defluorinate is carried out as described in Example 2.
Defluorination process 3：Defluorinate is carried out as described in Example 3.
Defluorination process 4：That is existing process, at 10-30 DEG C, to calcium carbonate is added in phosphoric acid by wet process, stirs, add starch,
Tannin, cellulose, Sodium Alginate and carboxymethylcellulose calcium, settle 20h, and filtering is obtained final product.
The phosphoric acid obtained by above-mentioned technique is taken respectively is detected that testing result is shown in Table 1：
The testing result of table 1
As seen from table, when present invention process carries out defluorinate to phosphoric acid by wet process, the solid content of the phosphoric acid clear liquid of gained is less than existing defluorinate
Technique (i.e. defluorination process 4), the solid content of phosphoric acid clear liquid is minimum up to 0.25%.Fluorine contains in the phosphoric acid obtained by present invention process simultaneously
Amount is minimum, less than defluorination process 4, in addition, the defluorinate rate of present invention process is higher, to reach as high as 92% up to 0.24g/L, than
Existing defluorination process is higher by 32%.
Compared with prior art, the inventive method defluorinate efficiency high, reaches as high as 92%, and Oil repellent is low in phosphoric acid, minimum
0.24g/L, defluorination effect is good, and the solid content of gained phosphoric acid clear liquid is low, and minimum 0.25%, fluorine removal efficiency is up to 92%, and
Process is simple.
Specific embodiment：
Embodiment 1：
A kind of defluorination method of phosphoric acid by wet process：At 30-40 DEG C, in the phosphoric acid by wet process that the mass fraction of phosphorus pentoxide is 35%
Defluorinating agent is added, 2h is stirred, sedimentation agent is added, 13h is settled, filtering is obtained final product；The addition of the defluorinating agent is phosphoric acid
2.5 times of middle fluorine ion；The defluorinating agent containing sodium carbonate 1.3g, calcium carbonate 1.5g and silica 1 .7g；The sedimentation agent
The concentration being configured to by polyoxyethylene 2.5g and dodecyl sodium sulfate 35g is 6.5% aqueous solution；The addition of the sedimentation agent
Measure is the 0.7% of phosphoric acid by wet process volume.
Embodiment 2：
A kind of defluorination method of phosphoric acid by wet process, at 30-40 DEG C, in the phosphoric acid by wet process that the mass fraction of phosphorus pentoxide is 30%
Defluorinating agent is added, 2.5h is stirred, sedimentation agent is added, 15h is settled, filtering is obtained final product；The addition of the defluorinating agent is phosphorus
3 times of fluorine ion in acid；The defluorinating agent containing sodium carbonate 1.5g, calcium carbonate 1.8g and silica 2g；The sedimentation agent by
The concentration that polyvinyl alcohol 5g and carboxymethylcellulose calcium 40g are configured to is 8% aqueous solution；The addition of the sedimentation agent is wet method
The 0.9% of phosphoric acid volume.
Embodiment 3：
A kind of defluorination method of phosphoric acid by wet process, at 30-40 DEG C, in the phosphoric acid by wet process that the mass fraction of phosphorus pentoxide is 40%
Defluorinating agent is added, 1.5h is stirred, sedimentation agent is added, 10h is settled, filtering is obtained final product；The addition of the defluorinating agent is phosphorus
2 times of fluorine ion in acid；The defluorinating agent containing sodium carbonate 1g, calcium carbonate 1.2g and silica 1 .5g；The sedimentation agent by
The concentration that polyvinyl alcohol 1g and carboxymethylcellulose calcium 30g are configured to is 5% aqueous solution；The addition of the sedimentation agent is wet method
The 0.5% of phosphoric acid volume.
Claims (10)
1. a kind of defluorination method of phosphoric acid by wet process, it is characterised in that：At 30-40 DEG C, to defluorinating agent is added in phosphoric acid by wet process, stir
1.5-2.5h, adds sedimentation agent, settles 10-15h, and filtering is obtained final product.
2. the defluorination method of phosphoric acid by wet process as claimed in claim 1, it is characterised in that：Contained phosphorus pentoxide in the phosphoric acid by wet process
Mass fraction be 30-40%.
3. the defluorination method of phosphoric acid by wet process as claimed in claim 2, it is characterised in that：The mass fraction of the phosphorus pentoxide is 35%.
4. the defluorination method of phosphoric acid by wet process as claimed in claim 1, it is characterised in that：The addition of the defluorinating agent is fluorine in phosphoric acid
2-3 times of ion.
5. the defluorination method of phosphoric acid by wet process as claimed in claim 4, it is characterised in that：The addition of the defluorinating agent is fluorine in phosphoric acid
2.5 times of ion.
6. the defluorination method of phosphoric acid by wet process as claimed in claim 1, it is characterised in that：Defluorinating agent component by weight is calculated, and is contained
Sodium carbonate 1-1.5 parts, calcium carbonate 1.2-1.8 parts and silica 1 .5-2 parts.
7. the defluorination method of phosphoric acid by wet process as claimed in claim 6, it is characterised in that：Defluorinating agent component by weight is calculated, and is contained
1.3 parts of sodium carbonate, 1.5 parts and silica 1 .7 parts of calcium carbonate.
8. the defluorination method of phosphoric acid by wet process as claimed in claim 1, it is characterised in that：The sedimentation agent parts by weights calculate by it is non-from
1-5 parts and anion surfactant 30-40 parts concentration being configured to of subtype flocculant is the aqueous solution of 5-8%；The sedimentation agent
Addition for phosphoric acid by wet process volume 0.5-0.9%.
9. the defluorination method of phosphoric acid by wet process as claimed in claim 8, it is characterised in that：The flocculant in non-ion type be polyoxyethylene,
Polyvinyl alcohol or polyacrylamide.
10. the defluorination method of phosphoric acid by wet process as claimed in claim 8, it is characterised in that：The anion surfactant is polypropylene
Hydrochlorate, carboxymethylcellulose calcium or dodecyl sodium sulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510784981.8A CN106698372A (en) | 2015-11-16 | 2015-11-16 | Wet-process phosphoric acid defluorination method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510784981.8A CN106698372A (en) | 2015-11-16 | 2015-11-16 | Wet-process phosphoric acid defluorination method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106698372A true CN106698372A (en) | 2017-05-24 |
Family
ID=58931556
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510784981.8A Pending CN106698372A (en) | 2015-11-16 | 2015-11-16 | Wet-process phosphoric acid defluorination method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106698372A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726496A (en) * | 2018-08-03 | 2018-11-02 | 禄丰天宝磷化工有限公司 | A kind of defluorination method of high-content sesquichloride phosphoric acid by wet process |
| CN110980675A (en) * | 2019-12-30 | 2020-04-10 | 南京乐透思环保科技有限公司 | Defluorination method of wet-process phosphoric acid |
-
2015
- 2015-11-16 CN CN201510784981.8A patent/CN106698372A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726496A (en) * | 2018-08-03 | 2018-11-02 | 禄丰天宝磷化工有限公司 | A kind of defluorination method of high-content sesquichloride phosphoric acid by wet process |
| CN110980675A (en) * | 2019-12-30 | 2020-04-10 | 南京乐透思环保科技有限公司 | Defluorination method of wet-process phosphoric acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102887535A (en) | Method for recycling high-purity fluorine and phosphorus from wastewater of phosphogypsum residue field | |
| CN101724756A (en) | Phosphorus and silicon removing method of vanadium-contained clinker leaching liquor | |
| CN102730721B (en) | Recovering method of by-product sodium chloride in polyphenylene sulfide production | |
| CN109795995B (en) | Method for efficiently removing impurities from phosphoric acid by hydrochloric acid wet process | |
| WO2013020428A1 (en) | Phosphorus chemical wastewater treatment method | |
| CN106830244A (en) | A kind of method that fluorine and acid are separated and recovered from acidic fluoride-containing waste water | |
| CN104843789A (en) | Method for purifying vanadium pentoxide | |
| CN106698372A (en) | Wet-process phosphoric acid defluorination method | |
| CN110330042B (en) | Deep impurity removal method for calcium-removing refined liquid in fly ash one-step acid dissolution process | |
| RU2634948C1 (en) | Method for acid processing of lean phosphate raw materials | |
| CN103014377B (en) | Vanadium liquid purification method | |
| CN108862517B (en) | Process for co-producing heavy metal treatment coagulant by using phosphogypsum and red mud to prepare acid | |
| CN107739121A (en) | A kind of further treatment technique of fluorine-containing silicon waste water | |
| CN103818940A (en) | Method for decalcifying aluminum chloride and method for extracting aluminum oxide from coal ash | |
| CN101709377B (en) | Purifying and impurity-removing method of leaching solution containing vanadium | |
| JP2017043503A (en) | Method of producing gypsum and method of producing cement composition | |
| CN104828795A (en) | Wet phosphoric acid production process through ceramic membrane method | |
| CN109809377A (en) | A kind of method of sulfuric acid process phosphoric acid by wet process efficient impurity removal | |
| CN112158977B (en) | Treatment method of triphenylphosphine oxide-containing wastewater | |
| CN109502826A (en) | A kind of processing method of fluoride waste | |
| TWI694057B (en) | Method for manufacturing gypsum and method for manufacturing cement composition | |
| CN112095025A (en) | Method for removing silicon and phosphorus from blank roasting-ammonia leaching vanadium liquid | |
| JP5167448B2 (en) | Method for removing calcium and magnesium ions in water | |
| CN106904585B (en) | A kind of diluted acid de-magging slurry processing method | |
| CN103803520A (en) | Production method for feed-grade calcium monohydrogenphosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170524 |