CN1022556C - Production of feed-grade calcium hydrogen phosphate by gravity floatation defluorination - Google Patents
Production of feed-grade calcium hydrogen phosphate by gravity floatation defluorination Download PDFInfo
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- CN1022556C CN1022556C CN 90105831 CN90105831A CN1022556C CN 1022556 C CN1022556 C CN 1022556C CN 90105831 CN90105831 CN 90105831 CN 90105831 A CN90105831 A CN 90105831A CN 1022556 C CN1022556 C CN 1022556C
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- minutes
- lime
- milk
- section
- neutralized
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- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 title claims abstract description 7
- 230000005484 gravity Effects 0.000 title claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000006115 defluorination reaction Methods 0.000 title claims description 5
- 235000019700 dicalcium phosphate Nutrition 0.000 title claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 16
- 239000011575 calcium Substances 0.000 claims description 15
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 13
- 229910052791 calcium Inorganic materials 0.000 claims description 13
- 239000000920 calcium hydroxide Substances 0.000 claims description 12
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 230000003472 neutralizing effect Effects 0.000 claims description 12
- 239000002367 phosphate rock Substances 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims 1
- 238000006386 neutralization reaction Methods 0.000 abstract description 11
- 238000011084 recovery Methods 0.000 abstract description 9
- 238000003483 aging Methods 0.000 abstract description 5
- 239000002244 precipitate Substances 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011737 fluorine Substances 0.000 abstract description 3
- 229910052731 fluorine Inorganic materials 0.000 abstract description 3
- 239000011574 phosphorus Substances 0.000 abstract description 3
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 abstract 1
- 235000011941 Tilia x europaea Nutrition 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 229910052816 inorganic phosphate Inorganic materials 0.000 abstract 1
- 239000004571 lime Substances 0.000 abstract 1
- 239000008267 milk Substances 0.000 abstract 1
- 210000004080 milk Anatomy 0.000 abstract 1
- 235000013336 milk Nutrition 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 235000011167 hydrochloric acid Nutrition 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229910004261 CaF 2 Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 229910017119 AlPO Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 235000011148 calcium chloride Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- LLSDKQJKOVVTOJ-UHFFFAOYSA-L calcium chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Ca+2] LLSDKQJKOVVTOJ-UHFFFAOYSA-L 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/324—Preparation from a reaction solution obtained by acidifying with an acid other than orthophosphoric acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/328—Defluorination during or after the preparation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Processing Of Solid Wastes (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The present invention belongs to the inorganic phosphate industry, and includes such technological steps as decomposing phosphorus ore by hydrochloric acid or sulfuric acid, primary neutralization by lime milk, separating fluorine-containing impurities by gravity floatation according to the flocculent precipitate and the settling speed difference of suspended matter, and secondary neutralization, ageing and separation to obtain P in conventional feed-grade calcium hydrogen phosphate2O5The recovery rate of the catalyst is improved from 30% to 80%.
Description
The present invention is a kind of method of utilizing feedstuff calcium hydrogen phosphate production by defluorination with gravity floatation.
The calcium hydrophosphate fodder production method of prior art, generally all adopt hydrochloric acid or sulfuric acid decomposing phosphate rock at home and abroad and carry out one section neutralization, defluorinate again after making acid hydrolysis solution, enter two sections neutralizations, filtration again, the precipitate and separate oven dry obtains calcium hydrophosphate fodder, " development of fodder additives secondary calcium phosphate " as the 21st volume third phase of Central China Normal University's journal (1987) report, use decomposing phosphate rock by chlorhydric acid, add the saturated aqueous common salt defluorinate, carry out one section neutralization and further defluorinate again, carry out two sections neutralizations thereafter, obtain calcium hydrophosphate fodder, feed P
2O
5The high energy of the rate of recovery reach 57.4%." the Production By Sulfuric Acid Process calcium hydrogen phosphate fodder craft discussion " of " phosphate industry " first phase report of and for example publishing in 1987, carry out defluorinate with adding sodium salt or sylvite in the technological process of sulfuric acid extraction phosphorus ore manufacturing calcium hydrophosphate fodder, its effect is all not good, can not reach the desired fluorine content of product standard, and draw a conclusion, use decomposing phosphate rock by chlorhydric acid, in its decomposed solution because of a large amount of Ca is arranged
++Ion exists, and produces the calcium effect, i.e. " common-ion effcet ", P when making its defluorinate
2O
5Loss is big, then can't improve feed grade P
2O
5The rate of recovery.
The objective of the invention is to improve feed grade P for overcoming " common-ion effcet "
2O
5The rate of recovery, and make product surpass GB8258-87(table two) standard-required; Make P
2O
5The rate of recovery reach 80%, present method also comprises with sulfuric acid and extracts phosphorus ore, the defluorination process of preparation such as general calcium leaching liquid calcium hydrophosphate fodder.
The present invention is achieved by the following technical solution, and is raw material with ground phosphate rock, adds hydrochloric acid or sulfuric acid and reacts, neutralizes, precipitates, filters, separates, dries and make calcium hydrophosphate fodder.It is characterized by: make complex ion ACF in the decomposing solution
3- 6AL with APO
4Precipitation is separated out, thereby discharges F
-Ion is with CaF
2Precipitation mode is removed, again reason " common-ion effcet " and be settled out a large amount of CaHPO simultaneously not
4Lose, take off F one section neutralization
-The time, the throw out that is generated has: AlPO
4, FePO
4, CaF
2, Si(OH)
4(H
2SiF
6The hydration H that hydrolysis goes out
2SiO
3H
2O), CaHPO
4, because they self solubleness and characteristic generate difform precipitation, AlPO
4, FePO
4, Si(OH)
2, generate unbodied flocks, CaF
2Generate the tiny settled suspended substance that is difficult to, because of the CaHPO of hydrolysis " common-ion effcet " generation
4Be more macrocrystalline crystalline precipitate, the former three not free settling that easily suspends, the latter is then opposite.According to this characteristic: to be neutralized to pH be 2.0~2.5 with containing CaO7~10% milk of lime, utilize the settling velocity difference of precipitation, the suspended substance of generating, from top to bottom the suspended substance that generates is sucked vacuum filter with siphon mode, separate deleterious impurity in the feeds product, under the condition of not using defluorinating agent, make the P in the feeds product
2O
5The rate of recovery improves.
Chemical reaction equation with decomposing phosphate rock by chlorhydric acid is as follows:
(1)
Impurity in the ore also participates in reaction:
Because in acidic solution, iron, aluminium and hydrogen fluoride generate difficult dissociated complex ion in (3) and (4).
The steady FeF of Pk
3- 6The steady AlF of=15.4Pk
3- 6=19.75
So AlF
3- 6Than SiF
3- 6Much stable, as using sodium, sylvite to generate Na
2SiF
6, K
2SiF
6Precipitation mode is removed complex ion AlF
3- 6In F be very difficult.
If adopt in one section of the milk of lime and defluorinate, its reaction formula is:
Complex compound AkF as can be known from (10) formula
3- 6Raise with pH, separate out precipitate A lPO
4And CaF
2, simultaneously in equation (8) and (1) formula owing to a large amount of CaCl
2Existence, promptly take place " common-ion effcet ", on the one hand CaCl
2Existence, under this acidity (pH) condition, CaHPO
4Solubleness reduce resultant Ca(H on the other hand
2PO
4)
2Hydrolysis takes place, and its reaction equation is:
Generate a large amount of CaHPO to making
4Precipitation makes P
2O
5Loss increases, and with impurity CaF
2, AlPO
4Deng being discarded together.
Fig. 1 is in a section of the embodiment of the invention and separation system figure;
Fig. 2 is the process flow sheet of the embodiment of the invention.
According to accompanying drawing invention is elaborated below:
Fig. 1, shown in Fig. 2, ground phosphate rock adds hydrochloric acid in decomposer (1) or sulfuric acid obtains acid decomposition liquid, acid decomposition liquid is put into one section neutralizing well (2), adding milk of lime stirs neutralization and generates suspended substance and precipitation, with siphon pipe (8) suspended substance in the neutralizing well (2) being sucked vacuum filter (3) consolidates, liquid separates, filtrate changes over to puts into ageing pond (5) ageing after two sections neutralizing wells (4) stir neutralization with milk of lime, change over to again vacuum filter (6) carry out solid liquid separate, filtrate is put into DFP pond (7) and is added the milk of lime clarification, separate, evaporation concentration obtains CaCl
2, send the drying room oven dry to make calcium hydrophosphate fodder after the filter cake washing.
1: one section neutralization reaction of embodiment and separation system add acid decomposition liquid 5M as shown in Figure 1 in one section neutralizing well (2)
3(P
2O
5Content 50.17g/L), be neutralized to pH2.0~2.5 with milk of lime (containing CaO7~10%) stirring, required time 1.0~1.5 hours, continue to stir 30 minutes, placed 15 minutes, and the suspended substance in one section neutralizing well (2) was sucked vacuum filter (3) (filtration area 5M from top to bottom with siphon pipe (8)
3) on carry out Gu liquid and separate, required time 3 hours, 7M
3Volumes of filtrate, and residual about 1M
3Neutralizer (comprising throw out) adds 5M then successively
3The volume decomposed solution, and carry out cyclical operation according to aforesaid method, obtain 8M at every turn
3Volumes of filtrate, mean P
2O
5Content is 26.35g/L, and F content is 0.05g/L, P
2O
5: F=527: 1, the phosphorous recovery of this section is 84.03%.
Embodiment 3, and to the leaching of general calcium, sulfuric acid decomposing phosphate rock system sink calcium, owing to there not being " common-ion effcet ", but the existence of Al arranged, and separate out CaF
2, pH improves then CaHPO
4Loss.Adopt one section isolating method of neutralization of embodiment 1, pH is controlled at 3.0~3.5, and phosphorous recovery also can reach 80%, and fluorine content also can be reduced to below the mark requirement.
Table one, ground phosphate rock are formed
Form title P
2O
5CaO
2MgO Al
2O
3Fe
2O
3F SiO
2
Content % 23.89 43.83 7.99 0.71 0.41 2.68 1
Table two, product analysis result
Project P Ca AS heavy metal fluoride fineness
Content % is (with P
2O
5Meter) (in Pb) (in F) 400 μ m
Sample number
P-3????19.93????26.37????0.001????0.0003????0.10????99.5
(45.65)
GB8258-87????≥16.0????≥21.0????≤0.003????≤0.002????0.18????95
Remarks: above product analysis result is six comprehensive sampling results that feed intake
Claims (2)
1, a kind of method of feedstuff calcium hydrogen phosphate production by defluorination with gravity floatation is characterized by this method and comprises the following steps:
A. ground phosphate rock is added and fills in the decomposer of hydrochloric acid, stir 40 minutes, obtain acid decomposition liquid;
B. acid decomposition liquid is put into one section neutralizing well, added the milk of lime that contains CaO7~10%, be neutralized to pH2.0~2.5, stirred 30 minutes, placed 15 minutes;
C. from top to bottom the slip in one section neutralizing well is sucked vacuum filter with siphon mode, carry out solid-liquid separation, residual will the slurry with decomposed solution dissolving next time;
The filtrate that obtains among the D.C is put into two sections neutralizing wells, adds the milk of lime contain CaO7~10%, is neutralized to pH4.5~5.0, stirs 30 minutes, and ageing is also carried out solid-liquid separation in vacuum filter, and filter cake washes with water, send to then dry calcium hydrophosphate fodder;
The filtrate that obtains among the E.D is put into the DFP pond, adds milk of lime and is neutralized to pH8~9, and clarification is isolated the calcium chloride clear liquid in the overflow mode and carried out other processing again, and raffinate returns two sections neutralizing wells.
2, by the described method of claim 1, it is characterized by with sulfuric acid decomposing phosphate rock thing, in one section and pH be 3.0~3.5.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 90105831 CN1022556C (en) | 1990-05-31 | 1990-05-31 | Production of feed-grade calcium hydrogen phosphate by gravity floatation defluorination |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 90105831 CN1022556C (en) | 1990-05-31 | 1990-05-31 | Production of feed-grade calcium hydrogen phosphate by gravity floatation defluorination |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1047063A CN1047063A (en) | 1990-11-21 |
CN1022556C true CN1022556C (en) | 1993-10-27 |
Family
ID=4879632
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN 90105831 Expired - Fee Related CN1022556C (en) | 1990-05-31 | 1990-05-31 | Production of feed-grade calcium hydrogen phosphate by gravity floatation defluorination |
Country Status (1)
Country | Link |
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CN (1) | CN1022556C (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1041812C (en) * | 1996-08-23 | 1999-01-27 | 四川绵竹龙蟒矿物质饲料集团有限公司 | Defluorination method in process of producing feed grade calcium hydrophosphate |
CN105819452B (en) * | 2016-04-01 | 2018-01-30 | 龚家竹 | A kind of method that fluorine resource is reclaimed in the defluorination residues from feed phosphate |
-
1990
- 1990-05-31 CN CN 90105831 patent/CN1022556C/en not_active Expired - Fee Related
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Publication number | Publication date |
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CN1047063A (en) | 1990-11-21 |
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CP03 | Change of name, title or address |
Address after: Mianzhu City, Sichuan Province, South Road 618200 Patentee after: Longmang Group Co., Ltd., Sichuan Prov Address before: 614009 Sichuan Leshan Shizhong fine feed factory Patentee before: Gong Jiazhu |
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C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
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