CN109455738B - Process for preparing high-quality industrial salt by utilizing garbage fly ash - Google Patents
Process for preparing high-quality industrial salt by utilizing garbage fly ash Download PDFInfo
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- CN109455738B CN109455738B CN201811620761.1A CN201811620761A CN109455738B CN 109455738 B CN109455738 B CN 109455738B CN 201811620761 A CN201811620761 A CN 201811620761A CN 109455738 B CN109455738 B CN 109455738B
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- 239000010881 fly ash Substances 0.000 title claims abstract description 124
- 150000003839 salts Chemical class 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 207
- 238000005406 washing Methods 0.000 claims abstract description 191
- 238000000926 separation method Methods 0.000 claims abstract description 113
- 239000007788 liquid Substances 0.000 claims abstract description 105
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 45
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 44
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical class [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 40
- 239000007787 solid Substances 0.000 claims abstract description 40
- 238000002425 crystallisation Methods 0.000 claims abstract description 38
- 230000008025 crystallization Effects 0.000 claims abstract description 38
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 239000011780 sodium chloride Substances 0.000 claims abstract description 22
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001103 potassium chloride Substances 0.000 claims abstract description 16
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 16
- 238000007670 refining Methods 0.000 claims abstract description 14
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011575 calcium Substances 0.000 claims abstract description 10
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 10
- 239000012452 mother liquor Substances 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 50
- 238000001223 reverse osmosis Methods 0.000 claims description 27
- 229910021529 ammonia Inorganic materials 0.000 claims description 25
- 239000012528 membrane Substances 0.000 claims description 25
- 238000010612 desalination reaction Methods 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 24
- 238000001238 wet grinding Methods 0.000 claims description 21
- 238000004064 recycling Methods 0.000 claims description 19
- 238000001704 evaporation Methods 0.000 claims description 17
- 230000008020 evaporation Effects 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 17
- 239000002699 waste material Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 12
- 239000004568 cement Substances 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 238000004042 decolorization Methods 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 229960002089 ferrous chloride Drugs 0.000 claims description 6
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 6
- 230000033116 oxidation-reduction process Effects 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005273 aeration Methods 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 24
- 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 abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052700 potassium Inorganic materials 0.000 abstract description 6
- 239000011591 potassium Substances 0.000 abstract description 6
- 229910052708 sodium Inorganic materials 0.000 abstract description 6
- 239000011734 sodium Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 18
- 238000005265 energy consumption Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000003480 eluent Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011278 co-treatment Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
- C01D3/16—Purification by precipitation or adsorption
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/22—Preparation in the form of granules, pieces, or other shaped products
- C01D3/24—Influencing the crystallisation process
Abstract
The invention discloses a process for preparing high-quality industrial salt by utilizing garbage fly ash, which comprises the steps of fly ash water washing, heavy metal removal, decoloration, calcium removal, evaporative crystallization and potassium-sodium separation, wherein when the density of mother liquor reaches 1.15-1.25 g/cm during the evaporative crystallization 3 And (3) performing primary centrifugal separation, collecting sodium chloride subjected to primary centrifugal separation, cooling and crystallizing liquid subjected to primary centrifugal separation, performing secondary centrifugal separation after cooling and crystallizing, re-performing heavy metal removal on liquid subjected to secondary centrifugal separation, refining the solid subjected to secondary centrifugal separation by taking saturated potassium chloride solution as refined washing liquid, performing tertiary centrifugal separation after refining, and collecting potassium chloride subjected to tertiary centrifugal separation. The invention can effectively separate potassium and sodium by an industrialized method, and can ensure that the content of salt heavy metals produced by the fly ash of garbage with different sources is within national standard requirements, and the quality of the produced industrial salt is stable.
Description
Technical Field
The invention relates to the technical field of environmental protection, in particular to a process for preparing high-quality industrial salt by utilizing garbage fly ash.
Background
With the rapid development of town, the urban domestic garbage yield of China is increased year by year, from 1.89 million in 2013 to 2.06 million tons in 2015, and the garbage incineration disposal amount of China is increased year by year due to the advantages of capacity reduction, weight reduction, energy recovery and the like of garbage incineration. Fly ash is an inevitable product of garbage incineration, and accounts for about 3-5% of the amount of incineration garbage. According to the calculation, the fly ash generated by garbage incineration is 10000-20000 tons/day in the future. Such a large amount of fly ash is produced, so that how to safely and effectively dispose of incineration fly ash becomes an environmental and social problem to be solved urgently.
Fly ash is a fine particulate matter collected in a flue gas cleaning system, including fly ash produced when the flue gas is treated with chemicals, and is present in the ash in an amount of about 10% to 20%. The fly ash is generally gray or dark gray, the grain diameter is less than 300 mu m, the water content is 10-23% and the burning rate is 34-51%, the fly ash is easy to frost heaving and difficult to compact, and the grain form is in irregular shapes such as rod shape, multi-angle shape, cotton floccule shape, sphere shape and the like. Meanwhile, the incineration fly ash contains harmful substances such as dioxin and heavy metals, and the incineration fly ash is regulated according to the domestic garbage incineration pollution control standard (GB 1885-2014): "fly ash from incineration of household garbage should be managed according to dangerous waste". Therefore, fly ash must be collected separately, and must not be mixed with household garbage, incineration residues, etc., nor with other hazardous wastes.
The applicant adopts the process design in the early stage to prepare the snow-melting agent by taking the waste fly ash as the raw material, the components of the snow-melting agent mainly comprise calcium chloride, potassium chloride and sodium chloride, the production of the snow-melting agent forms huge social and economic efficiency, how to separate potassium and sodium to form larger economic benefits, how to ensure that the produced sodium chloride and potassium chloride meet the national standard requirements, the inventor carries out further technical improvement around the two problems, the separation of potassium and sodium is a technical difficulty, the salt preparation of the waste fly ash is a new industry, no prior technical reference is needed, the special design is needed according to the process characteristics, the heavy metal content fluctuation in the salt is large due to the variety of the fly ash raw materials, certain heavy metal indexes are easy to exceed the standard, the national standard requirements are not met, the potential safety hazard exists, and how to ensure that the heavy metal content of the salt produced by the waste fly ash with different sources is within the national standard requirements, and the product with stable quality is also a problem to be solved.
Disclosure of Invention
The invention aims to solve the problems that heavy metals are easy to exceed standard and potassium and sodium are not easy to separate in the production of industrial salt by using fly ash, and provides a process for preparing high-quality industrial salt by using waste fly ash, which can effectively separate potassium and sodium by using an industrialized method, ensure that the content of the heavy metals in the salt produced by the waste fly ash from different sources is within national standard requirements, and ensure that the quality of the produced industrial salt is stable.
The technical scheme adopted for solving the technical problems is as follows:
a process for preparing high-quality industrial salt by utilizing garbage fly ash comprises the steps of fly ash water washing, heavy metal removal, decoloration, calcium removal, evaporative crystallization and potassium-sodium separation, wherein when the density of mother liquor reaches 1.15-1.25 g/cm during the evaporative crystallization 3 And then, carrying out primary centrifugal separation, and collecting the solid obtained by the primary centrifugal separation, namely a sodium chloride product, wherein the liquid obtained by the primary centrifugal separation enters a potassium-sodium separation step, and the potassium-sodium separation step specifically comprises the following steps: cooling and crystallizing the liquid subjected to primary centrifugal separation, performing secondary centrifugal separation after cooling and crystallizing, re-entering the heavy metal removal step by the liquid subjected to secondary centrifugal separation, refining the solid subjected to secondary centrifugal separation by taking saturated potassium chloride solution as refined washing liquid, performing tertiary centrifugal separation after refining, collecting the solid subjected to tertiary centrifugal separation, namely a potassium chloride product, and recycling the liquid subjected to tertiary centrifugal separation as refined washing liquid.
Although the heavy metal removal step can remove most of heavy metals, the heavy metals still enter the subsequent step and are carried out into the salt, so that the heavy metals in the salt exceed the standard.
Compared with the technology before improvement, the invention has obviously reduced evaporation capacity of the evaporative crystallization, the evaporation capacity is about one fifth of the original evaporation capacity, and the density of the mother liquor reaches 1.15-1.25 g/cm 3 At this time, centrifugal separation is performed, and at this time, the precipitation of sodium chloride is started, and at this time, the concentration of heavy metals in the mother liquor is low, and the water content of the centrifugally separated salt is fixed, so that the heavy metal content of the obtained sodium chloride is remarkably reduced, about one fifth of that of the original process. And (3) after primary centrifugal separation, the liquid containing sodium chloride and potassium chloride enters cooling crystallization, the potassium chloride is separated out independently by using cooling water, and then the liquid with the concentration of heavy metal rising after evaporation crystallization is conveyed back to the heavy metal removal step for reprocessing, so that the heavy metal can be removed continuously. A small amount of sodium chloride is carried out in the potassium chloride separated by the secondary centrifugation, so that the saturated potassium chloride solution is used as a refining washing liquid to refine the potassium chloride crystal, therebyThe finished product potassium chloride is obtained, the refined washing liquid can be recycled as the washing liquid again after three times of centrifugal separation, when the sodium chloride content in the washing liquid is more than 20%, the circulating washing liquid can not produce better refining effect, and the circulating washing liquid is sent back to the cooling crystallization step to recycle the potassium chloride and then is refined by using a new saturated potassium chloride solution.
The temperature of the cooling water for cooling and crystallizing is 5-30 ℃.
When the sodium chloride content in the liquid of the third centrifugal separation is above 20%, the liquid of the third centrifugal separation is combined with the liquid of the first centrifugal separation, and cooling crystallization is carried out again.
As a preferable scheme, the fly ash washing is three-stage countercurrent washing, comprising a first-stage washing, a second-stage washing and a third-stage washing;
solid-liquid separation is carried out after the first-stage water washing, the solid is crushed and then enters the second-stage water washing, the liquid enters the heavy metal removal step, and the mass ratio of the fly ash of the first-stage water washing to the water is 1:1;
solid-liquid separation is carried out after the second-stage water washing, the solid is crushed and then enters the third-stage water washing, and the liquid is used as a water source for the first-stage water washing;
and after the third-stage water washing, solid-liquid separation is carried out, the solid is sent to a cement kiln for cooperative treatment, the liquid adopts reverse osmosis membrane desalination treatment, concentrated water generated by the reverse osmosis membrane desalination treatment is used as a water source of the second-stage water washing, clear water generated by the reverse osmosis membrane desalination treatment is used as a water source of the third-stage water washing for recycling, and the mass ratio of fly ash and water in the third-stage water washing is=1:3.
For the fly ash after multi-stage water washing, such as three-stage countercurrent water washing, the chloride ion content can not meet the requirement of the cement kiln collaborative treatment, so that the consumption of water for water washing is increased to reduce the chloride ion content in the fly ash, a large amount of water washing eluent is caused to enter an evaporation crystallization step, the energy consumption for forming clear water for recycling through evaporation crystallization is greatly increased, and on the premise of not changing the existing equipment, no effective solution exists in the field. Although the chloride ion content in the fly ash can be reduced by increasing the washing stage number, the equipment and the process are required to be adjusted and increased, and the operation difficulty is high. Through long-term research, the inventor explores an effective solving way, increases the water consumption on the premise of not increasing the stage number of water washing, increases a reverse osmosis membrane desalination scheme in the final stage of water washing, and can recycle most of clean water through reverse osmosis membrane desalination, and the recycling cost is low, the energy consumption is low, and the effect of reducing the energy consumption is achieved by reducing the chloride ion content in fly ash to meet the cooperative treatment requirement of a cement kiln without increasing eluent entering an evaporation crystallization step. The reverse osmosis membrane desalination scheme is added in the final stage of water washing, mainly because the salt content in the fly ash is low in the final stage of water washing, and the eluent has low salt content under the condition of increasing water consumption, so that the reverse osmosis membrane can be well born and used. The conventional thinking manner for those skilled in the art will simply think that reverse osmosis membranes are used before the evaporative crystallization operation, however, the reverse osmosis membranes cannot be used at all because of the excessively high salt content of the liquid before the evaporative crystallization operation, and therefore, the reverse osmosis membrane desalination scheme has never been considered for use in the treatment of waste fly ash.
For the conventional three-stage countercurrent water washing, the chloride ion content can meet the cooperative treatment requirement of the cement kiln, and by adopting the solution of the invention, the solution can be achieved by only 1-2-stage water washing when the same requirement is met, and the process can be effectively shortened, and the equipment maintenance cost is reduced.
As another preferable scheme, before the fly ash washing step, wet grinding is carried out on the fly ash, and slurry formed after the wet grinding is sent into the fly ash washing step again; the fly ash washing is three-stage countercurrent washing, including first-stage washing, second-stage washing and third-stage washing;
solid-liquid separation is carried out after the first-stage water washing, the solid is crushed and then enters the second-stage water washing, the liquid enters the heavy metal removal step, and the mass ratio of the sum of the water consumption of the first-stage water washing and the water consumption of the wet grinding of the fly ash to the fly ash is=1:1;
solid-liquid separation is carried out after the second-stage water washing, the solid is crushed and then enters the third-stage water washing, one part of liquid is used as a water source for wet grinding of the fly ash, and the rest part of liquid is used as a water source for the first-stage water washing, wherein the mass ratio of the fly ash to the water is (1:0.3-0.5) when the fly ash is subjected to wet grinding;
and after the third-stage water washing, solid-liquid separation is carried out, the solid is sent to a cement kiln for cooperative treatment, the liquid adopts reverse osmosis membrane desalination treatment, concentrated water generated by the reverse osmosis membrane desalination treatment is used as a water source of the second-stage water washing, clear water generated by the reverse osmosis membrane desalination treatment is used as a water source of the third-stage water washing for recycling, and the mass ratio of fly ash and water in the third-stage water washing is=1:3.
Because the fly ash comes from the garbage incineration, a certain proportion of aggregated particles which are difficult to scatter are formed in the fly ash production process, the fly ash is directly mixed with water in a solid-liquid mode, the mixing is uneven, chloride ions in the fly ash particles are difficult to dissolve out, meanwhile, when the fly ash is washed with water, the fly ash particles are easy to agglomerate and agglomerate while stirring, and the chloride ions are difficult to dissolve out, so that the water washing stage number is often increased after the fly ash is washed with water for several stages, the chloride ion content in the fly ash is not further reduced, and the co-treatment of the fly ash entering a cement kiln is greatly influenced. The inventor researches and develops a solution how to solve the problem, and the inventor firstly grinds fly ash to form homogenate by introducing wet grinding before the first-stage water washing, and can fully disperse aggregated particles which are difficult to disperse in the fly ash in the wet grinding process, so that chloride ions are convenient to dissolve out, and the homogenate formed by the wet grinding enters the water washing, is more uniform in mixing and is difficult to agglomerate in the water washing process, so that the dissolution rate of the chloride ions can be effectively improved.
The mass ratio of the total water to the fly ash in the first-stage water washing is=1:1, wherein 0.3-0.5 part of water comes from wet grinding, and the added water in the first-stage water washing only needs to be supplemented to 1 part of water on the basis of 0.3-0.5 part of water. The wet grinding water comes from the liquid part of solid-liquid separation after the second-stage water washing, is recycled, and is free from additional addition, energy-saving and emission-reducing.
The invention strictly controls the mass ratio of the first-stage water washing fly ash to water (total water amount) to be 1:1, so that the water entering the evaporative crystallization always maintains to reach the minimum requirement that the fly ash can be stirred for water washing, and the burden is not increased for the subsequent evaporative crystallization. The mass ratio of the third-stage water-washed fly ash to water=1:3, and the fly ash can smoothly run by fine adjustment of the process to meet the mass ratio of the fly ash to water=1:1 during the first-stage water washing.
And in the three-stage countercurrent washing process, aeration stirring is carried out to remove ammonia from the fly ash, and an ammonia recovery port is arranged above a washing pool of each stage of washing, so that ammonia is sent to an ammonia absorption tower for absorption, and the formed ammonia is recycled to the power plant for denitration.
Distilled water generated in the evaporation crystallization step is used as a water source for third-stage water washing for recycling.
The heavy metal removal step comprises the following steps: slowly adding sodium sulfide solution into the filtrate obtained by washing fly ash under the stirring condition until the oxidation-reduction potential of the system reaches 0 to 50mV below zero, and then adding ferrous chloride solution until the oxidation-reduction potential of the system reaches 100 to 150mV below zero; the mass concentration of the sodium sulfide solution is 2-5%; the mass concentration of the ferrous chloride solution is 3-10%.
The decolorization is to add active carbon into filtrate after heavy metal removal, the dosage of the active carbon is one to five thousandths of the weight of the filtrate, the filtrate is stirred for 3 to 10 minutes, the filtrate is filtered, and the filter residue is collected and stored as dangerous waste, and the filtrate enters the next step of treatment.
And the calcium removal is to add sodium carbonate into the filtrate obtained after decolorization, stir for 10-20min, filter, collect calcium carbonate of solid part, and the filtrate enters the next treatment.
The beneficial effects of the invention are as follows:
1. the potassium and sodium can be effectively separated by an industrialized method, so that the content of salt heavy metals produced by the waste fly ash from different sources is ensured to be within national standard requirements, and the quality of the produced industrial salt is stable.
2. On the premise of not increasing the washing stage number, the energy consumption during evaporation and crystallization can be greatly reduced, and the production cost is reduced; the washing effect same as that of the prior art is achieved, the washing stage number can be reduced, the process is effectively shortened, and the equipment maintenance cost is reduced.
3. Can effectively improve the dissolution rate of chloride ions in the fly ash, and further reduces the lower limit of the content of chloride ions in the fly ash which cannot be reduced by multi-stage water washing.
Drawings
Fig. 1 is a first process flow diagram of the present invention.
Fig. 2 is a second process flow diagram of the present invention.
Fig. 3 is a third process flow diagram of the present invention.
Detailed Description
The technical scheme of the invention is further specifically described by the following specific examples.
In the present invention, the materials and equipment used are commercially available or commonly used in the art, unless otherwise specified. The methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
a process (figure 1) for preparing high-quality industrial salt by utilizing garbage fly ash comprises the steps of fly ash water washing, heavy metal removal, decoloration, calcium removal, evaporative crystallization and potassium-sodium separation, and specifically comprises the following steps:
the fly ash washing is three-stage countercurrent washing, including first-stage washing, second-stage washing and third-stage washing;
solid-liquid separation is carried out after the first-stage water washing, the solid is crushed and then enters the second-stage water washing, the liquid enters the heavy metal removal step, and the mass ratio of the fly ash of the first-stage water washing to the water is 1:1;
solid-liquid separation is carried out after the second-stage water washing, the solid is crushed and then enters the third-stage water washing, and the liquid is used as a water source for the first-stage water washing;
solid-liquid separation is carried out after the third-stage water washing, solids (the chloride ion content is about 0.95 percent) are sent to a cement kiln for cooperative treatment, reverse osmosis membrane desalination treatment is adopted for liquid, concentrated water generated by the reverse osmosis membrane desalination treatment is used as a water source of the second-stage water washing, clear water generated by the reverse osmosis membrane desalination treatment is used as the water source of the third-stage water washing for recycling, and the mass ratio of fly ash and water in the third-stage water washing is=1:3; and in the three-stage countercurrent washing process, aeration stirring is carried out to remove ammonia from the fly ash, and an ammonia recovery port is arranged above a washing pool of each stage of washing, so that ammonia is sent to an ammonia absorption tower for absorption, and the formed ammonia is recycled to the power plant for denitration.
When the mother liquor density reaches 1.15g/cm during the evaporation and crystallization 3 When the sodium chloride is separated, the solid obtained by the primary centrifugal separation is collected to be the sodium chloride product, and the sodium chloride product is separated by the primary centrifugal separationThe separated liquid enters a potassium-sodium separation step, wherein the potassium-sodium separation step specifically comprises the following steps: cooling and crystallizing the liquid subjected to primary centrifugal separation, cooling and crystallizing at a cooling water temperature of 5 ℃, entering secondary centrifugal separation after cooling and crystallizing, re-entering heavy metal removal step of the liquid subjected to secondary centrifugal separation, refining the solid subjected to secondary centrifugal separation by taking saturated potassium chloride solution as refined washing liquid, carrying out tertiary centrifugal separation after refining, collecting the solid subjected to tertiary centrifugal separation to obtain a potassium chloride product, and recycling the liquid subjected to tertiary centrifugal separation as refined washing liquid; when the sodium chloride content in the liquid of the third centrifugal separation is above 20%, the liquid of the third centrifugal separation is combined with the liquid of the first centrifugal separation, and cooling crystallization is carried out again. Distilled water generated in the evaporation crystallization step is used as a water source for third-stage water washing for recycling.
Example 2:
a process for preparing high-quality industrial salt by utilizing garbage fly ash (figure 2) comprises the steps of fly ash water washing, heavy metal removal, decoloration, calcium removal, evaporative crystallization and potassium-sodium separation, and specifically comprises the following steps:
before the step of washing the fly ash, wet grinding the fly ash, and then feeding the slurry formed after the wet grinding into the step of washing the fly ash;
the fly ash washing is three-stage countercurrent washing, including first-stage washing, second-stage washing and third-stage washing;
solid-liquid separation is carried out after the first-stage water washing, the solid is crushed and then enters the second-stage water washing, the liquid enters the heavy metal removal step, and the mass ratio of the sum of the water consumption of the first-stage water washing and the water consumption of the wet grinding of the fly ash to the fly ash is=1:1, namely the mass ratio of the fly ash to the water consumption of the first-stage water washing is=1:0.6;
solid-liquid separation is carried out after the second-stage water washing, the solid is crushed and then enters the third-stage water washing, one part of liquid is used as a water source for wet grinding of the fly ash, and the rest part of liquid is used as a water source for the first-stage water washing, wherein the mass ratio of the fly ash to the water is (1) 0.4;
solid-liquid separation is carried out after the third-stage water washing, solids (the chloride ion content is about 0.8 percent and is calculated by dry weight) are sent to a cement kiln for cooperative treatment, reverse osmosis membrane desalination treatment is adopted for liquid, concentrated water generated by the reverse osmosis membrane desalination treatment is used as a water source of the second-stage water washing, clear water generated by the reverse osmosis membrane desalination treatment is used as a water source of the third-stage water washing for recycling, and the mass ratio of fly ash and water in the third-stage water washing is=1:3; and in the three-stage countercurrent washing process, aeration stirring is carried out to remove ammonia from the fly ash, and an ammonia recovery port is arranged above a washing pool of each stage of washing, so that ammonia is sent to an ammonia absorption tower for absorption, and the formed ammonia is recycled to the power plant for denitration.
When the mother liquor density reaches 1.25g/cm during the evaporation and crystallization 3 And then, carrying out primary centrifugal separation, and collecting the solid obtained by the primary centrifugal separation, namely a sodium chloride product, wherein the liquid obtained by the primary centrifugal separation enters a potassium-sodium separation step, and the potassium-sodium separation step specifically comprises the following steps: cooling and crystallizing the liquid subjected to primary centrifugal separation, cooling and crystallizing at the temperature of 30 ℃, then entering secondary centrifugal separation, re-entering heavy metal removal step of the liquid subjected to secondary centrifugal separation, refining the solid subjected to secondary centrifugal separation by taking saturated potassium chloride solution as refined washing liquid, carrying out tertiary centrifugal separation after refining, collecting the solid subjected to tertiary centrifugal separation to obtain a potassium chloride product, and recycling the liquid subjected to tertiary centrifugal separation as refined washing liquid; when the sodium chloride content in the liquid of the third centrifugal separation is above 20%, the liquid of the third centrifugal separation is combined with the liquid of the first centrifugal separation, and cooling crystallization is carried out again. Distilled water generated in the evaporation crystallization step is used as a water source for third-stage water washing for recycling.
Example 3:
a process for preparing high-quality industrial salt by utilizing garbage fly ash (figure 3) comprises the steps of fly ash water washing, heavy metal removal, decoloration, calcium removal, evaporative crystallization and potassium-sodium separation, and specifically comprises the following steps:
the fly ash washing is three-stage countercurrent washing, including first-stage washing, second-stage washing and third-stage washing;
solid-liquid separation is carried out after the first-stage water washing, the solid is crushed and then enters the second-stage water washing, the liquid enters the heavy metal removal step, and the mass ratio of the water consumption of the first-stage water washing to the fly ash is 1:1;
carrying out solid-liquid separation after the second-stage water washing, wherein the mass ratio of the fly ash of the second-stage water washing to water is 1:1, crushing the solid, then entering the third-stage water washing, and taking the liquid as a water source of the first-stage water washing;
after the third-stage water washing, solid-liquid separation is carried out, the solid (the chloride ion content is about 1.2 percent and is calculated by dry weight) is sent to a cement kiln for cooperative treatment, the liquid is used as a water source for the second-stage water washing, and the mass ratio of the fly ash and the water in the third-stage water washing is 1:1.
And in the three-stage countercurrent washing process, aeration stirring is carried out to remove ammonia from the fly ash, and an ammonia recovery port is arranged above a washing pool of each stage of washing, so that ammonia is sent to an ammonia absorption tower for absorption, and the formed ammonia is recycled to the power plant for denitration.
When the mother liquor density reaches 1.2g/cm during the evaporation and crystallization 3 And then, carrying out primary centrifugal separation, and collecting the solid obtained by the primary centrifugal separation, namely a sodium chloride product, wherein the liquid obtained by the primary centrifugal separation enters a potassium-sodium separation step, and the potassium-sodium separation step specifically comprises the following steps: cooling and crystallizing the liquid subjected to primary centrifugal separation, cooling and crystallizing the cooled and crystallized cooling water at 15 ℃, then entering secondary centrifugal separation, re-entering heavy metal removal step of the liquid subjected to secondary centrifugal separation, refining the solid subjected to secondary centrifugal separation by taking saturated potassium chloride solution as refined washing liquid, carrying out tertiary centrifugal separation after refining, collecting the solid subjected to tertiary centrifugal separation to obtain a potassium chloride product, and recycling the liquid subjected to tertiary centrifugal separation as refined washing liquid; when the sodium chloride content in the liquid of the third centrifugal separation is above 20%, the liquid of the third centrifugal separation is combined with the liquid of the first centrifugal separation, and cooling crystallization is carried out again. Distilled water generated in the evaporation crystallization step is used as a water source for third-stage water washing for recycling.
The heavy metal removal step of the invention is as follows: under the stirring condition, slowly adding sodium sulfide solution into the filtrate obtained by washing fly ash until the oxidation-reduction potential of the system reaches 0 to 50mV, and then adding ferrous chloride solution until the oxidation-reduction potential of the system reaches 100 to 150 mV. The mass concentration of the sodium sulfide solution is 2-5%. The mass concentration of the ferrous chloride solution is 3-10%.
The decoloring is to add active carbon into filtrate after heavy metal removal, the dosage of the active carbon is one to five thousandths of the weight of the filtrate, the filtrate is stirred for 3 to 10 minutes, the filtrate is filtered and collected and stored as dangerous waste, and the filtrate enters the next step of treatment.
The method comprises the steps of adding sodium carbonate into filtrate obtained after decolorization, stirring for 10-20min, filtering, collecting solid calcium carbonate, and processing the filtrate in the next step.
The steps of heavy metal removal, decolorization, calcium removal and evaporative crystallization are not the core creation points of the invention, and the specific contents of the steps of heavy metal removal, decolorization, calcium removal and evaporative crystallization can be referred to the detailed description of the prior application of the inventor, and are not repeated here.
Taking three-stage countercurrent water washing as an example, the same dechlorination effect is achieved, the third-stage countercurrent water washing adopts the mass ratio of fly ash to water=1:3, the existing three-stage countercurrent water process (the third-stage countercurrent water washing does not adopt reverse osmosis desalination, and therefore, the mass ratio of the first-stage countercurrent water washing fly ash to water is also 1:3), compared with the process of the invention (the third-stage countercurrent water washing adopts reverse osmosis desalination, and the mass ratio of the first-stage countercurrent water washing fly ash to water is 1:1), the water quantity entering the evaporative crystallization is about one third of the existing three-stage countercurrent water process, and therefore, in order to achieve the purpose of reclaimed water recycling, the evaporation quantity of the existing three-stage countercurrent water process in the evaporative crystallization step is about three times that of the invention, and therefore, the energy consumption of the invention is about one third of the prior art.
Compared with the process without wet grinding, the process of adding wet grinding to different fly ash raw materials can obviously improve the dissolution rate of chloride ions in the fly ash, the lower limit of the content of chloride ions in the fly ash can not be reduced by multi-stage water washing, and the content of chloride ions in the fly ash after water washing can be reduced by 0.2-0.5 percent.
The detection of 30 batches of salt products of the technology before improvement shows that the quality is unstable when cadmium and lead in 3 batches of products exceed the detection limit of GB 5085.3-2007 standard. The sodium chloride and the potassium chloride obtained by adopting the improved process of the invention are detected, the heavy metal indexes of 50 batches of products meet the standard of GB 5085.3-2007, the standard is not exceeded, meanwhile, the sodium chloride meets the requirements of GBT5462-2016 delicate secondary industrial salt, the potassium chloride meets the requirements of GB6549-2011, the quality is stable, and no potential safety hazard exists.
The above-described embodiment is only a preferred embodiment of the present invention, and is not limited in any way, and other variations and modifications may be made without departing from the technical aspects set forth in the claims.
Claims (6)
1. A process for preparing high-quality industrial salt by utilizing garbage fly ash is characterized by comprising the steps of fly ash water washing, heavy metal removal, decoloration, calcium removal, evaporative crystallization and potassium-sodium separation, wherein when the density of mother liquor reaches 1.15-1.25 g/cm during the evaporative crystallization 3 And then, carrying out primary centrifugal separation, and collecting the solid obtained by the primary centrifugal separation, namely a sodium chloride product, wherein the liquid obtained by the primary centrifugal separation enters a potassium-sodium separation step, and the potassium-sodium separation step specifically comprises the following steps: cooling and crystallizing the liquid subjected to primary centrifugal separation, performing secondary centrifugal separation after cooling and crystallizing, re-entering the heavy metal removal step by the liquid subjected to secondary centrifugal separation, refining the solid subjected to secondary centrifugal separation by taking saturated potassium chloride solution as refined washing liquid, performing tertiary centrifugal separation after refining, collecting the solid subjected to tertiary centrifugal separation, namely a potassium chloride product, and recycling the liquid subjected to tertiary centrifugal separation as refined washing liquid;
the temperature of cooling water for cooling and crystallizing is 5-30 ℃; when the sodium chloride content in the liquid subjected to the third centrifugal separation is more than 20%, merging the liquid subjected to the third centrifugal separation with the liquid subjected to the first centrifugal separation, and carrying out cooling crystallization again;
the fly ash washing is three-stage countercurrent washing, including first-stage washing, second-stage washing and third-stage washing;
solid-liquid separation is carried out after the first-stage water washing, the solid is crushed and then enters the second-stage water washing, the liquid enters the heavy metal removal step, and the mass ratio of the fly ash of the first-stage water washing to the water is 1:1;
solid-liquid separation is carried out after the second-stage water washing, the solid is crushed and then enters the third-stage water washing, and the liquid is used as a water source for the first-stage water washing;
solid-liquid separation is carried out after the third-stage water washing, the solid is sent to a cement kiln for cooperative treatment, the liquid adopts reverse osmosis membrane desalination treatment, concentrated water generated by the reverse osmosis membrane desalination treatment is used as a water source of the second-stage water washing, clear water generated by the reverse osmosis membrane desalination treatment is used as the water source of the third-stage water washing for recycling, and the mass ratio of fly ash and water in the third-stage water washing is=1:3;
or before the step of washing the fly ash, carrying out wet grinding on the fly ash, and enabling slurry formed after the wet grinding to enter the step of washing the fly ash; the fly ash washing is three-stage countercurrent washing, including first-stage washing, second-stage washing and third-stage washing;
solid-liquid separation is carried out after the first-stage water washing, the solid is crushed and then enters the second-stage water washing, the liquid enters the heavy metal removal step, and the mass ratio of the sum of the water consumption of the first-stage water washing and the water consumption of the wet grinding of the fly ash to the fly ash is=1:1;
solid-liquid separation is carried out after the second-stage water washing, the solid is crushed and then enters the third-stage water washing, one part of liquid is used as a water source for wet grinding of the fly ash, and the rest part of liquid is used as a water source for the first-stage water washing, wherein the mass ratio of the fly ash to the water is (1:0.3-0.5) when the fly ash is subjected to wet grinding;
and after the third-stage water washing, solid-liquid separation is carried out, the solid is sent to a cement kiln for cooperative treatment, the liquid adopts reverse osmosis membrane desalination treatment, concentrated water generated by the reverse osmosis membrane desalination treatment is used as a water source of the second-stage water washing, clear water generated by the reverse osmosis membrane desalination treatment is used as a water source of the third-stage water washing for recycling, and the mass ratio of fly ash and water in the third-stage water washing is=1:3.
2. A process for preparing high quality industrial salt from waste fly ash as claimed in claim 1, wherein: and in the three-stage countercurrent washing process, aeration stirring is carried out to remove ammonia from the fly ash, and an ammonia recovery port is arranged above a washing pool of each stage of washing, so that ammonia is sent to an ammonia absorption tower for absorption, and the formed ammonia is recycled to the power plant for denitration.
3. A process for preparing high quality industrial salt from waste fly ash as claimed in claim 1, wherein: distilled water generated in the evaporation crystallization step is used as a water source for third-stage water washing for recycling.
4. A process for preparing high quality industrial salt from waste fly ash as claimed in claim 1, wherein: the heavy metal removal step comprises the following steps: slowly adding sodium sulfide solution into the filtrate obtained by washing fly ash under the stirring condition until the oxidation-reduction potential of the system reaches 0 to 50mV below zero, and then adding ferrous chloride solution until the oxidation-reduction potential of the system reaches 100 to 150mV below zero; the mass concentration of the sodium sulfide solution is 2-5%; the mass concentration of the ferrous chloride solution is 3-10%.
5. A process for preparing high quality industrial salt from waste fly ash as claimed in claim 1, wherein: the decolorization is to add active carbon into filtrate after heavy metal removal, the dosage of the active carbon is one to five thousandths of the weight of the filtrate, the filtrate is stirred for 3 to 10 minutes, the filtrate is filtered, and the filter residue is collected and stored as dangerous waste, and the filtrate enters the next step of treatment.
6. A process for preparing high quality industrial salt from waste fly ash as claimed in claim 1, wherein: and the calcium removal is to add sodium carbonate into the filtrate obtained after decolorization, stir for 10-20min, filter, collect calcium carbonate of solid part, and the filtrate enters the next treatment.
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| CN110040748B (en) * | 2019-04-11 | 2021-06-29 | 中国中材国际工程股份有限公司 | Method for producing potassium salt and sodium salt by utilizing waste incineration fly ash |
| CN111530901A (en) * | 2020-06-12 | 2020-08-14 | 重庆赛迪热工环保工程技术有限公司 | Washing process of dust removing ash containing salt |
| CN112275764B (en) * | 2020-08-31 | 2022-04-08 | 光大绿色环保管理（深圳）有限公司 | Hazardous waste incineration fly ash water washing utilization method and device |
| CN112588771B (en) * | 2020-10-30 | 2022-09-13 | 芜湖海创环保科技有限责任公司 | Water washing method for fly ash |
| CN113955889A (en) * | 2021-08-31 | 2022-01-21 | 江西盖亚环保科技有限公司 | Resource recovery process of fly ash washing liquid |
| CN113943011A (en) * | 2021-09-17 | 2022-01-18 | 光大环保技术研究院（深圳）有限公司 | Method for resource utilization of secondary fly ash after melting of hazardous waste plasma |
| CN114573005A (en) * | 2022-03-11 | 2022-06-03 | 苏州乔发环保科技股份有限公司 | Potassium-sodium salt recycling process for sintering machine head ash and garbage fly ash |
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| CN101234766A (en) * | 2008-03-03 | 2008-08-06 | 北京科技大学 | Method for producing potassium chloride by steel enterprise sintering electro-precipitating dust |
| JP2015072199A (en) * | 2013-10-03 | 2015-04-16 | Ｊｆｅエンジニアリング株式会社 | Fly ash cleaning apparatus and fly ash cleaning method |
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| CN101234766A (en) * | 2008-03-03 | 2008-08-06 | 北京科技大学 | Method for producing potassium chloride by steel enterprise sintering electro-precipitating dust |
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