CN117682553A - Recycling treatment method for waste lead plaster - Google Patents
Recycling treatment method for waste lead plaster Download PDFInfo
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- CN117682553A CN117682553A CN202311635599.1A CN202311635599A CN117682553A CN 117682553 A CN117682553 A CN 117682553A CN 202311635599 A CN202311635599 A CN 202311635599A CN 117682553 A CN117682553 A CN 117682553A
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- Prior art keywords
- lead
- lead plaster
- waste lead
- recycling waste
- acetic acid
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- 239000002699 waste material Substances 0.000 title claims abstract description 41
- 239000011505 plaster Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004064 recycling Methods 0.000 title claims abstract description 21
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 229940046892 lead acetate Drugs 0.000 claims abstract description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 238000001354 calcination Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 15
- 230000032683 aging Effects 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- YBCVMFKXIKNREZ-UHFFFAOYSA-N acoh acetic acid Chemical compound CC(O)=O.CC(O)=O YBCVMFKXIKNREZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000003480 eluent Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012047 saturated solution Substances 0.000 claims description 4
- 238000010517 secondary reaction Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000002253 acid Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000047 product Substances 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for recycling waste lead plaster, and relates to the technical field of waste lead plaster. According to the invention, the waste lead paste is used as a raw material, and the problems that the waste lead paste is difficult to efficiently prepare nano lead titanate products with uniform particle size and the like are solved by the steps of pretreatment, preparation of lead acetate crystals, preparation of nano lead titanate and the like, so that the environment-friendly recycling treatment of the waste lead paste is realized.
Description
Technical Field
The invention relates to the technical field of waste lead plaster, in particular to a waste lead plaster recycling treatment method.
Background
The lead plaster contained in the waste lead-acid battery contains a large amount of lead compounds. The proportion of the lead plaster in the waste lead-acid battery is generally 30-40 wt%, which is the most research value in the waste lead-acid battery and is the most difficult part to treat. At present, the traditional waste lead plaster recovery treatment process mainly comprises the following three types: the method has the outstanding problems of longer process flow, high energy consumption, secondary pollution of waste gas and the like.
Lead titanate (PT) is an excellent ferroelectric substrate substance, and has important research significance in the aspects of high-frequency filters, pyroelectric detectors, gas sensors, photocatalysts and the like. At present, the PT nano powder is generally prepared by adopting pure lead acetate and other raw materials.
Therefore, how to use the waste lead paste as the raw material to realize the efficient preparation of the nano lead titanate is one of the effective ideas for realizing the environment-friendly recycling treatment of the waste lead paste.
Disclosure of Invention
In order to solve the problems, the invention provides a method for recycling waste lead paste, which realizes the recycling treatment of the waste lead paste and the efficient preparation of nano lead titanate products with uniform particle size distribution.
The method for recycling the waste lead plaster comprises the following steps:
s1, grinding the lead plaster into powder, washing with distilled water until the pH of an eluent is stable, drying and sieving to obtain pretreated lead plaster;
the invention removes the residual sulfuric acid electrolyte and impurities on the lead plaster by multiple times of water washing, and ensures that the particle sizes of the sulfuric acid electrolyte and impurities are consistent by sieving so as to eliminate the negative influence of the non-uniformity of the particle size;
s2, mixing the pretreated lead plaster with (NH) 4 ) 2 CO 3 The solution is mixed evenly and reacted, and distilled water is used for removing residual (NH) in the solid sediment after filtration 4 ) 2 CO 3 Adding acetic acid saturated solution into the reaction product after calcining, and adding H 2 O 2 Carrying out secondary reaction, and standing after the reaction is finished to obtain lead acetate crystals;
s3, mixing the lead acetate crystal with acetic acid to obtain a lead acetate-acetic acid solution, mixing the lead acetate-acetic acid solution with butyl titanate-ethanol solution, reacting under intense stirring to obtain yellowish sol, aging the sol to obtain a gel material, and crushing and calcining the gel to obtain the nano lead titanate.
Further, the pH of the eluent in the step S1 is 6.0-7.0. Preferably, the pH of the eluent in the step S1 is 6.5.
Further, the drying temperature in S1 is 100 ℃, and the drying time is 1h.
Further, the granularity of the pretreated lead plaster in the step S1 is 160 meshes.
Further, in the S2 (NH 4 ) 2 CO 3 The concentration of the solution is 45mg/mL, and the concentration of the lead plaster and (NH) 4 ) 2 CO 3 The weight ratio of the reagent is 2.2:1.
further, the reaction time in S2 is 0.5h.
Further, the calcination temperature in the step S2 is 500 ℃, and the calcination time is 24 hours.
Further, the molar ratio of acetic acid to Pb in the S2 is 1.5, H 2 O 2 With PbO 2 The molar ratio of (2).
Further, the secondary reaction temperature in S2 is 60 ℃, and the reaction time is 2h.
Further, the standing time in the step S2 is 24 hours.
Further, the concentration of lead acetate in the lead acetate-acetic acid solution in the step S3 is 1.0mol/L, and the concentration of butyl titanate in the butyl titanate-ethanol solution is 1.0mol/L.
Further, the molar ratio of titanium to lead in the mixed solution in the step S3 is 0.5-2:1-3. Preferably, the molar ratio of titanium to lead in the mixed solution in the step S3 is 1:1.
Further, the reaction temperature in the S3 is 60-100 ℃ and the reaction time is 2-3.5 h. Preferably, the reaction temperature in the step S3 is 80 ℃ and the reaction time is 2h.
Further, the ageing time in the step S3 is 10-18, the thickness of gel in the ageing process is less than 1cm, and the ageing temperature is 70 ℃. Preferably, the aging time in S3 is 18 hours.
Further, in the step S3, the calcination temperature is 400-600 ℃ and the calcination time is 3h. Preferably, in S3, the calcination temperature is 400 ℃.
Compared with the prior art, the invention has the beneficial technical effects that:
because the waste lead plaster contains a large amount of impuritiesAnd is soaked in H for a long time 2 SO 4 The electrolyte solution causes that the waste lead paste is used as the raw material, so that the nanoscale lead titanate product with uniform particle size is difficult to obtain, and the conversion rate is generally lower even if the nanoscale lead titanate product can be prepared.
The invention overcomes the problems by combining proper raw material pretreatment process with specific process steps and process parameters, realizes the efficient preparation of nano lead titanate, ensures the high conversion rate of lead titanate and realizes the environment-friendly recycling treatment of waste lead paste.
Drawings
The invention is further described with reference to the following description of the drawings.
FIG. 1 is a sample of a lead plaster obtained by disassembly and breaking of the present invention;
FIG. 2 is a view showing lead acetate crystals produced by the present invention;
FIG. 3 is a view showing lead titanate powder produced by the present invention;
FIG. 4 is an SEM image of the product of the present invention;
figure 5 is an XRD of the product of the invention.
Detailed Description
The technical scheme provided by the invention is further described below by combining with the embodiment.
Example 1
A method for recycling waste lead plaster comprises the following steps:
s1, manually disassembling and crushing a waste lead-acid battery produced by GS brand in Japan to obtain waste lead-acid paste with pH of 6.2, wherein the waste lead-acid paste has reddish brown appearance and powdery appearance, grinding the waste lead-acid paste into powder, washing the powder with distilled water until the pH of an eluent is 6.5, drying the powder at 100 ℃ for 1h, and sieving the powder with a 160-mesh sieve to obtain pretreated lead-acid paste;
s2, mixing 50g of pretreated lead plaster with 500mL of (NH with concentration of 45mg/mL 4 ) 2 CO 3 After mixing uniformly, reacting for 0.5h, filtering, washing with distilled water for many times, and removing unreacted (NH) 4 ) 2 CO 3 Calcining the reaction product at 500 ℃ for 24 hours, adding acetic acid saturated solution, and adding H 2 O 2 At 6Reacting for 2 hours at the temperature of 0 ℃, and standing for 24 hours after the reaction is finished to obtain lead acetate crystals; wherein the molar ratio of acetic acid to Pb is 1.5, H 2 O 2 With PbO 2 The molar ratio of (2);
s3, mixing the lead acetate crystal with 158mL of acetic acid solution with the concentration of 5wt% to obtain 1mol/L lead acetate-acetic acid solution, mixing the lead acetate-acetic acid solution with butyl titanate-ethanol solution to enable the mol ratio of titanium to lead in the mixed solution to be 1:1, heating in a water bath at 80 ℃ under strong stirring to react for 2 hours to obtain pale yellow sol, aging the sol at 70 ℃ for 18 hours to obtain a gel material, wherein the gel thickness is less than 1cm in the aging process, calcining at 400 ℃ for 3 hours after the gel is crushed, and sufficiently grinding powder to obtain nano lead titanate. The conversion of lead titanate is detected to be 95.4%.
Example 2
A method for recycling waste lead plaster comprises the following steps:
s1, manually disassembling and crushing a sail brand waste lead-acid battery to obtain waste lead-acid paste with the pH value of 4.3, wherein the waste lead-acid paste is reddish brown in appearance color and powdery in appearance shape, grinding the waste lead-acid paste into powder, washing the powder with distilled water until the pH value of an eluent is 6.5, drying the powder at 100 ℃ for 1h, and sieving the powder with a 160-mesh sieve to obtain pretreated lead-acid paste;
s2, mixing 50g of pretreated lead plaster with 500mL of (NH with concentration of 45mg/mL 4 ) 2 CO 3 After mixing uniformly, reacting for 0.5h, filtering, washing with distilled water for many times, and removing unreacted (NH) 4 ) 2 CO 3 Calcining the reaction product at 500 ℃ for 24 hours, adding acetic acid saturated solution, and adding H 2 O 2 Reacting for 2 hours at 60 ℃, and standing for 24 hours after the reaction is finished to obtain lead acetate crystals; wherein the molar ratio of acetic acid to Pb is 1.5, H 2 O 2 With PbO 2 The molar ratio of (2);
s3, mixing the lead acetate crystal with acetic acid to obtain a lead acetate-acetic acid solution, mixing the lead acetate-acetic acid solution with butyl titanate-ethanol solution to enable the molar ratio of titanium to lead in the mixed solution to be 1:1, heating in a water bath at 80 ℃ under strong stirring to react for 2 hours to obtain yellowish sol, aging the sol at 70 ℃ for 18 hours to obtain a gel material, wherein the gel thickness is less than 1cm in the aging process, calcining the gel at 400 ℃ for 3 hours after crushing, and sufficiently grinding the powder to obtain the nano lead titanate.
The conversion of lead titanate is detected to be 96.3 percent.
Comparative example 1
The difference from example 1 is that: desulfurizing agent (NH) in S2 4 ) 2 CO 3 The concentration of the solution was 30mg/mL. The detection shows that the conversion rate of lead acetate is 79.1% and the conversion rate of lead titanate is 75.50%.
Comparative example 2
The difference from example 1 is that: the molar ratio acetic acid/lead in S2 was 0.5. The detection shows that the conversion rate of lead acetate is 84.7% and the conversion rate of lead titanate is 81.07%.
Comparative example 3
The difference from example 1 is that: h in S2 2 O 2 /PbO 2 The molar ratio of (2) was 1. The detection shows that the conversion rate of lead acetate is 65.3% and the conversion rate of lead titanate is 65.37%.
Comparative example 4
The difference from example 1 is that: the molar ratio of titanium to lead in S3 is 0.5. The conversion of lead titanate was examined to be 75.99%.
Comparative example 5
The difference from example 1 is that: the water bath temperature in S3 is 60 ℃. The conversion of lead titanate was found to be 71.12%.
Comparative example 6
The difference from example 1 is that: the calcination temperature in S3 was 600 ℃. The conversion of lead titanate was found to be 21.6%.
Comparative example 7
The difference from example 2 is that: grinding the waste lead plaster into powder, and directly performing S2. The lead titanate conversion was tested to be 43.70%.
Test example 1
SEM scanning was performed on the nano lead titanate prepared in the examples and comparative examples, and the results are shown in fig. 4. Wherein FIGS. 4-1, 4-2, 4-3 are SEM images of lead titanate prepared in example 1 at various scales. Fig. 4-4 are SEM images of the crystals of the product prepared in example 2. FIGS. 4-5 and 4-6 are SEM images of crystals of the products prepared in comparative examples 4 and 5. It can be seen that the lead titanate prepared by the embodiment has uniform size and good dispersibility.
Test example 2
XRD analysis was performed on the nano lead titanate prepared in the examples and comparative examples, and the results are shown in fig. 5. Wherein fig. 1 and 2 are XRD patterns of the product crystals of example 1 and example 2, respectively, and fig. 3 is an XRD pattern of the lead titanate crystal prepared in comparative example 7. It can be seen that the crystals of examples 1 and 2 are substantially free of impurities, and comprise PbTiO as the main component 3 However, in comparative example 7, since the acid substance and other impurity elements are contained, pbTiO is the main component 3 However, the background value is complex, and the purity of the crystal is greatly reduced.
The lead titanate powder prepared under the conditions of example 1 is optimal relative to the comparative example, as shown in fig. 4-3 and 5-1, in which the lead titanate powder is prepared by a sol-gel method, and the lead titanate particle size is affected by factors such as the amount ratio of the lead titanate material, the concentration of the reactant, the reaction temperature, and the calcination temperature.
The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to assist in understanding the methods of the present invention and the core ideas thereof; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.
Claims (9)
1. The method for recycling the waste lead plaster is characterized by comprising the following steps of:
s1, grinding the lead plaster into powder, washing with distilled water until the pH of an eluent is stable, drying and sieving to obtain pretreated lead plaster;
s2, mixing the pretreated lead plaster with (NH) 4 ) 2 CO 3 Mixing uniformly, reacting, filtering to remove unreacted lead paste, calcining the reaction product, adding acetic acid saturated solution,then add H 2 O 2 Carrying out secondary reaction, and standing after the reaction is finished to obtain lead acetate crystals;
s3, mixing the lead acetate crystal with acetic acid to obtain a lead acetate-acetic acid solution, mixing the lead acetate-acetic acid solution with butyl titanate-ethanol solution, reacting under intense stirring to obtain yellowish sol, aging the sol to obtain a gel material, and crushing and calcining the gel to obtain the nano lead titanate.
2. The method for recycling waste lead plaster according to claim 1, wherein the pH of the eluent in S1 is 6.0-7.0.
3. The method for recycling waste lead plaster according to claim 1, wherein the drying temperature in the step S1 is 100 ℃ and the drying time is 1h.
4. The method for recycling waste lead plaster according to claim 1, wherein the calcination temperature in the step S2 is 500 ℃ and the calcination time is 24 hours.
5. The method for recycling waste lead plaster according to claim 1, wherein the secondary reaction temperature in the step S2 is 60 ℃ and the reaction time is 2h.
6. The method for recycling waste lead plaster according to claim 1, wherein the molar ratio of titanium to lead in the mixed solution in the step S3 is 0.5-2:1-3.
7. The method for recycling waste lead plaster according to claim 1, wherein the reaction temperature in the step S3 is 60-100 ℃ and the reaction time is 2-3.5 h.
8. The method for recycling waste lead plaster according to claim 1, wherein the aging time in the step S3 is 10-18, the gel thickness in the aging process is less than 1cm, and the aging temperature is 70 ℃.
9. The method for recycling waste lead plaster according to claim 1, wherein in the step S3, the calcination temperature is 400-600 ℃ and the calcination time is 3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311635599.1A CN117682553A (en) | 2023-12-01 | 2023-12-01 | Recycling treatment method for waste lead plaster |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311635599.1A CN117682553A (en) | 2023-12-01 | 2023-12-01 | Recycling treatment method for waste lead plaster |
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| Publication Number | Publication Date |
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| CN117682553A true CN117682553A (en) | 2024-03-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311635599.1A Pending CN117682553A (en) | 2023-12-01 | 2023-12-01 | Recycling treatment method for waste lead plaster |
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| CN (1) | CN117682553A (en) |
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- 2023-12-01 CN CN202311635599.1A patent/CN117682553A/en active Pending
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