CN111573883A - Method for treating chemical nickel plating waste liquid through iron-based catalyst - Google Patents
Method for treating chemical nickel plating waste liquid through iron-based catalyst Download PDFInfo
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- CN111573883A CN111573883A CN202010316769.XA CN202010316769A CN111573883A CN 111573883 A CN111573883 A CN 111573883A CN 202010316769 A CN202010316769 A CN 202010316769A CN 111573883 A CN111573883 A CN 111573883A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 106
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000002699 waste material Substances 0.000 title claims abstract description 79
- 239000007788 liquid Substances 0.000 title claims abstract description 69
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 53
- 238000007747 plating Methods 0.000 title claims abstract description 52
- 239000000126 substance Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 41
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 40
- 239000003054 catalyst Substances 0.000 title claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000004576 sand Substances 0.000 claims abstract description 41
- 239000010902 straw Substances 0.000 claims abstract description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000005507 spraying Methods 0.000 claims abstract description 17
- 239000010881 fly ash Substances 0.000 claims abstract description 14
- 239000010451 perlite Substances 0.000 claims abstract description 14
- 235000019362 perlite Nutrition 0.000 claims abstract description 14
- 150000003839 salts Chemical class 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000011068 loading method Methods 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 230000005415 magnetization Effects 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims description 41
- 239000002994 raw material Substances 0.000 claims description 28
- 238000001354 calcination Methods 0.000 claims description 25
- 230000032683 aging Effects 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 238000004062 sedimentation Methods 0.000 claims description 9
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 7
- 241000209140 Triticum Species 0.000 claims description 7
- 235000021307 Triticum Nutrition 0.000 claims description 7
- 229910001453 nickel ion Inorganic materials 0.000 claims description 7
- 240000008042 Zea mays Species 0.000 claims description 6
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 6
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 6
- 235000005822 corn Nutrition 0.000 claims description 6
- 238000005273 aeration Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 229910001385 heavy metal Inorganic materials 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000005453 pelletization Methods 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims 4
- 239000012670 alkaline solution Substances 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 230000006835 compression Effects 0.000 claims 1
- 239000010802 sludge Substances 0.000 claims 1
- 239000000047 product Substances 0.000 description 22
- 238000010438 heat treatment Methods 0.000 description 12
- 238000001816 cooling Methods 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 241001156002 Anthonomus pomorum Species 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention provides a method for treating chemical nickel plating waste liquid by using an iron catalyst, which comprises the following steps: (1) preparation of the carrier: mixing diatomite, fly ash, perlite, phyllite and biological straw to prepare ceramsite sand for later use; (2) preparation of iron-based catalyst: mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution, then carrying out magnetization treatment, loading on ceramsite sand in a spraying manner, and drying to obtain an iron-based catalyst; (3) and (3) treating the chemical nickel plating waste liquid: adding CaO, an iron catalyst, NaOH and a polymeric flocculant into the chemical nickel plating waste liquid for treatment and then discharging; the method has the advantages of simple process and low operation cost in the aspect of treating the nickel plating waste liquid.
Description
Technical Field
The invention relates to the technical field of waste liquid treatment, in particular to a method for treating chemical nickel plating waste liquid by using an iron catalyst.
Background
Chemical plating, also known as electroless plating, is a novel metal surface treatment technology, and is increasingly concerned by people with its simple and convenient process, energy conservation and environmental protection. The chemical plating has wide application range, uniform gold plating layer and good decoration. In the aspect of protection performance, the corrosion resistance and the service life of the product can be improved; in terms of functionality, the special functions of wear resistance, conductivity, lubricating property and the like of the workpiece can be improved, so that the surface treatment technology is developed all over the world. The real discovery of electroless nickel plating technology and its application to date was in 1944, the discovery of a.brenner and g.riddell by the national institute of standards, the clear catalytic properties of the formed coating, and the discovery of a method of depositing non-powdered nickel, which makes the electroless nickel plating technology industrially applicable. The industrialized production of electroless nickel plating in China starts late, but the development is very rapid in recent years, and more than 300 manufacturers exist according to the statistics of the published article in the fifth chemical plating year, but the number is extremely conservative at that time. It is presumed that the total annual market size of electroless nickel plating in China should be around 300 billion yuan and develop at a rate of 10% to 15% per year.
Because waste liquid containing nickel, phosphorus and organic matters is generated in the chemical nickel plating solution process, if the waste liquid is discharged randomly without being treated, not only can serious damage be caused to the environmental ecology, but also the waste of resources is caused. Therefore, the chemical nickel plating waste liquid is effectively treated, the environmental pollution and the ecological damage can be reduced, and the method has important significance for changing waste into valuable. In the prior art, the treatment process of the chemical nickel plating waste liquid has the problems of complex process and higher cost. Therefore, a low-cost treatment method capable of recovering nickel and phosphorus resources to the maximum extent is needed.
Disclosure of Invention
In view of the above problems, the present invention provides a method for treating an electroless nickel plating waste liquid with an iron-based catalyst at low cost and with high recovery rate of nickel/phosphorus resources.
The technical scheme of the invention is as follows: a method for treating chemical nickel plating waste liquid by an iron catalyst specifically comprises the following steps:
the method comprises the following steps: preparation of the support
Mixing 45-60 parts of diatomite, 20-30 parts of fly ash, 15-25 parts of perlite, 13-20 parts of phyllite and 8-12 parts of biological straw according to parts by weight to prepare ceramsite sand for later use;
step two: preparation of iron-based catalyst
Mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then loading the primary slurry product on the ceramsite sand;
step three: treatment of waste chemical nickel plating liquid
Firstly, adding CaO into the chemical nickel plating waste liquid until the pH value of the waste liquid is 6-8, and then adding the iron catalyst into the chemical nickel plating waste liquid according to the adding amount of 15-25 g/L for continuously stirring for 15-25 min; and then adding NaOH into the chemical nickel plating waste liquid until the pH value of the waste liquid is 12-13, so that most of nickel ions and other heavy metal ions in the waste liquid are subjected to precipitation reaction, then adding a proper amount of polymeric flocculant, continuously stirring for 0.5-1.5 h, and then treating in a sedimentation tank for discharging.
Further, the carrier in the step one is prepared by the following specific steps:
a. respectively crushing diatomite, fly ash, perlite, phyllite and biological straw, and sieving with a 200-mesh sieve;
b. putting 45-60 parts of diatomite, 20-30 parts of fly ash, 15-25 parts of perlite, 13-20 parts of phyllite and 8-12 parts of biological straw into stirring equipment according to parts by weight to obtain a mixed raw material, and adding deionized water with the volume ratio of the mixed raw material being 1: 5-8 to fully stir to obtain mixed aggregate;
c. then, aging the mixed aggregate for 24-36 h at the temperature of 30-60 ℃; the specific aging steps are as follows: controlling the temperature to be 35-45 ℃, controlling the aeration rate to be 15-18L/min, and introducing air for oxidation for 3 h; controlling the temperature to be 30-40 ℃, and aging for 5 hours; then aging at 40-60 ℃ for the rest of time;
d. granulating the aged mixed aggregate by using a granulator to obtain spherical ceramsite raw material with the particle size of 1.35-3 mm; the granulation comprises the following specific steps: granulating the aged and sublimated mixed aggregate by using disc pelletizing equipment in a mode of spraying atomized water, wherein the spraying amount of the water is 18-20 wt% of the mixed aggregate;
e. pretreating a spherical ceramsite raw material and calcining to obtain ceramsite sand; the method comprises the following specific steps: maintaining and drying the spherical ceramsite raw material at room temperature for 3-5 days, and calcining at 600-1200 ℃ to obtain ceramsite sand;
diatomite, fly ash, perlite and phyllite are used as substrates of ceramsite, so that the ceramsite has the characteristics of light capacity and strong adsorption capacity; biological straw is adopted to enable the ceramsite to have biological activated carbon in the later-stage ceramsite calcining process, so that on one hand, the attachment gaps can be effectively increased on the ceramsite structure, and on the other hand, the biological straw can play an adsorption role in the later-stage waste liquid treatment.
Furthermore, the biological straws are one or more of rice straws, wheat straws and corn straws; the straw stalks, the wheat stalks and the corn stalks have the characteristics of easily obtained raw materials and lower cost, and can effectively reduce the operation cost.
Further, the calcination in step e comprises the following specific steps: heating to 600 ℃ at the speed of 50 ℃/min, preserving heat for 30-45 min, heating to 800-950 ℃ at the speed of 10-15 ℃/min, preserving heat for 20-30 min, heating to 1050-1200 ℃ at the speed of 5-10 ℃/min, preserving heat for 60-80 min, cooling to 600 ℃ at the speed of 50 ℃/min, and naturally cooling to finish calcination; the adoption of gradient operation can ensure that the mineral crystals completely develop during calcination; when the temperature is raised to 600 ℃ at the speed of 50 ℃/min during calcination, the temperature raising speed is reduced, so that the biological straws can be more fully combusted, the carbonization filtration can be greatly increased, and the void ratio after the ceramsite is formed can be effectively improved.
Further, the specific steps of the second step are as follows: mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then carrying out magnetization treatment on the primary slurry product in an environment with the magnetic field intensity of 1.3-1.5T to obtain magnetized slurry; then loading the magnetized slurry on the ceramsite sand in a spraying mode; then drying the mixture in the atmosphere of nitrogen to obtain an iron catalyst; wherein the volume ratio of the ceramsite sand to the magnetized slurry is 1: 1.2-1.4; the primary slurry product can be effectively attached to the surface of the ceramsite sand by a spraying mode.
Further, the specific steps of the second step are as follows: mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then, placing the ceramsite sand into the primary slurry product according to the volume ratio of 1:1.5, and soaking for 30-45 min in an environment with the magnetic field intensity of 1.3-1.5T; then placing the soaked ceramsite sand into a muffle furnace at 450 ℃ to be calcined for 2 hours to prepare an iron-based catalyst; the mode that utilizes to soak can make the slurried product of first generation combine more evenly with the ceramsite sand under the effect of magnetic field for the slurried product of first generation can permeate in the space of ceramsite sand effectively and go, possesses better performance in the waste liquid treatment of later stage.
Further, compressing the bottom waste residue of the sedimentation tank in the third step and then recycling the waste residue; the waste of resources that can avoid realizes that the wastes material becomes precious.
And further, polyaluminum chloride is adopted as the polymeric flocculant in the third step, and the adding amount is 1.5-3 mg/L.
Compared with the prior art, the invention has the beneficial effects that:
1. the method has the advantages of simple process and low operation cost in the aspect of treating the nickel plating waste liquid;
2. the iron catalyst prepared by adopting the high molecular polymeric iron can oxidize and break the complexing agent in the chemical nickel plating waste liquid to enable nickel ions to be in a free state, thereby being more beneficial to forming precipitates in the later period; the concentration of nickel ions in the waste liquid can be effectively reduced, and the subsequent standard-reaching treatment is facilitated;
3. in the invention, the iron catalyst prepared by using the specially-made ceramsite sand as the load is used for subsequent waste residue treatment, and the precipitate can be loaded on the ceramsite sand, so that the later waste residue treatment is more convenient.
Detailed Description
Example 1: a method for treating chemical nickel plating waste liquid by an iron catalyst specifically comprises the following steps:
the method comprises the following steps: preparation of the support
a. Respectively crushing diatomite, fly ash, perlite, phyllite and biological straw, and sieving with a 200-mesh sieve; wherein the biological straw is rice straw;
b. putting 45 parts of diatomite, 20 parts of fly ash, 15 parts of perlite, 13 parts of phyllite and 8 parts of biological straw into stirring equipment according to the parts by weight to obtain a mixed raw material, and adding deionized water with the volume ratio of the mixed raw material to the mixed raw material being 1:5 for fully stirring to obtain mixed aggregate;
c. then aging the mixed aggregate for 30 hours; the specific aging steps are as follows: controlling the temperature to be 35 ℃, controlling the aeration rate to be 15L/min, and introducing air for oxidation for 3 h; controlling the temperature to be 30 ℃, and aging for 5 h; then controlling the temperature to 40 ℃ and aging for 16 h;
d. granulating the aged mixed aggregate by using a granulator to obtain spherical ceramsite raw material with the particle size of 1.35-3 mm; the granulation comprises the following specific steps: granulating the aged and sublimated mixed aggregate by using a disc pelletizing device in a mode of spraying atomized water, wherein the spraying amount of the water is 18 wt% of the mixed aggregate;
e. pretreating a spherical ceramsite raw material and calcining to obtain ceramsite sand; the method comprises the following specific steps: maintaining and drying the spherical ceramsite raw material at room temperature for 3d, and then calcining to obtain ceramsite sand for later use; wherein, the calcination comprises the following specific steps: heating to 600 ℃ at the speed of 50 ℃/min, preserving heat for 30min, heating to 800 ℃ at the speed of 10 ℃/min, preserving heat for 20min, heating to 1050 ℃ at the speed of 5 ℃/min, preserving heat for 60min, cooling to 600 ℃ at the speed of 50 ℃/min, and naturally cooling to finish calcining;
step two: preparation of iron-based catalyst
Mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then carrying out magnetization treatment on the primary slurry product in an environment with the magnetic field intensity of 1.3T to obtain magnetized slurry; then loading the magnetized slurry on the ceramsite sand in a spraying mode; then drying the mixture in the atmosphere of nitrogen to obtain an iron catalyst; wherein the volume ratio of the ceramsite sand to the magnetized slurry is 1: 1.2;
step three: treatment of waste chemical nickel plating liquid
Firstly, adding CaO into the chemical nickel plating waste liquid until the pH value of the waste liquid is 6, and then adding an iron catalyst into the chemical nickel plating waste liquid according to the adding amount of 15g/L for continuously stirring for 15 min; then adding NaOH into the chemical nickel plating waste liquid until the pH value of the waste liquid is 12, leading most of nickel ions in the waste liquid and other heavy metal ions to have precipitation reaction, then adding a proper amount of polymeric flocculant, continuously stirring for 0.5h, and then treating the waste liquid in a sedimentation tank for discharging; wherein, the waste residue at the bottom of the sedimentation tank is compressed and then recycled; the polymeric flocculant is polyaluminium chloride, and the dosage is 1.5 mg/L.
Example 2: the difference from example 1 is: a method for treating chemical nickel plating waste liquid by an iron catalyst specifically comprises the following steps:
the method comprises the following steps: preparation of the support
a. Respectively crushing diatomite, fly ash, perlite, phyllite and biological straw, and sieving with a 200-mesh sieve; wherein the biological straw is wheat straw;
b. 50 parts of diatomite, 25 parts of fly ash, 20 parts of perlite, 18 parts of phyllite and 11 parts of biological straw are put into stirring equipment according to the parts by weight to obtain a mixed raw material, and then deionized water with the volume ratio of the mixed raw material to the mixed raw material being 1:7 is added for fully stirring to obtain mixed aggregate;
c. then aging the mixed aggregate for 30 hours; the specific aging steps are as follows: controlling the temperature at 40 ℃, controlling the aeration rate at 16L/min, and introducing air for oxidation for 3 h; controlling the temperature to be 35 ℃, and aging for 5 h; then aging for 22h at the temperature of 50 ℃;
d. granulating the aged mixed aggregate by using a granulator to obtain spherical ceramsite raw material with the particle size of 1.35-3 mm; the granulation comprises the following specific steps: granulating the aged and sublimated mixed aggregate by using a disc pelletizing device in a mode of spraying atomized water, wherein the spraying amount of the water is 19 wt% of the mixed aggregate;
e. pretreating a spherical ceramsite raw material and calcining to obtain ceramsite sand; the method comprises the following specific steps: maintaining and drying the spherical ceramsite raw material at room temperature for 4 days, and then calcining to obtain ceramsite sand for later use; wherein, the calcination comprises the following specific steps: heating to 600 ℃ at the speed of 50 ℃/min, preserving heat for 40min, heating to 900 ℃ at the speed of 15 ℃/min, preserving heat for 25min, heating to 1100 ℃ at the speed of 8 ℃/min, preserving heat for 70min, cooling to 600 ℃ at the speed of 50 ℃/min, and naturally cooling to finish calcining;
step two: preparation of iron-based catalyst
Mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then carrying out magnetization treatment on the primary slurry product in an environment with the magnetic field intensity of 1.4T to obtain magnetized slurry; then loading the magnetized slurry on the ceramsite sand in a spraying mode; then drying the mixture in the atmosphere of nitrogen to obtain an iron catalyst; wherein the volume ratio of the ceramsite sand to the magnetized slurry is 1: 1.3;
step three: treatment of waste chemical nickel plating liquid
Firstly, adding CaO into the chemical nickel plating waste liquid until the pH value of the waste liquid is 7, and then adding an iron catalyst into the chemical nickel plating waste liquid according to the adding amount of 20g/L for continuously stirring for 20 min; then adding NaOH into the chemical nickel plating waste liquid until the pH value of the waste liquid is 12, leading most of nickel ions in the waste liquid and other heavy metal ions to have precipitation reaction, then adding a proper amount of polymeric flocculant, continuously stirring for 1h, and then treating the mixture in a sedimentation tank for discharging; wherein, the waste residue at the bottom of the sedimentation tank is compressed and then recycled; the polymeric flocculant is polyaluminium chloride, and the dosage is 2 mg/L.
Example 3: the difference from example 1 is: a method for treating chemical nickel plating waste liquid by an iron catalyst specifically comprises the following steps:
the method comprises the following steps: preparation of the support
a. Respectively crushing diatomite, fly ash, perlite, phyllite and biological straw, and sieving with a 200-mesh sieve; wherein the biological straw is corn straw;
b. 60 parts of diatomite, 30 parts of fly ash, 25 parts of perlite, 20 parts of phyllite and 12 parts of biological straw are put into stirring equipment according to the parts by weight to obtain a mixed raw material, and then deionized water with the volume ratio of 1:8 to the mixed raw material is added for fully stirring to obtain mixed aggregate;
c. then, carrying out aging treatment on the mixed aggregate for 36 hours; the specific aging steps are as follows: controlling the temperature at 45 ℃ and the aeration rate at 18L/min, and introducing air for oxidation for 3 h; controlling the temperature to be 40 ℃, and aging for 5 h; then controlling the temperature to be 40-60 ℃ and aging for 28 h;
d. granulating the aged mixed aggregate by using a granulator to obtain spherical ceramsite raw material with the particle size of 1.35-3 mm; the granulation comprises the following specific steps: granulating the aged and sublimated mixed aggregate by using a disc pelletizing device in a mode of spraying atomized water, wherein the spraying amount of the water is 20 wt% of the mixed aggregate;
e. pretreating a spherical ceramsite raw material and calcining to obtain ceramsite sand; the method comprises the following specific steps: maintaining and drying the spherical ceramsite raw material at room temperature for 5 days, and then calcining to obtain ceramsite sand for later use; wherein, the calcination comprises the following specific steps: heating to 600 ℃ at the speed of 50 ℃/min, preserving heat for 45min, heating to 950 ℃ at the speed of 15 ℃/min, preserving heat for 30min, heating to 1200 ℃ at the speed of 10 ℃/min, preserving heat for 80min, cooling to 600 ℃ at the speed of 50 ℃/min, and naturally cooling to finish calcining;
step two: preparation of iron-based catalyst
Mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then carrying out magnetization treatment on the primary slurry product in an environment with the magnetic field intensity of 1.5T to obtain magnetized slurry; then loading the magnetized slurry on the ceramsite sand in a spraying mode; then drying the mixture in the atmosphere of nitrogen to obtain an iron catalyst; wherein the volume ratio of the ceramsite sand to the magnetized slurry is 1: 1.4;
step three: treatment of waste chemical nickel plating liquid
Firstly, adding CaO into the chemical nickel plating waste liquid until the pH value of the waste liquid is 8, and then adding an iron catalyst into the chemical nickel plating waste liquid according to the adding amount of 25g/L for continuously stirring for 25 min; then adding NaOH into the chemical nickel plating waste liquid until the pH value of the waste liquid is 13, so that most of nickel ions in the waste liquid and other heavy metal ions are subjected to precipitation reaction, then adding a proper amount of polymeric flocculant, continuously stirring for 0.5-1.5 h, and then treating the waste liquid in a sedimentation tank for discharging; wherein, the waste residue at the bottom of the sedimentation tank is compressed and then recycled; the polymeric flocculant is polyaluminium chloride, and the dosage is 3 mg/L.
Example 4: the difference from example 1 is: the biological straw is a mixture of straw, wheat straw and corn straw mixed according to a volume ratio of 1:2: 1; the second step can be replaced by: mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then placing the ceramsite sand into the primary slurry product according to the volume ratio of 1:1.5, and soaking for 30min in an environment with the magnetic field intensity of 1.3T; and then putting the soaked ceramsite sand into a muffle furnace at 450 ℃ for calcining for 2 hours to prepare the iron-based catalyst.
Example 5: the difference from example 1 is: a mixture of rice straw and wheat straw mixed according to the volume ratio of 1:1 is adopted; the second step can be replaced by: mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then placing the ceramsite sand into the primary slurry product according to the volume ratio of 1:1.5, and soaking for 40min in an environment with the magnetic field intensity of 1.4T; and then putting the soaked ceramsite sand into a muffle furnace at 450 ℃ for calcining for 2 hours to prepare the iron-based catalyst.
Example 6: the difference from example 1 is: a mixture of rice straw, wheat straw and corn straw in a volume ratio of 1:1:1 is adopted; the second step can be replaced by: mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then placing the ceramsite sand into the primary slurry product according to the volume ratio of 1:1.5, and soaking for 45min in an environment with the magnetic field intensity of 1.5T; and then putting the soaked ceramsite sand into a muffle furnace at 450 ℃ for calcining for 2 hours to prepare the iron-based catalyst.
Test example: the method of the embodiment 1-6 is used for treating the chemical nickel plating waste liquid of a certain enterprise, the waste liquid before treatment and the discharge liquid after treatment are respectively detected, and the detection results are shown in the table 1:
TABLE 1 monitoring results of the waste liquid before treatment and the effluent after treatment
And (4) conclusion: as can be seen from the above detection data, when the chemical nickel plating waste liquid is treated by the method of the embodiments 1 to 6 of the invention, the removal rate of nickel reaches more than 95%, and COD, phosphorus and ammonia nitrogen can reach the discharge standard.
Claims (8)
1. A method for treating chemical nickel plating waste liquid by an iron catalyst is characterized by comprising the following steps:
the method comprises the following steps: preparation of the support
Mixing 45-60 parts of diatomite, 20-30 parts of fly ash, 15-25 parts of perlite, 13-20 parts of phyllite and 8-12 parts of biological straw according to parts by weight to prepare ceramsite sand for later use;
step two: preparation of iron-based catalyst
Mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then loading the primary slurry product on the ceramsite sand;
step three: treatment of waste chemical nickel plating liquid
Firstly, adding CaO into the chemical nickel plating waste liquid until the pH value of the waste liquid is 6-8, and then adding the iron catalyst into the chemical nickel plating waste liquid according to the adding amount of 15-25 g/L for continuously stirring for 15-25 min; and then adding NaOH into the chemical nickel plating waste liquid until the pH value of the waste liquid is 12-13, so that most of nickel ions and other heavy metal ions in the waste liquid are subjected to precipitation reaction, then adding a proper amount of polymeric flocculant, continuously stirring for 0.5-1.5 h, and then treating in a sedimentation tank for discharging.
2. The method for treating chemical nickel plating waste liquid by using iron-based catalyst according to claim 1, wherein the carrier in the first step is prepared by the following specific steps:
a. respectively crushing diatomite, fly ash, perlite, phyllite and biological straw, and sieving with a 200-mesh sieve;
b. putting 45-60 parts of diatomite, 20-30 parts of fly ash, 15-25 parts of perlite, 13-20 parts of phyllite and 8-12 parts of biological straw into stirring equipment according to parts by weight to obtain a mixed raw material, and adding deionized water with the volume ratio of the mixed raw material being 1: 5-8 to fully stir to obtain mixed aggregate;
c. then, aging the mixed aggregate for 24-36 h at the temperature of 30-60 ℃; the specific aging steps are as follows: controlling the temperature to be 35-45 ℃, controlling the aeration rate to be 15-18L/min, and introducing air for oxidation for 3 h; controlling the temperature to be 30-40 ℃, and aging for 5 hours; then aging at 40-60 ℃ for the rest of time;
d. granulating the aged mixed aggregate by using a granulator to obtain spherical ceramsite raw material with the particle size of 1.35-3 mm; the granulation comprises the following specific steps: granulating the aged and sublimated mixed aggregate by using disc pelletizing equipment in a mode of spraying atomized water, wherein the spraying amount of the water is 18-20 wt% of the mixed aggregate;
e. pretreating a spherical ceramsite raw material and calcining to obtain ceramsite sand; the method comprises the following specific steps: and curing the spherical ceramsite raw material at room temperature, drying for 3-5 days, and calcining at 600-1200 ℃ to obtain the ceramsite sand.
3. The method for treating the chemical nickel plating waste liquid by the iron-based catalyst according to any one of claims 1 or 2, wherein the biological straw is one or more of straw, wheat straw and corn straw.
4. The method of claim 1 wherein said primary slurry product of step two is prepared by mixing polymeric ferric salt with an aqueous alkaline solution and reacting.
5. The method for treating the chemical nickel plating waste liquid by the iron-based catalyst according to claim 1, wherein the second step comprises the following specific steps: mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then carrying out magnetization treatment on the primary slurry product in an environment with the magnetic field intensity of 1.3-1.5T to obtain magnetized slurry; then loading the magnetized slurry on the ceramsite sand in a spraying mode; then drying the mixture in the atmosphere of nitrogen to obtain an iron catalyst; wherein the volume ratio of the ceramsite sand to the magnetized slurry is 1: 1.2-1.4.
6. The method for treating the chemical nickel plating waste liquid by the iron-based catalyst according to claim 1, wherein the second step comprises the following specific steps: mixing and reacting high-molecular polymeric ferric salt with an alkaline aqueous solution to obtain a primary slurry product; then, placing the ceramsite sand into the primary slurry product according to the volume ratio of 1:1.5, and soaking for 30-45 min in an environment with the magnetic field intensity of 1.3-1.5T; and then putting the soaked ceramsite sand into a muffle furnace at 450 ℃ for calcining for 2 hours to prepare the iron-based catalyst.
7. The method of claim 1 wherein the bottom sludge from step three is recycled after compression treatment.
8. The method of claim 1, wherein polymeric aluminum chloride is used as the polymeric flocculant in step three, and the dosage of polymeric aluminum chloride is 1.5-3 mg/L.
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