CN109516448A - The method that yellow phosphorus furnace slag and phosphoric acid by wet process prepare calcium monohydrogen phosphate and white carbon black - Google Patents
The method that yellow phosphorus furnace slag and phosphoric acid by wet process prepare calcium monohydrogen phosphate and white carbon black Download PDFInfo
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- CN109516448A CN109516448A CN201811553463.5A CN201811553463A CN109516448A CN 109516448 A CN109516448 A CN 109516448A CN 201811553463 A CN201811553463 A CN 201811553463A CN 109516448 A CN109516448 A CN 109516448A
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- phosphoric acid
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- furnace slag
- yellow phosphorus
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000002893 slag Substances 0.000 title claims abstract description 42
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 title claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000006229 carbon black Substances 0.000 title claims abstract description 27
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 title claims abstract description 25
- 235000019700 dicalcium phosphate Nutrition 0.000 title claims abstract description 9
- 239000011575 calcium Substances 0.000 claims abstract description 53
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 49
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000003337 fertilizer Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 59
- NGHMEZWZOZEZOH-UHFFFAOYSA-N silicic acid;hydrate Chemical compound O.O[Si](O)(O)O NGHMEZWZOZEZOH-UHFFFAOYSA-N 0.000 claims description 31
- 239000000706 filtrate Substances 0.000 claims description 30
- 239000011343 solid material Substances 0.000 claims description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000004115 Sodium Silicate Substances 0.000 claims description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 11
- 239000011574 phosphorus Substances 0.000 claims description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000006210 lotion Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 239000000292 calcium oxide Substances 0.000 claims description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000003763 carbonization Methods 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 235000013312 flour Nutrition 0.000 claims description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 239000000920 calcium hydroxide Substances 0.000 claims description 5
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 7
- 229910052731 fluorine Inorganic materials 0.000 description 6
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical group [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- MBVFGUGHATZQGK-UHFFFAOYSA-N calcium hydrogen phosphite Chemical compound [Ca++].OP([O-])[O-] MBVFGUGHATZQGK-UHFFFAOYSA-N 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- -1 phosphoric acid hydrogen Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/26—Compounds containing phosphorus
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/28—Silicates, e.g. perlites, zeolites or bentonites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Animal Husbandry (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a kind of methods that yellow phosphorus furnace slag and phosphoric acid by wet process prepare calcium monohydrogen phosphate and white carbon black, this method leaches yellow phosphorus furnace slag using phosphoric acid by wet process solution, leachate respectively obtains fertilizer calcium hydrophosphate and calcium hydrophosphate fodder product through two-step precipitation, and leached mud is through alkali soluble conversion, CO2Gas is carbonized to obtain white carbon black product；The method of the present invention process equipment is simple, operation is easy, is safe, and yellow phosphorus furnace slag resource utilization is high, is a kind of processing technology routine using trade waste production with high value added product, it can reach secondary resource comprehensive utilization, realize circular economy, energy-saving and emission-reduction purpose.
Description
Technical field
The invention belongs to industrial solid castoffs to utilize field, and in particular to a kind of yellow phosphorus furnace slag and phosphoric acid by wet process prepare phosphorus
The method of sour hydrogen calcium and white carbon black.
Background technique
When yellow phosphorus furnace slag is that electric furnace process produces yellow phosphorus using raw materials such as rock phosphate in powder, silica, coke, in 1400~1600 DEG C of height
The lower molten mass formed of temperature contains a large amount of SiO through having amorphous, high activity solid waste obtained by water quenching chilling2With
CaO.Currently, yellow phosphorus furnace slag is mainly for the production of low-value products such as calcium silicate fertilizer, cement, slag bricks, and utilization rate is lower, Duo Shuohuang
Phosphorus manufacturing enterprise be stacked it is to be processed, containing the harmful elements such as P, F, Fe, Al, Mg in yellow phosphorus furnace slag, the phosphorus largely stacked
Slag easily causes the pollution to surface water resources and river waterr resources, jeopardizes the ecological safety of runoff area and people, animal.
Yellow phosphorus furnace slag is rich in CaO and SiO2, can be used for producing calcic and siliceous product.It is produced at present using yellow phosphorus furnace slag white
The method of carbon black mainly has using salt Ore Leaching yellow phosphorus furnace slag, obtains white carbon black and calcium chloride product through alkali soluble, sour precipitating technique,
Wherein calcium chloride application market is limited, sales difficulty.Patent document CN101381082A is reported a kind of to be produced with yellow phosphorus furnace slag
The method of high quality silica, this method extract yellow phosphorus furnace slag using phosphoric acid by wet process, and nitric acid solution is added after leached mud is washed
Then refinement treatment obtains white carbon black product through drying, calcining.Patent document CN101381077B reports a kind of yellow phosphorus furnace slag
The method of preparing phosphoric acid hydrogen calcium, this method extracts yellow phosphorus furnace slag using phosphoric acid by wet process, and through separating, the leachate of phosphorous acid calcium salt is passed through
Dearsenification, heavy metal are purified, after condensing crystallizing removes the impurity such as fluorine, crystal is dissolved with water again, and calcium carbonate and calcium hydroxide is added
Suspension neutralizes to obtain calcium monophosphate product.This method needs the calcium monohydrogen phosphate purified, crystallization conversion can just obtain higher quality
Product, process flow are more complex.
Summary of the invention
The purpose of the present invention is to provide one using the main component Si and Ca contained in yellow phosphorus furnace slag, while producing mesh
The preceding market demand is very big and has the white carbon black and calcium monophosphate product of high added value, can reach secondary resource comprehensive utilization, real
Existing circular economy, energy-saving and emission-reduction purpose.
Technical scheme is as follows: leaching yellow phosphorus furnace slag using phosphoric acid solution, leachate is distinguished through two-step precipitation
Fertilizer calcium hydrophosphate and calcium hydrophosphate fodder product are obtained, leached mud is through alkali soluble conversion, CO2Gas is carbonized to obtain white carbon black
Product.
The method that yellow phosphorus furnace slag and phosphoric acid by wet process of the present invention prepare calcium monohydrogen phosphate and white carbon black, concrete operations are as follows:
(1) phosphoric acid solution of mass concentration 20~40% prepared by phosphoric acid by wet process is added in the reactor, according to phosphorus in reactor
The quality of acid, by 120~150% amount of the theory phosphoric acid amount of acid decomposed by phosphoric acid yellow phosphorus furnace slag, mixing speed is 300~
The finely ground yellow phosphorus furnace slag to 80~120 mesh of corresponding measurement is added under conditions of 500rpm in the reactor, is in normal pressure, temperature
0.5~2.0h of Leach reaction under the conditions of 50~90 DEG C, isolated leachate and silicic acid hydrate solid material, silicic acid hydrate solid
Material is washed with water 3 times；
(2) under conditions of normal pressure, natural temperature, mixing speed are 300~500rpm, by leachate obtained by step (1) and water
It closes silicic acid solid material washing lotion to merge and be uniformly mixed, the addition calcium neutralizer in mixed liquor, regulation system pH to 1.5~2.5,
Continue to be stirred to react 0.5~2.0h, isolated fertilizer grade calcium monophosphate product and filtrate, fertilizer calcium hydrophosphate is washed,
It is dried to obtain fertilizer grade calcium monophosphate product；
(3) under conditions of normal pressure, natural temperature, mixing speed are 300~500rpm, by filtrate obtained by step (2) and washing lotion
Mixing, is added calcium neutralizer, and regulation system pH to 4~5 continues to be stirred to react 0.5 ~ 2.0h, isolated feed grade phosphoric acid hydrogen
Calcium and filtrate, calcium hydrophosphate fodder is washed, is dried to obtain calcium hydrophosphate fodder product；
(4) hydroxide that mass concentration is 30~40% is added in the washed silicic acid hydrate solid material that step (1) obtains
Sodium solution is warming up to 80~90 DEG C and is stirred to react 2.0~4.0h, controls reaction end pH >=12, isolated sodium silicate solution；
(5) under the stirring condition of room temperature, normal pressure and 300~500rpm, lead in the isolated sodium silicate solution of step (4)
Enter CO2Gas carries out carbonization treatment, and when pH value of solution reaches 8~10, stopping is passed through CO2Gas continues 300~500rpm's
It is reacted under stirring condition 0.5~1.0 hour, then isolated filtrate and silicic acid hydrate precipitate；Silicic acid hydrate is washed with water 3 admittedly
It is secondary；
(6) step (5) washed silicic acid hydrate is deposited in 120~150 DEG C of dryings 2.0~3.0 hours, then 600~800
DEG C obtain White Carbon black product within temperature lower calcination 0.5~1.0 hour；
(7) step (5) isolated filtrate, is concentrated by evaporation, is crystallized, isolated sodium carbonate product.
Phosphoric acid by wet process in the step (1) refers to the phosphoric acid obtained using sulfuric acid extraction phosphorus ore.
Natural temperature in the step (2) and (3) is that Temperature fall reaches solution in process of production after previous step is handled
The temperature arrived.
Calcium neutralizer in the step (2) and (3) is mountain flour (calcium carbonate) suspension, milk of lime, CaO etc..
The present invention has following advantages and effect:
(1) silica and calcium oxide in the present invention effectively extraction and application yellow phosphorus furnace slag, prepares the production with high added value
Product provide a new technology for the utilization of yellow phosphorus furnace slag；
(2) in the method for the present invention process flow, while preparing calcium hydrophosphate fodder product using calcium oxide, pass through leaching
The conversion of slag alkali soluble, CO2The white carbon black product of gas carbonization preparation high-quality, can simultaneously obtain the silicon with high added value, calcium produces
Product, yellow phosphorus furnace slag resource utilization are high；
(3) the features such as present invention has process equipment simple, and operation is easy, is safe.
The solid slag preparation that the present invention is generated using phosphorus production has the calcium hydrophosphate fodder of high added value and white
Carbon black products can adequately and reasonably utilize resource, turn waste into wealth, and reduce environmental pollution, economize on resources, reach environmentally protective mesh
, it is of great significance to the recycling of resource.
Specific embodiment
Below by embodiment, invention is further described in detail, but the scope of the present invention is not limited in described
Hold.
Embodiment 1:
(1) phosphoric acid solution of mass concentration 40% prepared by phosphoric acid by wet process is added in the reactor, according to phosphoric acid in reactor
Quality, by 130% amount of the theory phosphoric acid amount of acid decomposed by phosphoric acid yellow phosphorus furnace slag, mixing speed be 300rpm under conditions of anti-
The finely ground yellow phosphorus furnace slag to 120 mesh that corresponding measurement is added in device is answered, Leach reaction under the conditions of normal pressure, temperature are 50 DEG C
1.0h, isolated leachate and silicic acid hydrate solid material, silicic acid hydrate solid material are washed with water 3 times；
(2) under conditions of normal pressure, natural temperature, mixing speed are 500rpm, by leachate obtained by step (1) and silicic acid hydrate
Solid material washing lotion merges and is uniformly mixed, and mountain flour suspension is added in mixed liquor, adjusts pH of mixed to 2.5, continues to stir
Reaction 1.5h, isolated fertilizer grade calcium monophosphate product and filtrate are mixed, fertilizer calcium hydrophosphate is washed, is dried to obtain fertilizer
Calcium hydrophosphate product；Through analyzing, the effective phosphorus pentoxide (P of the fertilizer grade calcium monophosphate product2O5) content be 25.43%；
(3) under conditions of normal pressure, natural temperature, mixing speed are 300rpm, filtrate obtained by step (2) and washing lotion are mixed,
Mountain flour suspension is added, adjusting pH of mixed to 4 continues to be stirred to react 2.0h, isolated calcium hydrophosphate fodder and filtrate,
Calcium hydrophosphate fodder is washed, is dried to obtain calcium hydrophosphate fodder product；Through analyzing, which contains
Phosphorus (P) 17.24%, calcium (Ca) 21.58%, fluorine (F) 0.08%；
(4) in the washed silicic acid hydrate solid material that step (1) obtains, the sodium hydroxide that mass concentration 30% is added is molten
Liquid is warming up to 90 DEG C and is stirred to react 2.0h, controls reaction end PH >=12, isolated sodium silicate solution；
(5) it under the stirring condition of room temperature, normal pressure and 400rpm, in the isolated sodium silicate solution of step (4), is passed through
CO2Gas carries out carbonization treatment, and when pH value of solution reaches 8, stopping is passed through CO2Gas continues anti-under the stirring condition of 400rpm
It answers 0.75 hour, then isolated filtrate and silicic acid hydrate precipitate；Silicic acid hydrate is washed with water 3 times admittedly；
(6) the washed silicic acid hydrate precipitating that step (5) obtains, it is 3.0 hours dry in 120 DEG C, then in 700 DEG C of temperature
Lower calcining obtains White Carbon black product in 1.0 hours；Through analyzing, white carbon black product SiO2Content is 98.75%, and appearance is white
Color；
(7) step (5) isolated filtrate, is concentrated by evaporation, is crystallized, isolated sodium carbonate product, through analyzing, the sodium carbonate
Product NaCO3Content is 98.86%, and appearance is white.
Embodiment 2:
(1) phosphoric acid solution of mass concentration 20% prepared by phosphoric acid by wet process is added in the reactor, according to phosphoric acid in reactor
Quality, by 150% amount of the theory phosphoric acid amount of acid decomposed by phosphoric acid yellow phosphorus furnace slag, low whipping speed be 400rpm under conditions of
The finely ground yellow phosphorus furnace slag to 90 mesh of corresponding measurement is added in reactor, Leach reaction under the conditions of normal pressure, temperature are 90 DEG C
0.5h, isolated leachate and silicic acid hydrate solid material, silicic acid hydrate solid material are washed with water 3 times；
(2) under conditions of normal pressure, natural temperature, mixing speed are 300rpm, by leachate obtained by step (1) and wash heat is leached
Liquid merges and is uniformly mixed, and milk of lime is added in mixed liquor, adjusts pH of mixed to 1.5, continues to be stirred to react 2.0h, separate
Fertilizer grade calcium monophosphate product and filtrate are obtained, fertilizer calcium hydrophosphate is washed, is dried to obtain fertilizer grade calcium monophosphate product；
Through analyzing, the effective phosphorus pentoxide (P of the fertilizer grade calcium monophosphate product2O5) content be 24.89%；
(3) under conditions of normal pressure, natural temperature, mixing speed are 500rpm, precipitation filtrates obtained by step (2) and washing lotion are mixed
It closes, milk of lime is added, regulation system pH to 5 continues to be stirred to react 0.5h, isolated calcium hydrophosphate fodder and filtrate, raises
Material calcium hydrophosphate is washed, is dried to obtain calcium hydrophosphate fodder product；Through analyzing, the calcium hydrophosphate fodder product is phosphorous
(P) 16.92%, calcium (Ca) 21.86%, fluorine (F) 0.10%；
(4) in the washed silicic acid hydrate solid material that step (1) obtains, the sodium hydroxide solution that concentration is 40% is added,
It is warming up to 80 DEG C and is stirred to react 3.0h, control reaction end pH >=12, isolated sodium silicate solution；
(5) it under the stirring condition of room temperature, normal pressure and 300rpm, in the isolated sodium silicate solution of step (4), is passed through
CO2Gas carries out carbonization treatment, and when pH value of solution reaches 10, stopping is passed through CO2Gas continues under the stirring condition of 300rpm
Reaction 1.0 hours, then isolated filtrate and silicic acid hydrate precipitate；Silicic acid hydrate is washed with water 3 times admittedly；
(6) the washed silicic acid hydrate precipitating that step (5) obtains, it is 2.0 hours dry in 150 DEG C, then in 750 DEG C of temperature
Lower calcining obtains White Carbon black product in 0.5 hour；Through analyzing, white carbon black product SiO2Content is 99.16%, and appearance is white
Color；
(7) step (5) isolated filtrate, is concentrated by evaporation, is crystallized, isolated sodium carbonate product, through analyzing, the sodium carbonate
Product NaCO3Content is 99.04%, and appearance is white.
Embodiment 3:
(1) phosphoric acid solution of mass concentration 30% prepared by phosphoric acid by wet process is added in the reactor, according to phosphoric acid in reactor
Quality, by 120% amount of the theory phosphoric acid amount of acid decomposed by phosphoric acid yellow phosphorus furnace slag, low whipping speed be 500rpm under conditions of
The finely ground yellow phosphorus furnace slag to 100 mesh of corresponding measurement is added in reactor, Leach reaction under the conditions of normal pressure, temperature are 65 DEG C
1.5h, isolated leachate and silicic acid hydrate solid material, silicic acid hydrate solid material are washed with water 3 times；
(2) under conditions of normal pressure, natural temperature, mixing speed are 400rpm, by leachate obtained by step (1) and wash heat is leached
Liquid merges and is uniformly mixed, and CaO, regulation system pH to 2.0 are added in mixed liquor, continues to be stirred to react 1.0h, isolated
Fertilizer grade calcium monophosphate product and filtrate, fertilizer calcium hydrophosphate is washed, is dried to obtain fertilizer grade calcium monophosphate product；Through dividing
Analysis, the effective phosphorus pentoxide (P of the fertilizer grade calcium monophosphate product2O5) content be 26.15%；
(3) under conditions of normal pressure, natural temperature, mixing speed are 450rpm, precipitation filtrates obtained by step (2) and washing lotion are mixed
It closes, CaO, regulation system pH to 4.5 is added, continues to be stirred to react 1.5h, isolated calcium hydrophosphate fodder and filtrate, feed
Calcium hydrophosphate is washed, is dried to obtain calcium hydrophosphate fodder product；Through analyzing, the calcium hydrophosphate fodder product is phosphorous
(P) 17.16%, calcium (Ca) 22.17%, fluorine (F) 0.14%；
(4) in the washed silicic acid hydrate solid material that step (1) obtains, the sodium hydroxide solution that concentration is 5% is added,
It is warming up to 85 DEG C and is stirred to react 4.0h, control reaction end PH >=12, isolated sodium silicate solution；
(5) it under the stirring condition of room temperature, normal pressure and 500rpm, in the isolated sodium silicate solution of step (4), is passed through
CO2Gas carries out carbonization treatment, and when solution PH reaches 9, stopping is passed through CO2Gas continues anti-under the stirring condition of 500rpm
It answers 0.5 hour, then isolated filtrate and silicic acid hydrate precipitate；Silicic acid hydrate is washed with water 3 times admittedly；
(6) the washed silicic acid hydrate precipitating that step (5) obtains, it is 2.0 hours dry in 140 DEG C, then in 600 DEG C of temperature
Lower calcining obtains White Carbon black product in 0.75 hour；Through analyzing, white carbon black product SiO2Content is 97.58%, and appearance is white
Color；
(7) step (5) isolated filtrate, is concentrated by evaporation, is crystallized, isolated sodium carbonate product, through analyzing, the sodium carbonate
Product NaCO3Content is 98.94%, and appearance is white.
Embodiment 4:
(1) phosphoric acid solution of mass concentration 35% prepared by phosphoric acid by wet process is added in the reactor, according to phosphoric acid in reactor
Quality, by 140% amount of the theory phosphoric acid amount of acid decomposed by phosphoric acid yellow phosphorus furnace slag, low whipping speed be 450rpm under conditions of
The finely ground yellow phosphorus furnace slag to 80 mesh of corresponding measurement is added in reactor, Leach reaction under the conditions of normal pressure, temperature are 80 DEG C
2.0h, isolated leachate and silicic acid hydrate solid material, silicic acid hydrate solid material are washed with water 3 times；
(2) under conditions of normal pressure, natural temperature, mixing speed are 500rpm, by leachate obtained by step (1) and wash heat is leached
Liquid merges and is uniformly mixed, and mountain flour (calcium carbonate) suspension is added in mixed liquor, and it is anti-to continue stirring by regulation system pH to 1.7
0.5h, isolated fertilizer grade calcium monophosphate product and filtrate are answered, fertilizer calcium hydrophosphate is washed, is dried to obtain fertilizer grade phosphorus
Sour hydrogen calcium product；Through analyzing, the effective phosphorus pentoxide (P of the fertilizer grade calcium monophosphate product2O5) content be 25.17%；
(3) under conditions of normal pressure, natural temperature, mixing speed are 400rpm, precipitation filtrates obtained by step (2) and washing lotion are mixed
It closes, mountain flour (calcium carbonate) suspension is added, regulation system pH to 4.8 continues to be stirred to react 1.0h, isolated feed grade phosphoric acid
Hydrogen calcium and filtrate, calcium hydrophosphate fodder is washed, is dried to obtain calcium hydrophosphate fodder product；Through analyzing, the feed grade phosphorus
Sour phosphorous (P) 17.03% of hydrogen calcium product, calcium (Ca) 21.92%, fluorine (F) 0.15%；
(4) in the washed silicic acid hydrate solid material that step (1) obtains, the sodium hydroxide that mass concentration is 38% is added
Solution, 80 DEG C of heating are stirred to react 3.5h, control reaction end PH >=12, isolated sodium silicate solution；
(5) it under the stirring condition of room temperature, normal pressure and 420rpm, in the isolated sodium silicate solution of step (4), is passed through
CO2Gas carries out carbonization treatment, and when solution PH reaches 8.5, stopping is passed through CO2Gas continues under the stirring condition of 420rpm
Reaction 1.0 hours, then isolated filtrate and silicic acid hydrate precipitate；Silicic acid hydrate is washed with water 3 times admittedly；
(6) the washed silicic acid hydrate precipitating that step (5) obtains, it is 2.5 hours dry in 130 DEG C, then in 800 DEG C of temperature
Lower calcining obtains White Carbon black product in 0.5 hour；Through analyzing, white carbon black product SiO2Content is 98.32%, and appearance is white
Color；
(7) step (5) isolated filtrate, is concentrated by evaporation, is crystallized, isolated sodium carbonate product, through analyzing, the sodium carbonate
Product NaCO3Content is 98.72%, and appearance is white.
Claims (4)
1. a kind of method that yellow phosphorus furnace slag and phosphoric acid by wet process prepare calcium monohydrogen phosphate and white carbon black, it is characterised in that according to the following steps into
Row:
(1) phosphoric acid solution of mass concentration 20~40% prepared by phosphoric acid by wet process is added in the reactor, according to phosphorus in reactor
The quality of acid, by 120~150% amount of the theory phosphoric acid amount of acid decomposed by phosphoric acid yellow phosphorus furnace slag, mixing speed is 300~
The finely ground yellow phosphorus furnace slag to 80~120 mesh of corresponding measurement is added under 500rpm in the reactor, is soaked at normal pressure, 50~90 DEG C
0.5~2.0h is reacted out, and isolated leachate and silicic acid hydrate solid material, silicic acid hydrate solid material are washed with water 3 times；
(2) under conditions of normal pressure, natural temperature, mixing speed are 300~500rpm, by leachate obtained by step (1) and water
It closes silicic acid solid material washing lotion to merge and be uniformly mixed, the addition calcium neutralizer in mixed liquor, adjusting pH of mixed to 1.5~
2.5, continue to be stirred to react 0.5~2.0h, isolated fertilizer grade calcium monophosphate product and filtrate, fertilizer calcium hydrophosphate is through washing
It washs, be dried to obtain fertilizer grade calcium monophosphate product；
(3) under conditions of normal pressure, natural temperature, mixing speed are 300~500rpm, by filtrate obtained by step (2) and washing lotion
Calcium neutralizer is added in mixing, adjusts pH of mixed to 4~5, continues to be stirred to react 0.5 ~ 2.0h, isolated feed grade phosphoric acid
Hydrogen calcium and filtrate, calcium hydrophosphate fodder is washed, is dried to obtain calcium hydrophosphate fodder product；
(4) sodium hydroxide solution of mass concentration 30~40% is added in the washed silicic acid hydrate solid material of step (1),
It is warming up to 80~90 DEG C and is stirred to react 2.0~4.0h, control reaction end pH >=12, isolated sodium silicate solution；
(5) under the stirring condition of room temperature, normal pressure and 300~500rpm, lead in the isolated sodium silicate solution of step (4)
Enter CO2Gas carries out carbonization treatment, and when pH value of solution reaches 8~10, stopping is passed through CO2Gas continues 300~500rpm's
It is reacted under stirring condition 0.5~1.0 hour, then isolated filtrate and silicic acid hydrate precipitate；Silicic acid hydrate precipitating is washed with water
It washs 3 times；
(6) step (5) washed silicic acid hydrate is deposited in 120~150 DEG C of dryings 2.0~3.0 hours, then 600~800
DEG C obtain White Carbon black product within temperature lower calcination 0.5~1.0 hour；
(7) step (5) isolated filtrate, is concentrated by evaporation, is crystallized, isolated sodium carbonate product.
2. the method that the yellow phosphorus furnace slag and phosphoric acid by wet process prepare calcium monohydrogen phosphate and white carbon black according to claim 1, special
Sign is: phosphoric acid by wet process refers to the phosphoric acid obtained using sulfuric acid extraction phosphorus ore.
3. the method that yellow phosphorus furnace slag according to claim 1 and phosphoric acid by wet process prepare calcium monohydrogen phosphate and white carbon black, feature
Be: natural temperature described in step (2) and step (3) is that Temperature fall reaches solution in process of production after previous step is handled
Temperature.
4. the method that yellow phosphorus furnace slag according to claim 1 and phosphoric acid by wet process prepare calcium monohydrogen phosphate and white carbon black, feature
Be: calcium neutralizer described in step (2) and step (3) is mountain flour suspension, milk of lime or CaO.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113023699A (en) * | 2021-04-28 | 2021-06-25 | 贵州福泉川东化工有限公司 | Method for separating and purifying ferrophosphorus and calcium silicate composite waste |
| CN114368755A (en) * | 2021-12-29 | 2022-04-19 | 四川马边龙泰磷电有限责任公司 | Process for producing precipitated white carbon black and light calcium carbonate by using yellow phosphorus waste side product |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1373086A (en) * | 2001-12-21 | 2002-10-09 | 叶天润 | Process for preparing both sodium carbonate and silica white |
| CN102807201A (en) * | 2012-02-09 | 2012-12-05 | 昆明川金诺化工股份有限公司 | Method for preparing feed-grade calcium hydrophosphate by wet-process phosphoric acid organic extraction and purification raffinate |
-
2018
- 2018-12-19 CN CN201811553463.5A patent/CN109516448A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1373086A (en) * | 2001-12-21 | 2002-10-09 | 叶天润 | Process for preparing both sodium carbonate and silica white |
| CN102807201A (en) * | 2012-02-09 | 2012-12-05 | 昆明川金诺化工股份有限公司 | Method for preparing feed-grade calcium hydrophosphate by wet-process phosphoric acid organic extraction and purification raffinate |
Non-Patent Citations (1)
| Title |
|---|
| 苏毅: ""黄磷炉渣提取白炭黑和磷酸氢钙的研究"", 《中国优秀博硕士学位论文全文数据库（博士） 工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113023699A (en) * | 2021-04-28 | 2021-06-25 | 贵州福泉川东化工有限公司 | Method for separating and purifying ferrophosphorus and calcium silicate composite waste |
| CN114368755A (en) * | 2021-12-29 | 2022-04-19 | 四川马边龙泰磷电有限责任公司 | Process for producing precipitated white carbon black and light calcium carbonate by using yellow phosphorus waste side product |
| CN114368755B (en) * | 2021-12-29 | 2024-04-05 | 四川马边龙泰磷电有限责任公司 | Process for by-producing precipitated white carbon black and light calcium carbonate by utilizing yellow phosphorus waste |
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