CN101381082A - Method for preparing high quality silica from yellow phosphorus slag - Google Patents
Method for preparing high quality silica from yellow phosphorus slag Download PDFInfo
- Publication number
- CN101381082A CN101381082A CNA2008102334533A CN200810233453A CN101381082A CN 101381082 A CN101381082 A CN 101381082A CN A2008102334533 A CNA2008102334533 A CN A2008102334533A CN 200810233453 A CN200810233453 A CN 200810233453A CN 101381082 A CN101381082 A CN 101381082A
- Authority
- CN
- China
- Prior art keywords
- yellow phosphorus
- phosphoric acid
- phosphorus slag
- slag
- high quality
- 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
- 239000002893 slag Substances 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 34
- 238000000034 method Methods 0.000 title claims abstract description 29
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 title claims description 37
- 239000000377 silicon dioxide Substances 0.000 title claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000006229 carbon black Substances 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011574 phosphorus Substances 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 238000000605 extraction Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 2
- 239000002440 industrial waste Substances 0.000 abstract 2
- 238000002386 leaching Methods 0.000 abstract 2
- 235000019739 Dicalciumphosphate Nutrition 0.000 abstract 1
- 241000872198 Serjania polyphylla Species 0.000 abstract 1
- 239000001506 calcium phosphate Substances 0.000 abstract 1
- 239000002537 cosmetic Substances 0.000 abstract 1
- NEFBYIFKOOEVPA-UHFFFAOYSA-K dicalcium phosphate Chemical compound [Ca+2].[Ca+2].[O-]P([O-])([O-])=O NEFBYIFKOOEVPA-UHFFFAOYSA-K 0.000 abstract 1
- 229940038472 dicalcium phosphate Drugs 0.000 abstract 1
- 229910000390 dicalcium phosphate Inorganic materials 0.000 abstract 1
- 239000003814 drug Substances 0.000 abstract 1
- 239000003973 paint Substances 0.000 abstract 1
- 238000005498 polishing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 6
- 239000002699 waste material Substances 0.000 description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000011575 calcium Substances 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
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention provides a method for producing high-quality white carbon black with phosphorus slag. The method is to leach phosphorus slag with wet-process phosphoric acid and obtain high-quality white carbon black after separation, washing, refining and calcination. The leaching process by wet-process phosphoric acid is carried out under the conditions of room temperature, a room temperature, a 25 to 40 percent concentration of phosphoric acid, a leaching time of 0.5 to 2.0 hours, a stirring speed of 200 to 500 r/min, a solid to liquid ratio of 1 to between 5 and 10, and granularity of more than 100 meshes for all phosphorus slag. The product is widely used industries such as rubber, paint, printing ink, medicine, paper manufacture, food, cosmetics, chemical and mechanical polishing. The method not only makes full use of phosphorus slag which is industrial waste and develops a new application of the phosphorus slag that changing the industrial waste into a useful thing, but also reduces the production costs of dicalcium phosphate and saves resources.
Description
Technical field
The invention belongs to chemical industry waste utilization technical field, the method for the preparing high quality silica from yellow phosphorus slag in specifically a kind of industrial production.
Background technology
Yellow phosphorus furnace slag is the solid waste of electric furnace process output when adopting raw material production yellow phosphorus such as Rock Phosphate (72Min BPL), silica, coke, but 8～10 tons of slags of 1 ton of yellow phosphorus output of industrial every production, according to the production status of the present yellow phosphorus of China, about 600～7,000,000 tons of the annual output yellow phosphorus furnace slag of China yellow phosphorus enterprise.Process shrend when yellow phosphorus furnace slag discharges from electric furnace, granularity is between 0.5～1.5mm, and yellow phosphorus enterprise is distributed in scarcely populated and more approaching area, phosphorus ore mountain mostly, the gradient is big, rainwater is concentrated, meet heavy rain, a large amount of phosphorus slags flow to low-lying river with rainwater and forms precipitation, brings harm such as hindering river, raising riverbed.Simultaneously, contain harmful elements such as P, F, Fe, Al, Mg in the yellow phosphorus furnace slag, be easy to cause pollution, jeopardize the life security of the runoff area masses, livestock surface water resources and river waterr resources.At present, yellow phosphorus furnace slag is mainly used in produces calcium silicate fertilizer, cement, brick etc., and utilization ratio is low, and value of the product is low.The method that adopts yellow phosphorus furnace slag to produce white carbon black mainly is to adopt hydrochloric acid to leach yellow phosphorus furnace slag at present, obtains white carbon black and calcium chloride product through molten, the sour precipitating technology of alkali, and wherein the calcium chloride application market is limited, sales difficulty, and white carbon black production complex process.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing the production of trade waste yellow phosphorus furnace slag to have the Chemicals high quality silica of higher-value, realized utilization of waste material, recycling economy, energy-saving and emission-reduction.
The present invention is achieved in that in beaker adding concentration is 25% or 40～45% phosphoric acid by wet process and to be mixed with phosphoric acid concentration be 25～40% solution, under the continuous stirring condition of normal temperature, add to-100 purpose yellow phosphorus furnace slags through porphyrize, every 100ml phosphoric acid solution adds 10～20g yellow phosphorus furnace slag, at stirring reaction under the natural temperature condition after 0.5～2.0 hour, solid-liquid separation also is washed with water to neutrality with filter residue, add concentration then and be 5～10% salpeter solution, making solid-to-liquid ratio is 1:3～8, also washing is extremely neutral for 2.0～4.0 hours after-filtration of stirring reaction under 70～95 ℃ temperature, drying then, 700～900 ℃ of temperature lower calcinations 0.5～1.0 hour, take out cooling, porphyrize gets the white carbon black product.
The present invention utilizes yellow phosphorus furnace slag to be rich in CaO and SiO
2, the characteristic that can be used for producing calcic and siliceous product is developed one and is utilized main component Si and the Ca that contains in the yellow phosphorus furnace slag, the white carbon black product that production existing market demand is very big, but while by-product calcium monophosphate product.The present invention adopts phosphoric acid by wet process to leach yellow phosphorus furnace slag, can directly obtain quality fine white carbon black product through refining, but while by-product calcium monophosphate product, not only can make full use of the trade waste yellow phosphorus furnace slag, for new application approach of utilization exploitation of yellow phosphorus furnace slag, turn waste into wealth, reduce environmental pollution, and can reduce the production cost of white carbon black, economize on resources.
Embodiment
Embodiment 1:
Adding concentration is 25% phosphoric acid by wet process 300ml in beaker, under the continuous stirring condition of normal temperature, add through porphyrize to-100 purpose yellow phosphorus furnace slags 50 grams, stirring reaction is after 1.0 hours under the condition of natural temperature and stirring velocity 400rpm, solid-liquid separation also is washed with water to neutrality with filter residue, add concentration then and be 6% salpeter solution, making solid-to-liquid ratio is 1:3, also washing is extremely neutral for 4 hours after-filtration of stirring reaction under 70 ℃ temperature, drying then, 700 ℃ of temperature lower calcinations 0.5 hour, take out cooling, porphyrize gets the white carbon black sample, this sample contains SiO by analysis
291.3%, whiteness is Wj=89%, and specific surface area is 203m
2/ g.
Embodiment 2:
Adding concentration is 25% phosphoric acid by wet process 400ml in beaker, under the continuous stirring condition of normal temperature, add through porphyrize to-100 purpose yellow phosphorus furnace slags 50 grams, stirring reaction is after 0.5 hour under the condition of natural temperature and stirring velocity 300rpm, solid-liquid separation also is washed with water to neutrality with filter residue, add concentration then and be 8% salpeter solution, making solid-to-liquid ratio is 1:5, also washing is extremely neutral for 3.5 hours after-filtration of stirring reaction under 75 ℃ temperature, drying then, 750 ℃ of temperature lower calcinations 0.5 hour, take out cooling, porphyrize gets the white carbon black sample, this sample contains SiO by analysis
294.7%, whiteness is Wj=91%, and specific surface area is 207m
2/ g.
Embodiment 3:
Adding concentration is 45% phosphoric acid by wet process 150ml in beaker, thin up is behind 250ml, under the continuous stirring condition of normal temperature, add through porphyrize to-100 purpose yellow phosphorus furnace slags 50 grams, stirring reaction is after 1.0 hours under the condition of natural temperature and stirring velocity 350rpm, solid-liquid separation also is washed with water to neutrality with filter residue, add concentration then and be 5% salpeter solution, making solid-to-liquid ratio is 1:7,3.5 hours after-filtration of stirring reaction and washing be to neutral under 80 ℃ temperature, and drying then was 800 ℃ of temperature lower calcinations 1 hour, take out cooling, porphyrize gets the white carbon black sample, and this sample contains SiO by analysis
296.1%, whiteness is 93%, and specific surface area is 217m
2/ g.
Embodiment 4:
Adding concentration is 45% phosphoric acid by wet process 200ml in beaker, thin up is behind 250ml, under the continuous stirring condition of normal temperature, add through porphyrize to-100 purpose yellow phosphorus furnace slags 50 grams, stirring reaction is after 1.0 hours under the condition of natural temperature and stirring velocity 450rpm, solid-liquid separation also is washed with water to neutrality with filter residue, add concentration then and be 7% salpeter solution, making solid-to-liquid ratio is 1:8,3 hours after-filtration of stirring reaction and washing be to neutral under 85 ℃ temperature, and drying then was 850 ℃ of temperature lower calcinations 0.5 hour, take out cooling, porphyrize gets the white carbon black sample, and this sample contains SiO by analysis
298.3%, whiteness is 93%, and specific surface area is 212m
2/ g.
Embodiment 5:
Adding concentration is 45% phosphoric acid by wet process 200ml in beaker, thin up is behind 250ml, under the continuous stirring condition of normal temperature, add through porphyrize to-100 purpose yellow phosphorus furnace slags 50 grams, stirring reaction is after 0.8 hour under the condition of natural temperature and stirring velocity 500rpm, solid-liquid separation also is washed with water to neutrality with filter residue, add concentration then and be 8% salpeter solution, making solid-to-liquid ratio is 1:6,3 hours after-filtration of stirring reaction and washing be to neutral under 90 ℃ temperature, and drying then was 900 ℃ of temperature lower calcinations 0.5 hour, take out cooling, porphyrize gets the white carbon black sample, and this sample contains SiO by analysis
297.8%, whiteness is 95%, and specific surface area is 208m
2/ g.
Embodiment 6:
Adding concentration is 45% phosphoric acid by wet process 200ml in beaker, thin up is behind 300ml, under the continuous stirring condition of normal temperature, add through porphyrize to-100 purpose yellow phosphorus furnace slags 50 grams, stirring reaction is after 1.0 hours under the condition of natural temperature and stirring velocity 400rpm, solid-liquid separation also is washed with water to neutrality with filter residue, add concentration then and be 10% salpeter solution, making solid-to-liquid ratio is 1:4,2 hours after-filtration of stirring reaction and washing be to neutral under 95 ℃ temperature, and drying then was 900 ℃ of temperature lower calcinations 0.5 hour, take out cooling, porphyrize gets the white carbon black sample, and this sample contains SiO by analysis
298.7%, whiteness is 94%, and specific surface area is 195m
2/ g.
Claims (4)
1. method with preparing high quality silica from yellow phosphorus slag, it is characterized in that: being mixed with phosphoric acid concentration with phosphoric acid by wet process is 25～40% solution, under the continuous stirring condition of normal temperature, add to-100 purpose yellow phosphorus furnace slags through porphyrize, every 100ml phosphoric acid solution adds 10～20g yellow phosphorus furnace slag, at stirring reaction under the natural temperature condition after 0.5～2.0 hour, solid-liquid separation also is washed with water to neutrality with filter residue, add concentration then and be 5～10% salpeter solution, making solid-to-liquid ratio is 1:3～8, also washing is extremely neutral for 2.0～4.0 hours after-filtration of stirring reaction under 70～95 ℃ temperature, drying then, 700～900 ℃ of temperature lower calcinations 0.5～1.0 hour, take out cooling, porphyrize gets the white carbon black product.
2. the method with preparing high quality silica from yellow phosphorus slag according to claim 1 is characterized in that: said yellow phosphorus furnace slag is meant solid slag output when industrial employing high-temperature electric resistance furnace method is produced yellow phosphorus, that obtain through shrend.
3. the method with preparing high quality silica from yellow phosphorus slag according to claim 1 is characterized in that: phosphoric acid by wet process is meant the phosphoric acid by wet process that adopts sulfuric acid extraction phosphorus ore to obtain.
4. the method with preparing high quality silica from yellow phosphorus slag according to claim 1 is characterized in that stirring velocity is 200～500rpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102334533A CN101381082A (en) | 2008-10-17 | 2008-10-17 | Method for preparing high quality silica from yellow phosphorus slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102334533A CN101381082A (en) | 2008-10-17 | 2008-10-17 | Method for preparing high quality silica from yellow phosphorus slag |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101381082A true CN101381082A (en) | 2009-03-11 |
Family
ID=40461168
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008102334533A Pending CN101381082A (en) | 2008-10-17 | 2008-10-17 | Method for preparing high quality silica from yellow phosphorus slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101381082A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850979A (en) * | 2010-04-29 | 2010-10-06 | 昆明理工大学 | Comprehensive utilization method of yellow phosphorus furnace slag |
| CN102616910A (en) * | 2012-03-31 | 2012-08-01 | 昆明理工大学 | Method for preparing inorganic high molecular flocculating agent ferric polysilicate from yellow phosphorus furnace slag |
| CN102815739A (en) * | 2012-08-29 | 2012-12-12 | 攀枝花市坤乃机械制造有限责任公司 | Spiral reactor and method for treating phosphorous slag and waste sulfuric acid |
| CN107902735A (en) * | 2017-10-23 | 2018-04-13 | 昆明理工大学 | A kind of yellow phosphorus furnace slag and coal ash for manufacturing for polysilicate flocculant method |
-
2008
- 2008-10-17 CN CNA2008102334533A patent/CN101381082A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850979A (en) * | 2010-04-29 | 2010-10-06 | 昆明理工大学 | Comprehensive utilization method of yellow phosphorus furnace slag |
| CN101850979B (en) * | 2010-04-29 | 2012-01-25 | 昆明理工大学 | Comprehensive utilization method of yellow phosphorus furnace slag |
| CN102616910A (en) * | 2012-03-31 | 2012-08-01 | 昆明理工大学 | Method for preparing inorganic high molecular flocculating agent ferric polysilicate from yellow phosphorus furnace slag |
| CN102815739A (en) * | 2012-08-29 | 2012-12-12 | 攀枝花市坤乃机械制造有限责任公司 | Spiral reactor and method for treating phosphorous slag and waste sulfuric acid |
| CN107902735A (en) * | 2017-10-23 | 2018-04-13 | 昆明理工大学 | A kind of yellow phosphorus furnace slag and coal ash for manufacturing for polysilicate flocculant method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101850979B (en) | Comprehensive utilization method of yellow phosphorus furnace slag | |
| CN102925956B (en) | Method for preparing calcium sulfate hemihydrate whiskers by taking ardealite as main raw material | |
| CN104495899B (en) | A kind of carbide slag and flyash work in coordination with the method for recycling | |
| CN102234116B (en) | Method for preparing nano white carbon black by utilizing iron tailings | |
| CN104445311B (en) | Clean poly-generation preparation method for flyash with high-content silicon dioxide | |
| CN111188087B (en) | Method for preparing calcium sulfate whisker from phosphogypsum | |
| CN102492994B (en) | Method for preparing calcium sulfate whiskers by using white carbon black industrial wastewater | |
| CN104694761A (en) | Method for extracting vanadium from vanadium solution through vanadium slag sodium salt roasting vanadium extraction process | |
| CN102634843B (en) | Method for preparing micron-sized calcium sulfate particles and crystal whiskers from phosphogypsum | |
| CN103510151B (en) | Method for preparing calcium sulfate whiskers from dolomite | |
| CN102757078B (en) | Method for separating useful components from bayer process red mud | |
| CN104294061A (en) | Technology for extraction of vanadium pentoxide from stone coal mine | |
| CN102424426B (en) | Method for preparing iron oxide red and sodium phosphate by using yellow phosphorus by-product phosphor-iron slag | |
| CN101381077B (en) | Method for preparing dicalcium phosphate from yellow phosphorus slag | |
| CN101381082A (en) | Method for preparing high quality silica from yellow phosphorus slag | |
| CN104512951A (en) | Method for co-production of ploysilicate aluminium ferric sulphate and waste water treatment powder by PAC (poly aluminum chloride) residues | |
| CN113354309A (en) | Modified red mud powder and preparation method thereof | |
| CN109536745B (en) | Method for preparing calcium sulfate whisker and polysilicate flocculant by using medium-low grade phosphate rock powder | |
| CN105350066B (en) | A kind of method that ardealite prepares hemihydrate calcium sulfate crystal whisker | |
| CN105133003A (en) | Production method for wet-process phosphoric acid byproduct alpha semi-hydrated gypsum whiskers | |
| CN111115673A (en) | Method for utilizing all components of caustic sludge | |
| CN107188209A (en) | The method that the hot method of the step alkali of andradite one handles middle-low bauxite production metallurgy grade aluminum oxide | |
| CN102602946B (en) | Method for preparing white carbon black with high specific surface area by recycling wastewater containing sodium sulfate | |
| CN102286783B (en) | New method for preparing calcium sulfate whiskers | |
| CN109399594A (en) | A kind of cleaning method of mid low grade phosphate rock powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090311 |