CN117983637A - Method for cooperatively disposing crushed mica and phosphogypsum solid waste - Google Patents
Method for cooperatively disposing crushed mica and phosphogypsum solid waste Download PDFInfo
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- CN117983637A CN117983637A CN202410235745.XA CN202410235745A CN117983637A CN 117983637 A CN117983637 A CN 117983637A CN 202410235745 A CN202410235745 A CN 202410235745A CN 117983637 A CN117983637 A CN 117983637A
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- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 title claims abstract description 68
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 44
- 239000010445 mica Substances 0.000 title claims abstract description 43
- 239000002910 solid waste Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 49
- 229910052628 phlogopite Inorganic materials 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims description 6
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052627 muscovite Inorganic materials 0.000 claims description 3
- 229910052626 biotite Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 4
- 230000002195 synergetic effect Effects 0.000 claims 4
- 239000012071 phase Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 9
- 230000008859 change Effects 0.000 abstract description 7
- 230000009471 action Effects 0.000 abstract description 6
- 239000008346 aqueous phase Substances 0.000 abstract description 3
- 238000003801 milling Methods 0.000 abstract description 3
- 241000282414 Homo sapiens Species 0.000 abstract description 2
- 239000005431 greenhouse gas Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 15
- 238000002386 leaching Methods 0.000 description 13
- 239000007787 solid Substances 0.000 description 11
- 229910052602 gypsum Inorganic materials 0.000 description 10
- 239000010440 gypsum Substances 0.000 description 9
- 150000004683 dihydrates Chemical class 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 6
- 239000011591 potassium Substances 0.000 description 6
- 229910052700 potassium Inorganic materials 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000003090 exacerbative effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
- B09B3/35—Shredding, crushing or cutting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
- B09B3/38—Stirring or kneading
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/80—Destroying solid waste or transforming solid waste into something useful or harmless involving an extraction step
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for cooperatively disposing crushed mica and phosphogypsum solid waste. Uniformly mixing crushed mica and phosphogypsum according to the mass ratio of 1-2:1-3.5, performing ball milling to obtain mixed powder, adding water into the mixed powder to make the solid-liquid ratio be 1 g:1-100 mL, and performing solid-liquid separation after stirring. According to the invention, through simple mechanical ball milling, the phlogopite and a large amount of solid waste phosphogypsum are mixed according to a proper proportion, the activity of the difficultly leached K + is promoted by a one-step mixed milling method, K + enters into an aqueous phase to promote the pH value in the solution, then CO 2 in the air is absorbed into the solution phase by simple stirring, the main component in the phosphogypsum is CaSO 4.2H2 O, caCO 3 is formed and sealed under the action of lean CO 2 in the air, and the greenhouse gas CO 2 is absorbed, so that the speed of global climate change is helped to human beings.
Description
Technical Field
The invention belongs to the field of solid waste treatment, and particularly relates to a method for cooperatively disposing broken mica and phosphogypsum solid waste.
Background
Phosphogypsum (PG) is an industrial by-product of the industrial wet process for the preparation of phosphoric acid and fertilizer, where about 4.5 to 5 tons of PG will be produced per 1 ton of phosphoric acid produced. The annual yield of PG worldwide is currently up to 2.8 billion tons per year, with incomplete statistics. The PG has complex components, the main component is gypsum dihydrate (CaSO 4·2H2 O), and the harmful impurities such as phosphorus, fluorine, organic matters and the like remained in the storage process have great negative influence on the resource utilization and the environment of the PG. Worse still, infiltration of rain water can result in PG releasing a large amount of contaminants when it encounters rain. For operation of PG storage, security risks require strict measures. On the other hand, mica is widely applied to chemical industries such as building material industry, fire-fighting industry, fire extinguishing agent, pearlescent pigment and the like. Whereas among the micas, muscovite and Phlogopite (PE) may contain about 10% potassium, they are widely present around the world. However, excessive mica crushing is a common phenomenon that a large amount of waste mica is generated in the mica processing industry, the utilization rate of the crushed mica in industrial life is greatly reduced, a large amount of piled crushed mica becomes solid waste, and the waste of resources is caused and meanwhile the waste mica is stored as the solid waste. The huge solid waste is piled up, so that the land is occupied, and soil damage, even water, atmosphere and the like are influenced.
Carbon dioxide is mainly derived from burning fossil fuels such as coal, oil and natural gas, and industrial processes and agricultural activities. Carbon dioxide generated by these activities is released into the atmosphere, exacerbating the greenhouse effect, leading to an increase in global air temperature, and it is desirable to use the solid waste to fix carbon dioxide in the air. Aiming at the above-mentioned mica crushed aggregates and phosphogypsum solid waste background, a practical and feasible scheme capable of simultaneously disposing the solid waste phlogopite crushed aggregates and phosphogypsum and fixing CO 2 in the air is found to have profound significance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for cooperatively disposing crushed mica and phosphogypsum solid waste. The invention provides a method for mixing and grinding crushed mica and phosphogypsum by a simple mechanochemical activation method, wherein strong interfacial reaction occurs between the two phases by the ball milling action of mechanochemistry, so that the potassium activity between calcium and phlogopite in the phosphogypsum is promoted, finally, K in the phlogopite is completely leached out by stirring with simple water and under the action of thin CO 2 in natural air, the pH of a solution of K + in an aqueous phase is increased to be favorable for absorption of CO 2, and the main component CaSO 4·2H2 O in the phosphogypsum is converted into a CaCO 3 form to be stored and fixed.
The aim of the invention is achieved by the following technical scheme:
A method for cooperatively disposing crushed mica and phosphogypsum solid waste comprises the following steps: uniformly mixing crushed mica and phosphogypsum according to the mass ratio of 1-2:1-3.5, performing ball milling to obtain mixed powder, adding water into the mixed powder to make the solid-liquid ratio be 1 g:1-100 mL, and performing solid-liquid separation after stirring. The separated solid components mainly comprise silicate slag and calcium carbonate, wherein the calcium carbonate is generated by absorbing CO 2 in the air by phosphogypsum; the main component of the separated liquid is K 2SO4, K + containing ions, and the recovered K 2SO4 can be used in the agricultural, industrial and medical fields.
Preferably, the particle size of the crushed mica is 2-5 mm.
Preferably, the crushed mica is at least one of crushed phlogopite, muscovite and biotite.
Preferably, the mass ratio of the crushed mica to the phosphogypsum is 2:1, 1:2 and 1:3.5.
Preferably, the rotation speed of the ball milling is 300-600 rpm, and the time of the ball milling is 2-6 h. The interface reaction between the two phases of mica and phosphogypsum is achieved by controlling the proper ball milling rotating speed, and finally the purpose of treating solid waste is achieved.
Preferably, the ball milling medium is ZrO 2, and the ball ratio is 35:1.
Preferably, the stirring speed is 400rpm, and the stirring time is 1-72 h. The solution containing high-concentration K + is obtained under the stirring action, and the potassium fertilizer can be prepared by one-step evaporation, so that the high-temperature strong acid process brought by mica potassium extraction can be avoided, and the subsequent treatment of acidic wastewater can be lightened. In addition, the high concentration K + released from the solution can enhance the alkalinity of the solution, which is favorable for adsorbing lean CO 2 in the air and further fixing the lean CO 2 in the air.
Preferably, the solid-liquid separation mode is filtration or suction filtration.
The chemical reaction formula related by the invention is as follows:
2KMg3(AlSi3O10)(OH)2+CaSO4·2H2O+CO2＝K2SO4+xMgOyAl2O3zSiO2+CaCO3+2H2O
The invention relates to the atomic activity of the interface between two ores, calcium becomes CaCO 3 finally instead of being stored between mica layers under the ion exchange effect, the chemical formula can also show that the dissolution of potassium improves the pH value, and the rest product is silicate slag instead of simple ion replacement after calcium is added.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, through simple mechanical ball milling, the phlogopite and a large amount of solid waste phosphogypsum are mixed according to a proper proportion, the activity of the difficultly leached K + is promoted by a one-step mixed milling method, K + enters into an aqueous phase to promote the pH value in the solution, then CO 2 in the air is absorbed into the solution phase by simple stirring, the main component in the phosphogypsum is CaSO 4.2H2 O, caCO 3 is formed and sealed under the action of lean CO 2 in the air, and the greenhouse gas CO 2 is absorbed, so that the speed of global climate change is helped to human beings.
(2) The invention can simply and efficiently treat the phlogopite and phosphogypsum solid waste synchronously, fix CO 2 in the air at normal temperature and normal pressure, and finally recover and subsequently use the ionic K + in the solution.
Drawings
FIG. 1 shows XRD diffraction patterns of phosphogypsum and phlogopite used in the present invention as they are.
Fig. 2 is an XRD diffractogram of the mixed powder obtained after ball milling of examples 1 to 3, wherein PE represents phlogopite.
FIG. 3 is a graph showing the comparative column of the leaching rate of K + in the liquid obtained after solid-liquid separation of examples 1to 3 and comparative examples 1to 6, wherein the Mixed corresponds to examples 1to 3, co-milling corresponds to examples 1to 3, and Raw corresponds to examples 4 to 6.
FIG. 4 is a graph showing the change in leaching rate and pH of K + in the liquid obtained after solid-liquid separation in examples 4 to 6, wherein PE represents phlogopite and CSH represents phosphogypsum.
FIG. 5 is a graph showing the change in leaching rate and pH of K + in the liquid obtained after solid-liquid separation in examples 1 to 3, wherein PE represents phlogopite and CSH represents phosphogypsum.
FIG. 6 is an XRD diffraction pattern of the solid obtained by filtration separation after stirring for 3d in example 2.
FIG. 7 is an infrared spectrum of the solid obtained by filtration after stirring for 3d in example 2.
FIG. 8 is a graph comparing XPS full spectrum with K2p spectrum of the solid filtered before and after 3d of agitation in example 2.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The phlogopite used in examples and comparative examples was from Guangxi and Xinghai mining development Co., ltd, and phosphogypsum was from Hubei Jinmen Dayang group Co., ltd. The samples were all further purified or otherwise processed. Table 1 and Table 2 show the chemical composition of the solid waste of crushed phlogopite and phosphogypsum, respectively, FIG. 1 shows XRD patterns of phlogopite and phosphogypsum, and FIG. 1 shows phase patterns of almost pure-phase phlogopite and dihydrate gypsum, respectively.
TABLE 1 list of chemical compositions of phlogopite
TABLE 2 chemical composition list of phosphogypsum
Example 1
A method for cooperatively disposing crushed mica and phosphogypsum solid waste comprises the following steps:
Crushed phlogopite and phosphogypsum are mixed according to a ratio of 2:1, and then ball milling is carried out after the evenly mixed mass ratio, wherein the ball milling rotating speed is 600rpm, the ball milling time is 2 hours, the ball milling medium is zirconium balls with the diameter of 15mm, and the ball ratio is 35:1, obtaining a mixed powder, and then adding water to the mixed powder so that the solid-to-liquid ratio is 1g:25mL, stirred at 400rpm for 3d, and finally filtered to separate the solid and liquid.
Example 2
A method for cooperatively disposing crushed mica and phosphogypsum solid waste comprises the following steps:
On the basis of example 1, "phlogopite and phosphogypsum were mixed according to a ratio of 2:1 is uniformly mixed with crushed phlogopite and phosphogypsum according to the mass ratio of 1:2, uniformly mixing the components according to the mass ratio, and keeping other steps unchanged.
Example 3
A method for cooperatively disposing crushed mica and phosphogypsum solid waste comprises the following steps:
On the basis of example 1, "phlogopite and phosphogypsum were mixed according to a ratio of 2:1 is uniformly mixed with crushed phlogopite and phosphogypsum according to the mass ratio of 1:3.5, mixing uniformly, and keeping other steps unchanged.
Example 4
A method for cooperatively disposing crushed mica and phosphogypsum solid waste comprises the following steps:
based on example 1, "rotation speed of ball milling was 600rpm," ball milling time was 2h "instead of" rotation speed of ball milling was 300rpm, "ball milling time was 2h," and other steps were unchanged.
Example 5
A method for cooperatively disposing crushed mica and phosphogypsum solid waste comprises the following steps:
Based on example 2, "rotation speed of ball milling was 600rpm," ball milling time was 2h "instead of" rotation speed of ball milling was 300rpm, "ball milling time was 2h," and other steps were unchanged.
Example 6
A method for cooperatively disposing crushed mica and phosphogypsum solid waste comprises the following steps:
Based on example 3, "rotation speed of ball milling was 600rpm," ball milling time was 2h "instead of" rotation speed of ball milling was 300rpm, "ball milling time was 2h," and other steps were unchanged.
Comparative example 1
2G of phlogopite and 1g of phosphogypsum are respectively weighed and subjected to independent ball milling, the ball milling rotating speed is 600rpm, the ball milling time is 2 hours, the ball milling medium is zirconium balls with the diameter of 15mm, and the ball ratio is 35:1, obtaining a mixed powder, and then adding water to the mixed powder so that the solid-to-liquid ratio is 1g:25mL, stirred at 400rpm for 3d, and finally filtered to separate the solid and liquid.
Comparative example 2
1G of phlogopite and 2g of phosphogypsum are respectively weighed and subjected to independent ball milling, the ball milling rotating speed is 600rpm, the ball milling time is 2 hours, the ball milling medium is zirconium balls with the diameter of 15mm, and the ball ratios are all unified to be 35:1, obtaining a mixed powder, and then adding water to the mixed powder so that the solid-to-liquid ratio is 1g:25mL, stirred at 400rpm for 3d, and finally filtered to separate the solid and liquid.
Comparative example 3
1G of phlogopite and 3.5g of phosphogypsum are respectively weighed and subjected to independent ball milling, the ball milling speed is 600rpm, the ball milling time is 2 hours, the ball milling medium is ZrO 2, and the ball-to-ball ratio is 35:1, obtaining a mixed powder, and then adding water to the mixed powder so that the solid-to-liquid ratio is 1g:25mL, stirred at 400rpm for 3d, and finally filtered to separate the solid and liquid.
Comparative example 4
The ball milling step was omitted on the basis of comparative 1, the other steps being unchanged.
Comparative example 5
The ball milling step was omitted on the basis of comparative 1, the other steps being unchanged.
Comparative example 6
The ball milling step was omitted on the basis of comparative 1, the other steps being unchanged.
Fig. 1 shows XRD diffractograms of phosphogypsum and phlogopite as such employed in the present invention, as we can see from fig. 1: the crushed phlogopite and phosphogypsum are nearly pure phases.
Fig. 2 shows XRD diffractograms of the mixed powders obtained after ball milling for examples 1 to 3, as can be seen from fig. 2: the phase of the product changed significantly, at 2:1 and 1:2, the phlogopite and the dihydrate gypsum are subjected to chemical reaction under the condition of being close to an amorphous state, and the dosage of the phosphogypsum is continuously increased, so that the phenomenon that the dihydrate gypsum is too much can be seen, all the dihydrate gypsum can not be absorbed, and the residual dihydrate gypsum is gradually converted into hemihydrate gypsum under the action of mechanical force, so that the ratio of the dihydrate gypsum to the dihydrate gypsum is 1: and 3.5, into semi-hydrated gypsum.
The concentrations of K + in the liquids obtained after the solid-liquid separation of examples 1 to 3 and comparative examples 1 to 6 were examined using atomic absorption spectroscopy (AA 6880) to obtain the leaching rate of K + thereof, the examination results are shown in fig. 3, and it can be seen from fig. 3: at each ratio of ball milling alone (comparative examples 1-3) and not ball milling (comparative examples 4-6), the concentration variation of K + was not significant, the overall K + leaching rate was below 20%, while the phlogopite and phosphogypsum were found at 2:1,1:2 and 1:3.5, the leaching rate of K + of the co-ground sample under three conditions reaches 35.2%, 90.25% and 91%, which proves that chemical reaction occurs between phlogopite and calcium sulfate dihydrate in the co-grinding process, and the leaching efficiency of K + in the phlogopite becomes high along with the adjustment of the proportion, which is beneficial to the subsequent solution pH promotion and carbon fixation effect.
With the extension of the stirring time, 1mL of the solid-liquid mixture was withdrawn by a syringe at the time nodes of 2h,12h,24h and 48h, and then filtered by a 0.22um filter, and whether the K + after the reaction was changed was detected, and then whether the pH was changed was observed at the time nodes of 2h,12h,24h,36h,48h and 72 h. Examples 4 to 6 the change in leaching rate and pH of K + in the liquid obtained after solid-liquid separation, the detection results are shown in fig. 4, and it can be seen from fig. 4: under the condition of ball milling rotating speed of 300rpm, the proportion is 1: and 3.5, the leaching rate of K + in the solution gradually increases, and finally the leaching rate of K + in the sample after 48 hours is approximately 20%. The sample changes at the other two ratios were not significant enough, indicating insufficient reaction strength between the two at a ball mill speed of 300 rpm. The corresponding pH change can be seen that the pH value of the sample in the solution after ball milling activation is alkaline, and the proportion is 2:1,1:2 and 1: the pH at three conditions of 3.5 was approximately 9.4,9.48 and 8.4, respectively. Along with the adsorption of CO 2 in the air, the pH in the solution gradually decreases, which indicates that the three substances have different degrees of adsorption on CO 2.
Referring to the detection method of fig. 4, the change in leaching rate and pH of K + in the liquid obtained after the solid-liquid separation of examples 1 to 3 was detected with the extension of the stirring time, and the detection result was shown in fig. 5, and it can be seen from fig. 5: increasing the ball milling speed to 600rpm greatly increased the leaching rate of sample K +, while the corresponding initial pH values were 9.52, 10.2 and 9.02, respectively, indicating that the mass ratio of phlogopite to phosphogypsum was 1:2 is most beneficial to leaching the sample K + under the condition of 2, and meanwhile, the acid calcium sulfate in the ratio does not excessively influence the alkalinity released by the product, thereby being beneficial to raising the pH value of the solution and also being beneficial to capturing CO 2 in the follow-up process. The corresponding pH of each proportion of sample at 600rpm also decreases with time, because K + in the product dissolves out in a large amount, resulting in rapid increase of alkalinity in the solution, while as CO 2 in the adsorbed air increases, the pH of the solution gradually decreases and finally becomes stable.
Example 2 after stirring for 3d, the XRD diffraction pattern of the solid obtained by filtration separation is shown in FIG. 6, and it can be seen from FIG. 6 that the XRD main phase of the product residue after the reaction changes to CaCO 3. The infrared spectrum of the solid obtained by the filtration is shown in fig. 7, and can be seen from fig. 7: significant stretching and bending vibration peaks of CO 3 2- can be seen at 1428cm -1 and 873cm -1, which indicate that CO 2 in the air is adsorbed on the sample surface and eventually gradually converted to the form of CO 3 2-.
XPS full spectrum and K2p spectrum of the solid filtered before and after stirring for 3d as described in example 2 were examined, and the examination results are shown in FIG. 8, and can be seen from FIG. 8: the K2p in the product after adsorption of carbon is significantly reduced, since during stirring, K + is largely eluted from the solid phase and enters the liquid phase, eventually leading to a reduction of potassium in the residue phase.
In summary, the invention provides a method for not only absorbing the solid waste phosphogypsum to obtain K + resource, but also effectively sealing and storing CO 2 in the air, and has better application prospect.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any of various other corresponding changes and modifications made according to the technical idea of the present invention should be included in the scope of the claims of the present invention.
Claims (10)
1. The method for cooperatively disposing the crushed mica and phosphogypsum solid waste is characterized by comprising the following steps: uniformly mixing crushed mica and phosphogypsum according to the mass ratio of 1-2:1-3.5, performing ball milling to obtain mixed powder, adding water into the mixed powder to make the solid-liquid ratio be 1 g:1-100 mL, and performing solid-liquid separation after stirring.
2. The method for cooperatively disposing of crushed mica and phosphogypsum solid waste according to claim 1, wherein the mass ratio of the crushed mica to the phosphogypsum is 2:1, 1:2 and 1:3.5.
3. The method for the synergistic disposal of crushed mica and phosphogypsum solid waste as claimed in claim 1, wherein water is added to the mixed powder so that the solid-to-liquid ratio is 1g:25ml.
4. A method for the synergistic disposal of crushed mica and phosphogypsum solid waste as claimed in any one of claims 1 to 3, characterized in that the particle size of crushed mica is 2 to 5mm.
5. The method for co-disposal of crushed mica and phosphogypsum solid waste according to claim 4, wherein the crushed mica is at least one of crushed phlogopite, crushed muscovite and crushed biotite.
6. A method for the synergistic disposal of crushed mica and phosphogypsum solid waste as claimed in any one of claims 1 to 3, characterized in that the rotational speed of the ball mill is 300 to 600rpm and the time of the ball mill is 2 to 6 hours.
7. The method for cooperatively disposing of crushed mica and phosphogypsum solid waste according to claim 6, wherein the ball milling medium is zirconia balls with a ball ratio of 35:1.
8. The method for co-disposal of crushed mica and phosphogypsum solid waste according to claim 7, wherein the diameter of the zirconia balls is 15mm.
9. A method for the synergistic disposal of crushed mica and phosphogypsum solid waste as claimed in any one of claims 1 to 3, characterized in that the stirring speed is 400rpm and the stirring time is 1 to 72 hours.
10. The method for cooperatively disposing of crushed mica and phosphogypsum solid waste according to claim 1, wherein the solid-liquid separation mode is filtration or suction filtration.
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