CN113772708A - Comprehensive recycling treatment process for complex waste salt system - Google Patents
Comprehensive recycling treatment process for complex waste salt system Download PDFInfo
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- CN113772708A CN113772708A CN202111117102.8A CN202111117102A CN113772708A CN 113772708 A CN113772708 A CN 113772708A CN 202111117102 A CN202111117102 A CN 202111117102A CN 113772708 A CN113772708 A CN 113772708A
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- 239000002699 waste material Substances 0.000 title claims abstract description 170
- 150000003839 salts Chemical class 0.000 title claims abstract description 157
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000004064 recycling Methods 0.000 title claims abstract description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 76
- 239000012452 mother liquor Substances 0.000 claims abstract description 62
- 238000002360 preparation method Methods 0.000 claims abstract description 55
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 52
- 238000001704 evaporation Methods 0.000 claims abstract description 46
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 39
- 239000011780 sodium chloride Substances 0.000 claims abstract description 38
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 36
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 36
- 239000011591 potassium Substances 0.000 claims abstract description 36
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 36
- 239000000126 substance Substances 0.000 claims abstract description 36
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 29
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 29
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 28
- 230000008020 evaporation Effects 0.000 claims abstract description 27
- 239000001103 potassium chloride Substances 0.000 claims abstract description 26
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 26
- 239000010440 gypsum Substances 0.000 claims abstract description 19
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 19
- 239000012267 brine Substances 0.000 claims abstract description 14
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 230000001502 supplementing effect Effects 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 66
- 239000010881 fly ash Substances 0.000 claims description 46
- 239000002956 ash Substances 0.000 claims description 42
- 239000002920 hazardous waste Substances 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 150000002500 ions Chemical class 0.000 claims description 21
- 239000010813 municipal solid waste Substances 0.000 claims description 20
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 239000001110 calcium chloride Substances 0.000 claims description 10
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 10
- 235000011056 potassium acetate Nutrition 0.000 claims description 10
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 239000003610 charcoal Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000010808 liquid waste Substances 0.000 claims description 6
- 239000010887 waste solvent Substances 0.000 claims description 6
- 159000000003 magnesium salts Chemical class 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 description 43
- 230000000052 comparative effect Effects 0.000 description 12
- 241000196324 Embryophyta Species 0.000 description 8
- 239000004568 cement Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000010791 domestic waste Substances 0.000 description 5
- 239000002910 solid waste Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 3
- 235000011613 Pinus brutia Nutrition 0.000 description 3
- 241000018646 Pinus brutia Species 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000010413 mother solution Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000032696 parturition Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002904 solvent 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 239000006227 byproduct Substances 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
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The application relates to the technical field of inorganic chemical industry, and particularly discloses a comprehensive recycling treatment process for a complex waste salt system. The treatment process comprises the following steps: s1, dissolving waste salt; s2, removing heavy metals; s3, supplementing sodium sulfate to obtain calcium sulfate and refined brine; s4, performing anti-scaling multi-effect evaporation on the refined brine by adopting a gypsum crystal seed method to obtain industrial salt, calcium sulfate and salt preparation mother liquor; s5, evaporating the salt-making mother liquor at the temperature of 90-130 ℃ to obtain industrial salt and potassium-rich mother liquor; s6, evaporating the salt-rich mother liquor at the temperature of 40-80 ℃ to obtain potassium chloride and a potassium preparation mother liquor; s7, burning part of the potassium preparation mother liquor, and returning part of the potassium preparation mother liquor to the salt preparation mother liquor for evaporation. The process for treating the waste salt improves the recovery rate of the sodium chloride and the potassium chloride, and has the characteristics of strong raw material adaptability, reasonable production process, low cost, reduction, harmlessness and reclamation of the waste salt.
Description
Technical Field
The application relates to the technical field of inorganic chemical industry, in particular to a comprehensive recycling treatment process for a complex waste salt system.
Background
The complex waste salt system refers to a high-salinity wastewater crystallization product or an intermediate byproduct of chemical synthesis in the production process of the industries such as chemical industry, petroleum industry, textile industry, printing and dyeing industry, medicine industry, pesticide industry and the like.
The treatment method of the complex waste salt system comprises landfill treatment, incineration and high-temperature treatment. Landfill disposal may result in greater secondary pollution due to leachate leakage. And a large amount of chlorine in the waste salt can generate dioxin in the high-temperature incineration process, so that more serious harm is caused.
In view of the above-mentioned related technologies, the applicant considers that the search for a reasonable resource process of a complex waste salt system is a major issue that needs to be solved urgently in the environmental protection industry.
Disclosure of Invention
In order to improve the resource utilization of the complex waste salt system, the application provides a complex waste salt system resource comprehensive treatment process.
The application provides a comprehensive resource treatment process for a complex waste salt system, which adopts the following technical scheme:
a comprehensive resource treatment process for a complex waste salt system comprises the following steps:
s1, dissolving a waste salt system to obtain a dissolving solution and waste residues:
s2, removing heavy metals in the dissolving solution;
s3, supplementing sodium sulfate into the dissolved solution obtained after the heavy metals are removed in the step S2, and carrying out equilibrium reaction at the temperature of 25-70 ℃ for 0.1-8h to obtain calcium sulfate and refined brine;
s4, performing anti-scale multi-effect evaporation on the refined brine obtained in the step S3 by adopting a gypsum seed crystal method, wherein the evaporation temperature is 40-130 ℃, and obtaining industrial salt, calcium sulfate and salt preparation mother liquor;
s5, evaporating the salt preparation mother liquor obtained in the step S4 at the temperature of 90-130 ℃ to obtain industrial salt and potassium-rich mother liquor;
s6, evaporating the potassium-rich mother liquor obtained in the step S5 at the temperature of 40-80 ℃ to obtain potassium chloride and a potassium preparation mother liquor;
s7. the potassium preparation mother liquor with the weight percentage of 1.5 to 4.0 percent in the potassium preparation mother liquor obtained in S6 is incinerated to recover industrial salt, and the rest part of the potassium preparation mother liquor is evaporated together with the salt preparation mother liquor in S5.
By adopting the technical scheme, after a complex waste salt system is dissolved and heavy metals are removed, the complex waste salt system and sodium sulfate are subjected to equilibrium reaction, and calcium chloride in a dissolving solution is removed to obtain calcium sulfate; then, the Ca in the solution is prevented from multi-effect evaporation by a paste crystal seed method2+、SO4 2-Condensing on the gypsum crystal nucleus, and removing calcium sulfate in the solution; and then carrying out fractional evaporation on the solution, evaporating at the temperature of 90-130 ℃ to separate out sodium chloride, then reducing the evaporation temperature to 40-80 ℃ to continue evaporation, supersaturating potassium chloride in the solution to separate out in the cooling process to obtain a potassium preparation mother solution, returning part of the potassium preparation mother solution to the temperature of 90-130 ℃ to evaporate, and burning part of the potassium preparation mother solution to obtain sodium chloride and potassium chloride.
Preferably, the waste salt system comprises waste salt, hazardous waste fly ash and household garbage fly ash;
the waste salt comprises the following components in percentage by weight: 30-60% of sodium chloride, 20-50% of sodium sulfate, 0-15% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 1-10% of water;
the hazardous waste fly ash comprises the following components in percentage by weight: 40-60% of sodium chloride, 15-20% of sodium sulfate, 10-40% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and the like, and 1-2% of water;
the household garbage fly ash comprises the following components in percentage by weight: 10-15% of sodium chloride, 15-20% of calcium chloride, 1.5-4% of potassium chloride, 60-65% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and the like, and 1-2% of water.
By adopting the technical scheme, the concentration range of the components in the complex system which can be treated is wide, the waste salt containing different contents of sodium chloride, sodium sulfate, calcium chloride and other components can be recycled by using the process, and the applicability is wide.
Preferably, the specific steps of dissolving the complex waste salt system in the S1 are as follows:
the waste salt is dissolved by adopting the condensate water in a countercurrent way, the dissolving time is 1-2 hours, and the dissolving temperature is 25-70 ℃, so that waste salt dissolving liquid and waste salt dissolving ash are obtained;
the hazardous waste fly ash is dissolved in a counter-current manner by using condensed water, the dissolving time is 1-2 hours, and the dissolving temperature is 25-70 ℃, so that a hazardous waste dissolving liquid and hazardous waste dissolving ash are obtained;
the fly ash of the household garbage is dissolved by adopting the counter flow of condensed water, the dissolving time is 1 to 2 hours, and the dissolving temperature is 25 to 70 ℃, so as to obtain raw waste dissolving liquid and raw waste dissolving ash;
the dissolving solution comprises a waste salt dissolving solution, a dangerous waste dissolving solution and a raw waste dissolving solution;
the waste residue comprises waste salt dissolving waste residue, hazardous waste dissolving ash residue and raw waste solvent waste residue.
Through adopting above-mentioned technical scheme, because the waste salt, the useless flying ash of danger, the composition content is different in the domestic waste flying ash, so dissolve waste salt, the useless flying ash of danger, the domestic waste flying ash of life respectively, can improve the dissolution effect of complicated waste salt system on the one hand, the waste salt that on the other hand produced dissolves the waste residue, the useless lime-ash that dissolves of danger, the content and the kind of harmful component in the useless solvent waste residue of giving birth are also not completely the same, can dissolve waste residue with waste salt, the useless lime-ash that dissolves of danger, useless solvent waste residue of giving birth to carries out subsequent processing respectively, further reduce the pollution to the environment, be favorable to environmental protection.
Preferably, in the step S4, the mass concentration of the gypsum in the evaporation environment is maintained at 20-35 g/L.
By adopting the technical scheme, the crystal seeds can not be obtained due to too low gypsum concentration in the evaporation system, and Ca can not be obtained2+、SO4 2-The lack of attachment sites results in incomplete removal of calcium sulfate, while too high a concentration of gypsum affects the evaporation capacity, and gypsum in this concentration range can play a better role in removing calcium sulfate from the solution.
Preferably, the sodium sulfate in step S3 includes the following components by weight percentage: na (Na)2SO4 40-98%55-1% of NaCl and the balance of inevitable impurities.
By adopting the technical scheme, the sodium sulfate is generally purchased industrial sodium sulfate, and the main component of the purchased sodium sulfate is Na2SO4With NaCl, control Na in sodium sulfate2SO4The proportion of the Na and NaCl can be regulated and controlled2SO4With CaCl2The proportion of the calcium chloride is higher, so that a better calcium chloride removing effect is achieved.
Preferably, the heavy metal ions in step S2 are removed by a modified biochar adsorption method, and the modified biochar preparation method includes:
treating the biochar with a potassium acetate solution to obtain modified biochar, wherein the dosage ratio of the biochar to the potassium acetate solution is as follows: 1g of biochar is treated with 50-60ml of potassium acetate solution.
By adopting the technical scheme, the potassium acetate is used for modifying the biochar, the specific surface area of the biochar is improved, oxygen-containing functional groups on the surface of the biochar are increased, more surface functional groups are added, and the mechanism of carbonate surface precipitation is adopted, so that the biochar can treat Pb2 +、Fe2+、Mn2+、Cu2+、Zn2+The adsorptivity of heavy metal ions is improved, and the effect of removing heavy metals is improved.
Preferably, the biochar is prepared by carbonizing pine wood.
Preferably, the particle size of the biochar is 100-150 μm.
By adopting the technical scheme, the biochar in the particle size range can play a better adsorption role.
Preferably, the waste salt, the dangerous waste fly ash and the household garbage fly ash all contain soluble water-soluble magnesium salt with the weight percentage of less than 0.2 percent.
Preferably, before the step S3, Mg in the solution is removed by a double alkali method2+。
By adopting the technical scheme, the waste salt containing the soluble magnesium salt can be recycled by using the process, and the process has a wide application range.
In summary, the present application has the following beneficial effects:
1. by adopting the process to carry out resource treatment on the complex waste salt system, the recovery rate of sodium chloride in the waste salt system reaches 94.59-97.56%, the recovery rate of potassium chloride reaches 93.74-96.68%, and the resource utilization effect is better.
2. In the application, the modified biochar is preferably adopted for removing heavy metals, and Pb in solution after the heavy metals are removed2+Is 0.71-0.81mg/L, and reduces the pollution of heavy metal to the environment.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example of intermediate
Preparation example 1
The preparation method of the modified biochar comprises the following steps:
cleaning pine, drying at 80 ℃ to constant weight, carbonizing the dried pine at 450 ℃ under an anoxic condition for 2h, cooling to room temperature, and grinding into particles with the particle size of 100 microns to obtain charcoal;
mixing 1kg of biochar with 50L of potassium acetate solution with the substance amount concentration of 2mol/L, oscillating for 2h at 25 ℃ to obtain a crude product, then putting the crude product into 100L of water, stirring for 30min at the speed of 100, and finally washing for 4 times by using clear water to obtain the modified biochar.
Preparation example 2
In contrast to preparation example 1, the amount of potassium acetate solution used was 55L.
Preparation example 3
In contrast to preparation example 1, the amount of potassium acetate solution used was 60L.
Preparation example 4
Unlike preparation example 2, the biochar had a particle size of 120 μm.
Preparation example 5
Unlike preparation example 2, the biochar had a particle size of 30 μm.
Preparation example 6
Unlike preparation example 2, the biochar had a particle size of 450 μm.
Preparation example 7
Unlike preparation example 2, the biochar had a particle size of 150 μm.
Examples
Example 1
A comprehensive resource treatment process for a complex waste salt system comprises the following steps:
s1, dissolving a waste salt system to obtain a dissolving solution and waste residues:
the waste salt system comprises 1 ton of waste salt, 1 ton of hazardous waste fly ash and 6 ton of domestic waste fly ash;
the waste salt comprises 60% of sodium chloride, 20% of sodium sulfate, 10% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 10% of water;
the hazardous waste fly ash comprises 60% of sodium chloride, 15% of sodium sulfate, 24% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 1% of water;
the household garbage fly ash comprises 15% of sodium chloride, 20% of calcium chloride, 4% of potassium chloride, 60% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 1% of water;
uniformly mixing waste salt, hazardous waste fly ash and household garbage fly ash, and then carrying out countercurrent dissolution by using 22 tons of condensed water, wherein the dissolution time is 1h, and the dissolution temperature is 30 ℃;
s2, removing heavy metals in the dissolving solution by using charcoal;
s3, supplementing 1.42 tons of sodium sulfate into the dissolved solution obtained after the heavy metals are removed in the step S2, and carrying out equilibrium reaction at the temperature of 25 ℃ for 8 hours to obtain calcium sulfate and refined brine; the purchased sodium sulfate comprises the following components: na (Na)2SO440 percent of NaCl, 55 percent of NaCl and the balance of inevitable impurities.
S4, performing anti-scale four-effect evaporation on the refined brine obtained in the step S3 by adopting a gypsum seed crystal method, wherein the evaporation temperature is 40 ℃, and the mass concentration of gypsum in an evaporation environment is kept at 20g/L, so that industrial salt, calcium sulfate and salt making mother liquor are obtained;
s5, evaporating the salt making mother liquor obtained in the step S4 at the temperature of 90 ℃ to obtain industrial salt and potassium-rich mother liquor;
s6, evaporating the salt-rich mother liquor obtained in the step S5 at the temperature of 40 ℃ to obtain potassium chloride and a potassium preparation mother liquor;
s7. burning 1.5 wt% of the mother liquor for preparing potassium obtained in S6 at 650 deg.C to recover industrial salt, and evaporating the rest of the mother liquor together with the mother liquor for preparing salt in S5.
Example 2
A comprehensive resource treatment process for a complex waste salt system comprises the following steps:
s1, dissolving a waste salt system to obtain a dissolving solution and waste residues:
the waste salt system comprises 1 ton of waste salt, 1 ton of hazardous waste fly ash and 6 ton of domestic waste fly ash;
the waste salt comprises 50% of sodium chloride, 30% of sodium sulfate, 12% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 8% of water;
the hazardous waste fly ash comprises 50% of sodium chloride, 20% of sodium sulfate, 28% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 2% of water;
the household garbage fly ash comprises 13% of sodium chloride, 20% of calcium chloride, 2% of potassium chloride, 63% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 2% of water;
uniformly mixing waste salt, hazardous waste fly ash and household garbage fly ash, and then carrying out countercurrent dissolution by using 22 tons of condensed water, wherein the dissolution time is 1h, and the dissolution temperature is 30 ℃;
s2, removing heavy metals in the dissolving solution by using charcoal;
s3, supplementing 1.13 tons of sodium sulfate into the dissolved solution obtained after the heavy metals are removed in the step S2, and carrying out equilibrium reaction at the temperature of 50 ℃ for 5 hours to obtain calcium sulfate and refined brine;
s4, performing anti-scale four-effect evaporation on the refined brine obtained in the step S3 by adopting a gypsum seed crystal method, wherein the evaporation temperature is 90 ℃, and obtaining industrial salt, calcium sulfate and salt making mother liquor;
s5, evaporating the salt preparation mother liquor obtained in the step S4 at the temperature of 110 ℃ to obtain industrial salt and potassium-rich mother liquor;
s6, evaporating the salt-rich mother liquor obtained in the step S5 at the temperature of 60 ℃ to obtain potassium chloride and a potassium preparation mother liquor;
s7. burning 3 wt% of the mother liquor for preparing potassium obtained in S6 at 650 deg.C to recover industrial salt, and evaporating the rest of the mother liquor together with the mother liquor for preparing salt in S5.
Example 3
A comprehensive resource treatment process for a complex waste salt system comprises the following steps:
s1, dissolving a waste salt system to obtain a dissolving solution and waste residues:
the waste salt system comprises 1 ton of waste salt, 1 ton of hazardous waste fly ash and 6 ton of domestic waste fly ash;
the waste salt comprises 30 percent of sodium chloride, 50 percent of sodium sulfate, 15 percent of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 5 percent of water;
the hazardous waste fly ash comprises 40% of sodium chloride, 20% of sodium sulfate, 38% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 2% of water;
the household garbage fly ash comprises 10% of sodium chloride, 20% of calcium chloride, 4% of potassium chloride, 65% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 1% of water;
uniformly mixing waste salt, hazardous waste fly ash and household garbage fly ash, and then carrying out countercurrent dissolution by adopting 23 tons of condensed water, wherein the dissolution time is 1h, and the dissolution temperature is 30 ℃;
s2, removing heavy metals in the dissolving solution by using charcoal;
s3, supplementing 1 ton of sodium sulfate into the dissolved solution obtained after the heavy metals are removed in the step S2, and carrying out equilibrium reaction at the temperature of 70 ℃ for 2 hours to obtain calcium sulfate and refined brine;
s4, performing anti-scale four-effect evaporation on the refined brine obtained in the step S3 by adopting a gypsum seed crystal method, wherein the evaporation temperature is 130 ℃, and obtaining industrial salt, calcium sulfate and salt making mother liquor;
s5, evaporating the salt preparation mother liquor obtained in the step S4 at the temperature of 130 ℃ to obtain industrial salt and potassium-rich mother liquor;
s6, evaporating the salt-rich mother liquor obtained in the step S5 at the temperature of 80 ℃ to obtain potassium chloride and a potassium preparation mother liquor;
s7, burning 4 percent of the potassium preparation mother liquor in the potassium preparation mother liquor obtained in S6 at the burning temperature of 650 ℃ to recover industrial salt, and evaporating the rest part of the potassium preparation mother liquor and the salt preparation mother liquor in S5.
Example 4
Different from the example 2, the specific steps for dissolving the complex waste salt system in the S1 are as follows:
the waste salt is subjected to secondary countercurrent dissolution by using 2.06 tons of condensed water, the dissolution time is 1 hour, and the dissolution temperature is 70 ℃, so that a waste salt dissolution solution and waste salt dissolution ash are obtained; carrying out common solid waste landfill treatment on the waste salt dissolved ash;
performing secondary countercurrent dissolution on the hazardous waste fly ash by using 1.875 tons of condensed water, wherein the dissolution time is 2 hours, and the dissolution temperature is 25 ℃, so as to obtain a hazardous waste dissolution liquid and hazardous waste dissolution ash; the hazardous waste dissolved ash is treated in a cement plant or a flexible landfill;
secondary countercurrent dissolving of the household garbage fly ash by adopting 18 tons of condensed water, wherein the dissolving time is 1 hour, and the dissolving temperature is 25 ℃, so that raw waste dissolving liquid and raw waste dissolving ash are obtained; the raw waste dissolved ash is sent to a cement plant or a flexible landfill;
the dissolving solution comprises a waste salt dissolving solution, a dangerous waste dissolving solution and a raw waste dissolving solution;
the waste residue comprises waste salt dissolving waste residue, hazardous waste dissolving ash residue and raw waste solvent waste residue.
Example 5
Different from the example 2, the specific steps for dissolving the complex waste salt system in the S1 are as follows:
the waste salt is subjected to secondary countercurrent dissolution by using 2.06 tons of condensed water, the dissolution time is 1.5 hours, and the dissolution temperature is 50 ℃, so that a waste salt dissolution solution and waste salt dissolution ash are obtained; carrying out common solid waste landfill treatment on the waste salt dissolved ash;
performing secondary countercurrent dissolution on the hazardous waste fly ash by using 1.875 tons of condensed water, wherein the dissolution time is 1.5 hours, and the dissolution temperature is 50 ℃, so as to obtain a hazardous waste dissolution liquid and hazardous waste dissolution ash; the hazardous waste dissolved ash is treated in a cement plant or a flexible landfill;
secondary countercurrent dissolving of the household garbage fly ash by adopting 18 tons of condensed water, wherein the dissolving time is 1.5 hours, and the dissolving temperature is 50 ℃, so that raw waste dissolving liquid and raw waste dissolving ash are obtained; the raw waste dissolved ash is sent to a cement plant or a flexible landfill;
the dissolving solution comprises a waste salt dissolving solution, a dangerous waste dissolving solution and a raw waste dissolving solution;
the waste residue comprises waste salt dissolving waste residue, hazardous waste dissolving ash residue and raw waste solvent waste residue.
Example 6
Different from the example 2, the specific steps for dissolving the complex waste salt system in the S1 are as follows:
the waste salt is subjected to secondary countercurrent dissolution by using 2.06 tons of condensed water, the dissolution time is 1 hour, and the dissolution temperature is 70 ℃, so that a waste salt dissolution solution and waste salt dissolution ash are obtained; carrying out common solid waste landfill treatment on the waste salt dissolved ash;
performing secondary countercurrent dissolution on the hazardous waste fly ash by using 1.875 tons of condensed water, wherein the dissolution time is 2 hours, and the dissolution temperature is 25 ℃, so as to obtain a hazardous waste dissolution liquid and hazardous waste dissolution ash; the hazardous waste dissolved ash is treated in a cement plant or a flexible landfill;
secondary countercurrent dissolving of the household garbage fly ash by adopting 18 tons of condensed water, wherein the dissolving time is 1 hour, and the dissolving temperature is 70 ℃, so that raw waste dissolving liquid and raw waste dissolving ash are obtained; the raw waste dissolved ash is sent to a cement plant or a flexible landfill;
the dissolving solution comprises a waste salt dissolving solution, a dangerous waste dissolving solution and a raw waste dissolving solution;
the waste residue comprises waste salt dissolving waste residue, hazardous waste dissolving ash residue and raw waste solvent waste residue.
Example 7
Different from the example 2, the specific steps for dissolving the complex waste salt system in the S1 are as follows:
the waste salt is dissolved by adopting the condensate water in a countercurrent way, the dissolving time is 3 hours, and the dissolving temperature is 10 ℃, so that a waste salt dissolving solution and waste salt dissolving ash are obtained; carrying out common solid waste landfill treatment on the waste salt dissolved ash;
the hazardous waste fly ash is dissolved in a counter-current manner by using condensed water, the dissolving time is 3 hours, and the dissolving temperature is 10 ℃, so that a hazardous waste dissolving liquid and hazardous waste dissolving ash are obtained; the hazardous waste dissolved ash is treated in a cement plant or a flexible landfill;
the household garbage fly ash is dissolved by adopting the counter flow of condensed water, the dissolving time is 3 hours, and the dissolving temperature is 10 ℃, so that raw waste dissolving liquid and raw waste dissolving ash are obtained; the raw waste dissolved ash is sent to a cement plant or a flexible landfill;
the dissolving solution comprises a waste salt dissolving solution, a dangerous waste dissolving solution and a raw waste dissolving solution;
the waste residue comprises waste salt dissolving waste residue, hazardous waste dissolving ash residue and raw waste solvent waste residue.
Example 8
Unlike example 5, the mass concentration of gypsum in the evaporation atmosphere in step S4 was maintained at 35 g/L.
Example 9
Unlike example 5, the mass concentration of gypsum in the evaporation atmosphere in step S4 was maintained at 5 g/L.
Example 10
Unlike example 5, the mass concentration of gypsum in the evaporation atmosphere in step S4 was maintained at 60 g/L.
Example 11
In contrast to example 8, the biochar was replaced by the same amount of modified biochar from preparation 1.
Examples 12 to 17
In contrast to example 11, modified biochar was obtained from preparation examples 2 to 7, respectively.
Example 18
Unlike example 14, the sodium sulfate in step S3 included the following ingredients: na (Na)2SO498%, NaCl1%, and the balance unavoidable impurities.
Example 19
Unlike example 14, the sodium sulfate in step S3 included the following ingredients: na (Na)2SO435 percent of NaC60 percent and the balance of inevitable impurities.
Example 20
A comprehensive resource treatment process for a complex waste salt system comprises the following steps:
s1 and S2 are the same as in example 3;
s3, supplementing 85kg of sodium hydroxide into the dissolved solution obtained after the heavy metals are removed in the step S2, and reacting to obtain magnesium hydroxide and a reaction solution;
s4, supplementing 1.42 tons of sodium sulfate into the reaction liquid in the step S3, and carrying out equilibrium reaction at the temperature of 25 ℃ for 8 hours to obtain calcium sulfate and refined brine; the purchased sodium sulfate comprises the following components: na (Na)2SO440 percent of NaCl, 55 percent of NaCl and the balance of inevitable impurities.
S5, performing anti-scale four-effect evaporation on the refined brine obtained in the step S4 by adopting a gypsum seed crystal method, wherein the evaporation temperature is 40 ℃, and the mass concentration of gypsum in an evaporation environment is kept at 20g/L, so that industrial salt, calcium sulfate and salt making mother liquor are obtained;
s6, evaporating the salt making mother liquor obtained in the step S5 at the temperature of 90 ℃ to obtain industrial salt and potassium-rich mother liquor;
s7, evaporating the salt-rich mother liquor obtained in the step S6 at the temperature of 40 ℃ to obtain potassium chloride and a potassium preparation mother liquor;
s8, burning 1.5 percent of the potassium preparation mother liquor in the weight percentage in the potassium preparation mother liquor obtained in S7 at the burning temperature of 650 ℃ to recover industrial salt, and evaporating the rest part of the potassium preparation mother liquor and the salt preparation mother liquor in S6.
Comparative example
Comparative example 1
In contrast to example 1, the solution from which the heavy metals were removed was incinerated at 700 ℃.
Comparative example 2
Unlike example 1, all of the potassium production mother liquor obtained in step S7 was evaporated together with the salt production mother liquor in S5.
Performance test
Detection method/test method
And (3) detection of recovery rate: the recovery rates of sodium chloride and potassium chloride in examples 1 to 20 and comparative examples 1 to 2 were measured:
recovery = (actual production/theoretical production 100%)
The actual yield is the amount of sodium chloride or potassium chloride actually obtained; the theoretical yield is the amount of sodium chloride or potassium chloride theoretically contained in the waste salt system.
Determination of heavy metal ions: the contents of heavy metals in the solutions obtained in examples 1 to 20 and comparative examples 1 to 2 were measured. And (3) determining the content of lead ions by referring to HJ787-2016 (determination of lead and cadmium in solid wastes) graphite furnace atomic absorption spectrophotometry.
Determination of COD: the COD content of the waste streams generated in examples 1-20 and comparative examples 1-2 was determined according to GB 1994-1989.
The results of the performance measurements are shown in Table 1.
TABLE 1 Performance test results
| Examples | Recovery rate of sodium chloride (100%) | Recovery ratio of potassium chloride (%) | Pb2+Concentration (mg/L) | COD concentration (mg/L) |
| Example 1 | 94.68 | 93.83 | 0.89 | 15.68 |
| Example 2 | 95.15 | 94.30 | 0.92 | 15.91 |
| Example 3 | 94.89 | 94.04 | 0.88 | 15.78 |
| Example 4 | 96.65 | 95.78 | 0.87 | 15.86 |
| Example 5 | 96.86 | 95.99 | 0.85 | 15.84 |
| Example 6 | 96.72 | 95.85 | 0.88 | 15.83 |
| Example 7 | 95.69 | 94.83 | 0.91 | 15.86 |
| Example 8 | 97.14 | 96.27 | 0.84 | 15.82 |
| Example 9 | 94.59 | 93.74 | 0.86 | 15.85 |
| Example 10 | 95.95 | 95.09 | 0.85 | 15.81 |
| Example 11 | 97.20 | 96.33 | 0.75 | 15.83 |
| Example 12 | 97.18 | 96.31 | 0.71 | 15.82 |
| Example 13 | 97.16 | 96.29 | 0.73 | 15.84 |
| Example 14 | 97.15 | 96.28 | 0.72 | 15.85 |
| Example 15 | 97.19 | 96.32 | 0.74 | 15.83 |
| Example 16 | 96.16 | 95.30 | 0.79 | 15.81 |
| Example 17 | 97.18 | 96.31 | 0.81 | 15.84 |
| Example 18 | 97.56 | 96.68 | 0.73 | 15.86 |
| Example 19 | 96.86 | 95.99 | 0.78 | 15.85 |
| Example 20 | 94.86 | 94.01 | 0.89 | 15.83 |
| Comparative example 1 | 86.54 | 85.77 | 0.90 | 18.89 |
| Comparative example 2 | 92.56 | 91.73 | 0.89 | 17.95 |
By combining the examples 1 to 20 and the comparative example 1 and combining the table 1, it can be seen that the recovery rates of sodium chloride and potassium chloride in the examples 1 to 20 are obviously higher than that in the comparative example 1, which shows that the waste salt recycling treatment process of the application can improve the recovery rate of salts in the waste salt, so that the waste salt can be better recycled; by combining examples 1-20 with comparative examples 1-2 and table 1, it can be seen that the COD concentration in examples 1-20 is lower, which indicates that the resource treatment process of the present application can reduce the COD content in the waste liquid and is beneficial to environmental protection.
It can be seen from the combination of examples 1-7 and Table 1 that the recovery rates of NaCl and KCl in examples 4-7 are higher than those in comparative examples 1-3, which shows that the respective dissolution of waste salt, hazardous waste fly ash and household garbage fly ash can increase the recovery rates of NaCl and KCl, probably because the respective countercurrent dissolution can increase the dissolution effect of soluble substances in the waste salt, hazardous waste fly ash and household garbage fly ash, so that NaCl and KCl can be more completely dissolved and then recovered.
As can be seen by combining examples 5 with examples 8 to 10 and Table 1, the recovery rates of sodium chloride and potassium chloride were reduced in examples 9 to 10, probably because the concentration of gypsum affects Ca2+、SO4 2Thereby affecting the purification of other substances in the solution.
When example 8 is combined with examples 11 to 17 and Table 1 is combined, it can be seen that the recovery rates of sodium chloride and potassium chloride in examples 11 to 17 are not much different from that in example 8, but Pb in examples 11 to 17 is not much different from that in example 82+The concentration is obviously reduced, which shows that the modified biochar has better effect of removing heavy metal ions.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. A comprehensive resource treatment process for a complex waste salt system is characterized by comprising the following steps:
s1, dissolving a waste salt system to obtain a dissolving solution and waste residues;
s2, removing heavy metals in the dissolving solution;
s3, supplementing sodium sulfate into the dissolved solution obtained after the heavy metals are removed in the step S2, and carrying out equilibrium reaction at the temperature of 25-70 ℃ for 0.1-8h to obtain calcium sulfate and refined brine;
s4, performing anti-scale multi-effect evaporation on the refined brine obtained in the step S3 by adopting a gypsum seed crystal method, wherein the evaporation temperature is 40-130 ℃, and obtaining industrial salt, calcium sulfate and salt preparation mother liquor;
s5, evaporating the salt preparation mother liquor obtained in the step S4 at the temperature of 90-130 ℃ to obtain industrial salt and potassium-rich mother liquor;
s6, evaporating the potassium-rich mother liquor obtained in the step S5 at the temperature of 40-80 ℃ to obtain potassium chloride and a potassium preparation mother liquor;
s7. the potassium preparation mother liquor with the weight percentage of 1.5 to 4.0 percent in the potassium preparation mother liquor obtained in S6 is incinerated to recover industrial salt, and the rest part of the potassium preparation mother liquor is evaporated together with the salt preparation mother liquor in S5.
2. The comprehensive recycling treatment process for the complex waste salt system according to claim 1, which is characterized in that: the waste salt system comprises waste salt, dangerous waste fly ash and household garbage fly ash;
the waste salt comprises the following components in percentage by weight: 30-60% of sodium chloride, 20-50% of sodium sulfate, 0-15% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and 1-10% of water;
the hazardous waste fly ash comprises the following components in percentage by weight: 40-60% of sodium chloride, 15-20% of sodium sulfate, 10-40% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and the like, and 1-2% of water;
the household garbage fly ash comprises the following components in percentage by weight: 10-15% of sodium chloride, 15-20% of calcium chloride, 1.5-4% of potassium chloride, 60-65% of heavy metal ions, COD (chemical oxygen demand) and insoluble substances and the like, and 1-2% of water.
3. The comprehensive recycling treatment process for the complex waste salt system according to claim 2, which is characterized in that: the specific steps for dissolving the complex waste salt system in the S1 are as follows:
the waste salt is dissolved by adopting the condensate water in a countercurrent way, the dissolving time is 1-2 hours, and the dissolving temperature is 25-70 ℃, so that waste salt dissolving liquid and waste salt dissolving ash are obtained;
the hazardous waste fly ash is dissolved in a counter-current manner by using condensed water, the dissolving time is 1-2 hours, and the dissolving temperature is 25-70 ℃, so that a hazardous waste dissolving liquid and hazardous waste dissolving ash are obtained;
the fly ash of the household garbage is dissolved by adopting the counter flow of condensed water, the dissolving time is 1 to 2 hours, and the dissolving temperature is 25 to 70 ℃, so as to obtain raw waste dissolving liquid and raw waste dissolving ash;
the dissolving solution comprises a waste salt dissolving solution, a dangerous waste dissolving solution and a raw waste dissolving solution;
the waste residue comprises waste salt dissolving waste residue, hazardous waste dissolving ash residue and raw waste solvent waste residue.
4. The comprehensive recycling treatment process for the complex waste salt system according to claim 1, which is characterized in that: in the step S4, the mass concentration of the gypsum in the evaporation environment is kept between 20 and 35 g/L.
5. The comprehensive recycling treatment process for the complex waste salt system according to claim 1, which is characterized in that: the sodium sulfate in the step S3 comprises the following components in percentage by weight: na (Na)2SO440-98%, NaCl 1-55%, and the balance of inevitable impurities.
6. The comprehensive recycling treatment process for the complex waste salt system according to claim 1, which is characterized in that: the heavy metal ions in the step S2 are removed by a modified charcoal adsorption method, and the preparation method of the modified charcoal comprises the following steps:
treating the biochar with a potassium acetate solution to obtain modified biochar, wherein the dosage ratio of the biochar to the potassium acetate solution is as follows: 1g of biochar is treated with 50-60ml of potassium acetate solution.
7. The comprehensive recycling treatment process for the complex waste salt system according to claim 6, which is characterized in that: the particle size of the biochar is 100-150 mu m.
8. The comprehensive recycling treatment process for the complex waste salt system according to claim 2, which is characterized in that: the waste salt, the dangerous waste fly ash and the household garbage fly ash can all contain soluble water-soluble magnesium salt with the weight percentage of less than 0.2 percent.
9. The comprehensive recycling treatment process for the complex waste salt system according to claim 8, which is characterized in that: removing Mg in the solution before the step S32+。
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