CN106698372A - Wet-process phosphoric acid defluorination method - Google Patents
Wet-process phosphoric acid defluorination method Download PDFInfo
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- 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
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- Prior art keywords
- phosphoric acid
- wet process
- defluorination
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- defluorination method
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 238000000034 method Methods 0.000 title claims abstract description 101
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 78
- 238000006115 defluorination reaction Methods 0.000 title claims abstract description 46
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 39
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 12
- 239000011737 fluorine Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000004062 sedimentation Methods 0.000 claims description 19
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229940084030 carboxymethylcellulose calcium Drugs 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- -1 polyoxyethylene Polymers 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 241000047703 Nonion Species 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000003945 anionic surfactant Substances 0.000 claims description 4
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 125000001153 fluoro group Chemical group F* 0.000 claims 2
- 150000002500 ions Chemical class 0.000 claims 2
- 239000004743 Polypropylene Substances 0.000 claims 1
- 229920001155 polypropylene Polymers 0.000 claims 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 10
- 239000007787 solid Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000006228 supernatant Substances 0.000 abstract 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000005871 repellent Substances 0.000 description 4
- 230000002940 repellent Effects 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 235000010980 cellulose Nutrition 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000661 sodium alginate Substances 0.000 description 2
- 235000010413 sodium alginate Nutrition 0.000 description 2
- 229940005550 sodium alginate Drugs 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000001648 tannin Substances 0.000 description 2
- 235000018553 tannin Nutrition 0.000 description 2
- 229920001864 tannin Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MPPQGYCZBNURDG-UHFFFAOYSA-N 2-propionyl-6-dimethylaminonaphthalene Chemical compound C1=C(N(C)C)C=CC2=CC(C(=O)CC)=CC=C21 MPPQGYCZBNURDG-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- FYHXNYLLNIKZMR-UHFFFAOYSA-N calcium;carbonic acid Chemical compound [Ca].OC(O)=O FYHXNYLLNIKZMR-UHFFFAOYSA-N 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 229940105329 carboxymethylcellulose Drugs 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
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 |
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| 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 |
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| Country | Link |
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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 | Defluorination method of high-content sesquioxide wet-process phosphoric acid |
| 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 | Defluorination method of high-content sesquioxide wet-process phosphoric acid |
| 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 |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170524 |