CN111282965B - Method for preparing magnetic material LDH (layered double hydroxide) by recycling electroplating sludge - Google Patents
Method for preparing magnetic material LDH (layered double hydroxide) by recycling electroplating sludge Download PDFInfo
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- 239000010802 sludge Substances 0.000 title claims abstract description 51
- 238000009713 electroplating Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000000696 magnetic material Substances 0.000 title claims abstract description 13
- 238000004064 recycling Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 49
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000002253 acid Substances 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 229910052742 iron Inorganic materials 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000002386 leaching Methods 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000010335 hydrothermal treatment Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 9
- 238000010790 dilution Methods 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 230000005389 magnetism Effects 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 238000007865 diluting Methods 0.000 abstract 1
- 238000007747 plating Methods 0.000 description 13
- 239000000047 product Substances 0.000 description 12
- 239000003929 acidic solution Substances 0.000 description 7
- 229910021645 metal ion Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000012670 alkaline solution Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 239000012716 precipitator Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
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- 238000004458 analytical method Methods 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 208000007443 Neurasthenia Diseases 0.000 description 1
- 206010042496 Sunburn Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000035475 disorder Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/80—Destroying solid waste or transforming solid waste into something useful or harmless involving an extraction step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for preparing magnetic material LDH by recycling electroplating sludge, which comprises the following steps: (1) Ultrasonic leaching of metal elements in the nickel-containing electroplating sludge by using a dilute acid solution, and mechanical removal of insoluble matters in the nickel-containing electroplating sludge to obtain a dilute acid solution containing metal elements; (2) Adding ferric salt or iron-containing solution of leached iron ore, and stirring until the mixture is uniform to obtain dilute acid solution containing iron; (3) Diluting with water, adding urea, performing hydrothermal treatment, filtering to obtain brown solid, washing, drying, and grinding. The invention uses Fe 3+ And Ni 2+ The constructed magnetic centers are dispersed in the LDHs structure, so that the magnetic structure is introduced, and the demagnetizing phenomenon can be avoided; the used equipment is simple, the treatment process is economic and efficient, the environment is protected, the obtained LDH has stronger magnetism and large specific surface area, and the LDH has higher adsorption performance on organic pollutants in water.
Description
Technical Field
The invention relates to the technical field of solid waste recycling, in particular to a method for preparing magnetic material LDH by recycling electroplating sludge.
Background
Nickel-containing plating sludge produced by the nickel plating process is classified as hazardous waste (346-054-17) in many countries and regions, and the current plating sludge treatment methods include solidification treatment, chemical treatment, heat treatment, physical treatment and the like. The solidification treatment method is to wrap the electroplating sludge by using cement materials and then to fill the electroplating sludge, and the treatment method has the advantages of low cost and simple technology, and becomes a main mode for treating the electroplating sludge, however, metal ions such as Ni, cr, zn, cu in the solidified product are dissolved out and permeated into soil and groundwater after sunburn and rain, so that diseases such as human skin inflammation, neurasthenia, physiological system disorder and the like are caused. The chemical treatment method has the advantages of high speed, high efficiency and thorough treatment, but a large amount of concentrated waste acid, waste alkali and complex leaching solution are required to be treated in the method. Harmless and resource treatment of nickel-containing sludge is urgent.
2.88 in precursor<M 2+ ：M 3+ <And 4, forming layered double hydroxide nano materials (LDHs), rapidly generating high-crystalline LDHs by controlling a double-jet precipitation method CDJP, removing copper and zinc in wastewater, and preparing NiFe-LDHs by a coprecipitation hydrothermal method. LDHs has the characteristics of anion exchangeability, large specific surface area, flexible structure and the like, so the LDHs is often used as an adsorbent and has extensive research in the field of water pollution treatment. There are reports on research using LDH, LDO as ion exchanger or adsorbent in printing and dyeing, paper making, electroplating, and nuclear wastewater treatment. Removal of complex anions of certain metal ions in solution, e.g. NiCN, by ion exchange, e.g. with LDH + 、CrO 4 Etc.; the ion exchange performance of LDHs is similar to that of anion exchange resin, but the ion exchange capacity is relatively larger like hydrotalcite, 3.33mg/g, high temperature resistance of 300 ℃, radiation resistance, no aging, high density and small volume. LDO has stronger adsorption capacity to metal ions, such as Co ions in nuclear wastewater, and powdery LDHs has the problems of difficult recovery and easy secondary pollution.
With researchers using Fe 3 O 4 As a magnetic center, fe was constructed 3 O 4 LDHs composite material, but Fe in the structure has two types of divalent and trivalent, has weak acid resistance and is easy to oxidize into ferric oxide (Fe) 2 O 3 ) Resulting in structural deformation and degaussing, and are subject to a number of limitations in use in aqueous systems. Therefore, how to utilize electroplating sludge for recyclingPreparing magnetic material LDHs is a problem that needs to be addressed by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a method for preparing magnetic material LDH by recycling electroplating sludge, which takes electroplating sludge (mainly nickel-containing sludge) as a starting point, and acid leaching is carried out on metal ions in the electroplating sludge, and a hydrothermal process flow is adopted to prepare the magnetic material LDH by using the electroplating sludge as a precursor, so that not only can sludge accumulated in the electroplating industry be treated, but also a new economical idea and a new technological demonstration are provided for the treatment of sludge of electroplating enterprises, the equipment is simple, the operability is high, the large-scale continuous industrial production can be realized, and the current environmental problem can be solved.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the method for preparing the magnetic material LDH by recycling the electroplating sludge specifically comprises the following steps:
(1) Ultrasonic leaching of metal elements in the nickel-containing electroplating sludge by using a dilute acid solution, and mechanical removal of insoluble matters in the nickel-containing electroplating sludge to obtain a dilute acid solution containing metal elements;
(2) Adding ferric salt or iron-containing solution for leaching iron ore into the dilute acid solution containing metal elements obtained in the step (1), and stirring until the mixture is uniform to obtain the dilute acid solution containing iron;
(3) Adding water into the dilute acid solution containing iron obtained in the step (2) for dilution, then adding urea for hydro-thermal treatment, filtering to obtain brown solid, washing, drying and grinding to obtain the magnetic material LDH.
The reaction principle of the invention is as follows: in the hydrothermal process, alpha-Ni (OH) is synthesized 2 At the beginning of the reaction of the structure, urea is neutral in aqueous solution and metal ions form a homogeneous solution with OC (NH 2 ) 2 Decomposition of (2) to generate OCN - And NH 4 + The pH value in the solution is synchronously improved, ni 2+ /Fe 3+ The plasma metal ions generate complex and hydrolysis process to generate Ni (H) 2 O) 6 2+ Due to Fe 3+ Is easier to hydrolyze to form Fe (OH) 3 Nanocrystal core, fe (OH) 3 And Ni(H 2 O) 6 2+ Water loss to become magnetic Fe 2 NiO 3 ，Ni(NH 3 ) 6 2+ 、Ni(NCO) 2 、NiNCO + And the plasma grows around the magnetic center, and finally NiFe-LDHs is formed.
The invention has the beneficial effects that: using Fe 3+ And Ni 2+ The constructed magnetic centers are dispersed in the LDHs structure, so that the magnetic structure is introduced, and the demagnetizing phenomenon can be avoided; the method has the advantages of simple equipment, economic and efficient treatment process, green and environment-friendly treatment, and the obtained LDH has stronger magnetism, large specific surface area and higher adsorption performance on organic pollutants in water.
Further, in the step (1), the nickel component content in the nickel-containing plating sludge is more than 90wt%.
Further, in the step (1), the dilute acid solution is a hydrochloric acid solution or a sulfuric acid solution, preferably a hydrochloric acid solution; the concentration is 0.5 to 5mol/L, preferably 1mol/L.
The method has the further beneficial effect that the dilute acid solution is added for dissolving the metal ions in the solid nickel-containing electroplating sludge.
Further, in the step (1), the time of the ultrasonic treatment is 0.5 to 4 hours, preferably 1 hour.
The ultrasonic wave is used for accelerating the dissolution process, and finally a transparent green solution is formed.
Further, in the above step (2), the iron salt or iron-containing solution for leaching iron ore is used in such an amount that Ni in the final product 2+ And Fe (Fe) 3+ The molar ratio of (2) is 3.5 to 4, preferably 3.8.
Further, in the step (2), the pH of the diluted hydrochloric acid solution containing iron is 1 to 3, preferably 2.
In the step (3), urea is used in an amount such that the pH of the hydrothermal solution is 9 to 10.
Further, in the step (3), the hydrothermal temperature of the hydrothermal treatment is 100 to 200 ℃, preferably 160 ℃; the time is 1.5 to 15 hours, preferably 10 hours.
The adoption of the method has the further beneficial effects that in the hydrothermal process, ni2+ and Fe3+ form precipitation or complexation along with the improvement of alkalinity, and the target product is generated by crystallization.
In the step (3), the washing method comprises centrifugation, suction filtration and filtration.
Further, the method also comprises the following step (4): and (3) circulating the solution obtained by filtering in the step (3) as dilution water, and obtaining high-quality metal salt by adopting a fractional precipitation method when impurity ions in the filtrate are high to a certain degree.
Compared with the prior art, the invention discloses a method for preparing magnetic material LDH by electroplating sludge recycling, which has the following beneficial effects;
(1) Breaks through the technical bottleneck of recycling the electroplating sludge, has high economic benefit and strong operability;
(2) Preparing a NiFe-LDHs adsorbent with a magnetic center;
(3) Provides a new economical and applicable idea and process demonstration for sludge treatment for electroplating enterprises.
Drawings
Fig. 1 is a process flow diagram of a method for preparing magnetic material LDH by electroplating sludge recycling according to the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the examples of the present invention, XRF component analysis of the plating sludge is shown in Table 1.
TABLE 1 XRF component analysis Table for electroplating sludge
Example 1
(1) 1.0000g of electroplating sludge (pretreated by drying, grinding and sieving at 105 ℃ C., the specific components are shown in the following table) is weighed, firstly, 49.00mL of aqueous solution is used for soaking for 10min, then 17mL of 1mol/L hydrochloric acid solution is added, ultrasonic treatment is carried out for 30min, and supernatant fluid is centrifugally taken;
(2) Taking 15.00mL of clear liquid obtained in the step (1), adding 0.2700g of FeCl 3 ·H 2 O, such that Ni in the final product 2+ And Fe (Fe) 3+ The molar ratio of (2) is 3.8;
(3) Adding deionized water (or filtrate) into the acidic solution obtained in the step (2) to dilute 60.00mL, then adding 0.5400g urea as a precipitator, transferring the mixed system to a polytetrafluoroethylene lining of 100mL, putting into a stainless steel reaction kettle, heating to 160 ℃ in an oven for 10 hours, filtering to obtain brown solid, washing, drying and grinding to obtain an LDHs sample;
(4) The solution obtained by filtration is alkaline solution, and can be returned to the step (3) to be used as dilution water, and when the impurity ions in the filtrate are high to a certain degree, a step-by-step precipitation method is adopted to obtain high-quality metal salt.
The electroplating sludge is treated in the embodiment 1, and 0.42g (the yield is 185.20%) of chemical products with higher added value of magnetic LDHs are obtained. ( Remarks: yield = mass of magnetic LDHs obtained/mass of total plating sludge in plating sludge leaching solution. )
Example 2
(1) Weighing 10.0000g of electroplating sludge (subjected to pretreatment of drying, grinding and sieving at 105 ℃), soaking for 10min by 490.0mL of aqueous solution, adding 170mL of 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 30min, and centrifuging to obtain supernatant;
(2) Taking 150.00mL of clear liquid obtained in the step (1), adding 2.700g of FeCl 3 ·H 2 O, so that Ni in the final acidic solution 2+ And Fe (Fe) 3+ The molar ratio of (2) is 3.8;
(3) Adding deionized water (or filtrate) into the acidic solution obtained in the step (2) to dilute to 600.00mL, then adding 5.400g of urea as a precipitator, transferring the mixed system to a 1L polytetrafluoroethylene lining, putting into a stainless steel reaction kettle, heating to 160 ℃ in an oven for 10 hours, filtering to obtain brown solid, washing, drying and grinding to obtain an LDHs sample;
(4) The solution obtained by filtration is alkaline solution, and can be returned to the step (3) to be used as dilution water, and when the impurity ions in the filtrate are high to a certain degree, a step-by-step precipitation method is adopted to obtain high-quality metal salt.
The electroplating sludge is treated in the embodiment 2, so that 4.2g (yield is 185.20%) of chemical products with higher added value of magnetic LDHs are obtained, and the products reach the class II first-class product standard (GB/T6009-2014) through testing. ( Remarks: yield = mass of magnetic LDHs obtained/mass of total plating sludge in plating sludge leaching solution. )
Example 3
(1) Weighing 100.0000g of electroplating sludge (subjected to pretreatment of drying, grinding and sieving at 105 ℃), soaking for 10min by using 4.9L of aqueous solution, adding 1.7L of 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 30min, and centrifuging to obtain supernatant;
(2) Taking 1.5L of clear liquid obtained in the step (1), adding 27.00g of FeCl 3 ·H 2 O, so that Ni in the final acidic solution 2+ And Fe (Fe) 3+ The molar ratio of (2) is 3.8;
(3) Adding deionized water into the acidic solution obtained in the step (2) to dilute to 6L, then adding 54g of urea as a precipitator, transferring the mixed system to a 10L polytetrafluoroethylene lining, putting into a stainless steel reaction kettle, heating to 160 ℃ in an oven, maintaining for 10h, filtering to obtain brown solid, washing, drying and grinding to obtain an LDHs sample;
(4) The solution obtained by filtration is alkaline solution, and can be returned to the step (3) to be used as dilution water, and when the impurity ions in the filtrate are high to a certain degree, a step-by-step precipitation method is adopted to obtain high-quality metal salt.
The embodiment processes electroplating sludge to obtain chemical products with high added value, wherein the magnetic LDHs is 42g (yield is 185.20%), and the products reach the class II first-class product standard (GB/T6009-2014) through testing. ( Remarks: yield = mass of magnetic LDHs obtained/mass of total plating sludge in plating sludge leaching solution. )
Example 4
(1) Weighing 1kg of electroplating sludge (subjected to pretreatment of drying, grinding and sieving at 105 ℃), soaking for 10min by using 49L of aqueous solution, adding 17L of 1mol/L hydrochloric acid solution, performing ultrasonic treatment for 30min, and centrifuging to obtain supernatant;
(2) Taking 15L of clear liquid obtained in the step (1), adding 2.7kg of FeCl 3 ·H 2 O, so that Ni in the final acidic solution 2+ And Fe (Fe) 3+ The molar ratio of (2) is 3.8;
(3) Adding deionized water (or filtrate) into the acidic solution obtained in the step (2) to dilute to 60L, then adding 0.5400g of urea as a precipitator, transferring the mixed system to a 100L polytetrafluoroethylene lining, putting into a stainless steel reaction kettle, heating to 160 ℃ in an oven for 10h, filtering to obtain brown solid, washing, drying and grinding to obtain an LDHs sample;
(4) The solution obtained by filtration is alkaline solution, and can be returned to the step (3) to be used as dilution water, and when the impurity ions in the filtrate are high to a certain degree, a step-by-step precipitation method is adopted to obtain high-quality metal salt.
The embodiment processes electroplating sludge to obtain 420g (yield is 185.20%) of magnetic LDHs chemical products with higher added value, and the products reach the class II first-class product standard (GB/T6009-2014) through test. ( Remarks: yield = mass of magnetic LDHs obtained/mass of total plating sludge in plating sludge leaching solution. )
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (1)
1. The method for preparing the magnetic material LDH by recycling the electroplating sludge is characterized by comprising the following steps of:
(1) Using dilute acid solution to carry out ultrasonic treatment for 0.5-4 hours to leach metal elements in the nickel-containing electroplating sludge, and mechanically removing insoluble matters in the nickel-containing electroplating sludge to obtain dilute acid solution containing metal elements;
wherein the nickel component content in the nickel-containing electroplating sludge is more than 90wt%;
the dilute acid solution is hydrochloric acid solution or sulfuric acid solution, and the concentration is 0.5-5 mol/L;
(2) Adding ferric salt or iron-containing solution for leaching iron ore into dilute acid solution containing metal elements obtained in step (1) to enable Ni in final product 2+ And Fe (Fe) 3+ The molar ratio of (2) is 3.5-4, and stirring is carried out until the mixture is uniformly mixed, thus obtaining a dilute acid solution containing iron with the pH value of 1-3;
(3) Adding water into the dilute acid solution containing iron obtained in the step (2) for dilution, then adding urea for hydro-thermal treatment, filtering to obtain brown solid, washing, drying and grinding to obtain the magnetic material LDH;
the dosage of the urea is that the pH value of the solution after hydrothermal treatment is 9-10; the hydrothermal temperature of the hydrothermal treatment is 100-200 ℃ and the time is 1.5-10 h; the washing mode comprises centrifugation, suction filtration and filtration;
(4) And (3) circulating the solution obtained by filtering in the step (3) as dilution water, and obtaining high-quality metal salt by adopting a fractional precipitation method when impurity ions in filtrate are high to a certain degree.
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| CN202010152249.XA CN111282965B (en) | 2020-03-06 | 2020-03-06 | Method for preparing magnetic material LDH (layered double hydroxide) by recycling electroplating sludge |
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| CN113083216B (en) * | 2021-04-23 | 2023-11-10 | 江苏大学 | Two-dimensional nickel-based composite metal oxide adsorbent, preparation method and application of adsorbent in removing phosphate radical |
| CN114984932B (en) * | 2022-06-01 | 2023-11-21 | 纽博恩(佛山)科技有限公司 | Method for preparing LDHs adsorption material by using electroplating sludge and application |
| CN115193394A (en) * | 2022-07-15 | 2022-10-18 | 江苏大学 | Method for preparing defluorination separation column filler by using double-solid waste sludge |
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