CN115089999B - Application of composite extractant in recycling waste acid in waste aluminum chemical polishing solution - Google Patents
Application of composite extractant in recycling waste acid in waste aluminum chemical polishing solution Download PDFInfo
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- CN115089999B CN115089999B CN202210642558.4A CN202210642558A CN115089999B CN 115089999 B CN115089999 B CN 115089999B CN 202210642558 A CN202210642558 A CN 202210642558A CN 115089999 B CN115089999 B CN 115089999B
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- 239000002699 waste material Substances 0.000 title claims abstract description 115
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 88
- 238000005498 polishing Methods 0.000 title claims abstract description 83
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000000126 substance Substances 0.000 title claims abstract description 81
- 239000002131 composite material Substances 0.000 title claims abstract description 71
- 239000002253 acid Substances 0.000 title claims abstract description 36
- 238000004064 recycling Methods 0.000 title claims abstract description 23
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000012074 organic phase Substances 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 50
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 238000000605 extraction Methods 0.000 claims description 122
- 239000000243 solution Substances 0.000 claims description 67
- 229910019142 PO4 Inorganic materials 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 2
- -1 aluminum ions Chemical class 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 6
- 239000001257 hydrogen Substances 0.000 abstract description 6
- 229910014033 C-OH Inorganic materials 0.000 abstract description 3
- 229910014570 C—OH Inorganic materials 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000010815 organic waste Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 30
- 238000000926 separation method Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- 238000005192 partition Methods 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/02—Light metals
- C23F3/03—Light metals with acidic solutions
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses an application of a composite extractant in recycling waste acid in waste aluminum chemical polishing liquid. The composite extractant consists of tributyl phosphate and n-butyl alcohol, and the volume ratio of tributyl phosphate to n-butyl alcohol is (6-9): (1-4) when the catalyst is applied to the waste aluminum material chemical polishing solution, P=O in tributyl phosphate and C-OH in n-butyl alcohol can form hydrogen bonds with protons of waste acid in the waste aluminum material chemical polishing solution, so that waste acid molecules in the waste aluminum material chemical polishing solution are extracted into an organic phase, and waste acid is efficiently recovered; meanwhile, the volume ratio of tributyl phosphate to n-butyl alcohol is regulated, so that waste acid and impurity aluminum ions are effectively separated, and further the extracted and recovered waste acid can be recycled to use the aluminum chemical polishing solution.
Description
Technical Field
The invention relates to the technical field of extraction, in particular to application of a composite extractant to recycling waste acid in waste aluminum chemical polishing liquid.
Background
Aluminum and its alloys are used as an excellent metal material, and are widely used in modern society by virtue of their bright metallic luster and corrosion resistance. In daily necessities, aluminum and its alloys require surface finish to meet aesthetic or further corrosion protection requirements. In the use process, along with the consumption of hydrogen ions, the metal parts are gradually dissolved, the concentration of the metal ions in the chemical polishing solution is continuously increased, and further the polishing effect is gradually deteriorated, and the aluminum chemical polishing solution is invalid. Moreover, the aluminum chemical polishing solution contains high-concentration H 3PO4、H2SO4, al 3+ and the like, and is already listed in the national hazardous waste directory (HW 17) to seriously influence the ecological environment and cannot be directly discharged.
In order to avoid the influence of the waste aluminum material chemical polishing liquid on the ecological environment, the traditional treatment method is to treat the waste aluminum material chemical polishing liquid as waste, namely, alkaline substances or metal ions which can generate precipitation with waste acid are added, and the waste aluminum material chemical polishing liquid can be converted into relatively safe solid residues after solid-liquid separation, but the treatment method cannot realize the recovery of the waste acid in the waste aluminum material chemical polishing liquid.
In the prior art, an extraction method is often adopted to recycle waste acid in waste liquid, for example, the prior art discloses a recycling method of electroplating phosphoric acid waste liquid, tributyl phosphate is used as an extractant to extract and recycle phosphoric acid in the phosphoric acid waste liquid, and meanwhile, the iron content and the aluminum content in the phosphoric acid waste liquid are reduced; however, this treatment method is only aimed at separating and recovering a single phosphoric acid from aluminum, and cannot realize separation and recovery from Al 3+ when H 3PO4 and H 2SO4 exist simultaneously.
Disclosure of Invention
The invention aims to overcome the defect and the defect that the existing extractant is difficult to effectively separate high-concentration H 3PO4、H2SO4 from impurity Al 3+ in the aluminum alloy waste polishing solution, and provides an application of a composite extractant in recycling waste aluminum alloy chemical polishing solution, wherein the composite extractant consists of tributyl phosphate and n-butyl alcohol, and the volume ratio of tributyl phosphate to n-butyl alcohol is (6-9): (1-4) realizing recovery of high-concentration residual acid in the aluminum alloy waste polishing solution and simultaneously removing impurity aluminum ions.
Another object of the present invention is to provide an aluminum chemical polishing liquid.
The above object of the present invention is achieved by the following technical scheme:
the application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises tributyl phosphate and n-butyl alcohol, wherein the volume ratio of the tributyl phosphate to the n-butyl alcohol is (6-9): (1-4).
The composite extractant disclosed by the invention consists of tributyl phosphate and n-butyl alcohol, wherein P=O in tributyl phosphate can form a hydrogen bond with protons in H 3PO4 and H 2SO4, meanwhile, C-OH in n-butyl alcohol can also form a hydrogen bond with protons of H 3PO4 and H 2SO4, namely, the composite extractant extracts H 3PO4 and H 2SO4 in waste liquid into an organic phase through the hydrogen bond effect, and the existence of H 2SO4 can also inhibit dissociation of H 3PO4, so that the extraction effect of phosphoric acid is improved.
In addition, the composite extractant can effectively increase beta (H 3PO4/Al3+)、β(H2SO4/Al3+) simultaneously by adding n-butanol into tributyl phosphate, so that H 3PO4、H2SO4 and Al 3+ can be effectively separated. The solubility of the n-butyl alcohol in water is higher than that of tributyl phosphate in water, and the n-butyl alcohol dissolved in water brings impurity aluminum ions in the waste liquid into an organic phase, and in the back extraction process, H 3PO4 and H 2SO4 in the organic phase enter the aqueous phase, and the impurity aluminum ions enter the back extraction liquid along with H 3PO4 and H 2SO4. Therefore, when the content of n-butanol in the composite extractant is too high, the separation effect of H 3PO4 and H 2SO4 from impurity aluminum ions is deteriorated; when the content of n-butanol in the composite extractant is too low, the effects of extracting H 3PO4 and H 2SO4 of the composite extractant are too poor, and the waste acid is further influenced to be circularly applied to the aluminum chemical polishing solution.
Preferably, the volume ratio of tributyl phosphate to n-butanol is (6-7): (3-4).
In a specific embodiment, the application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
S1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device for fully mixing, and extracting and phase-separating to obtain a load organic phase and raffinate;
S2, adding the loaded organic phase and water in the S1 into an extraction device for fully mixing, and carrying out back extraction to obtain an organic phase and a back extraction liquid;
Wherein the strip liquor in S2 is a mixed solution of H 3PO4 and H 2SO4.
Preferably, the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution in the step S1 is (1-4): 1.
In the extraction process, along with the increase of the addition amount of the composite extractant, H 3PO4 and H 2SO4 in the waste aluminum material chemical polishing solution are easier to extract into an organic phase, so that the extraction rate of H 3PO4 and H 2SO4 is improved; however, when the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is more than 4:1, the extraction rates of H 3PO4 and H 2SO4 basically tend to be stable along with the increase of the addition amount of the composite extractant.
Preferably, the volume ratio of the loaded organic phase to water in S2 is (2-7): 1.
In the back extraction process, H 3PO4 and H 2SO4 in the loaded organic phase are back extracted to the water phase, and the purposes of enriching and concentrating H 3PO4 and H 2SO4 can be achieved by increasing the volume ratio of the loaded organic phase to water.
In a specific embodiment, the extraction temperature in the step S1 is 10-50 ℃, and the stripping temperature in the step S2 is 10-50 ℃.
In a specific embodiment, the waste aluminum material chemical polishing solution comprises H 3PO4、H2SO4 and Al 3+.
Specifically, the solubility of H 3PO4 in the waste aluminum material chemical polishing solution is 373.96-378.73 g/L, H 2SO4, the concentration is 246.67-268.56 g/L, al 3+ and the concentration is 24.54-25.95 g/L.
In a specific embodiment, the extraction stage number of the extraction in the step S1 is 1-8; and S2, the extraction stage number of the back extraction is 1-8.
The invention also protects an aluminum product chemical polishing solution prepared by taking the strip liquor as a raw material.
Compared with the prior art, the invention has the beneficial effects that:
the composite extractant consists of tributyl phosphate and n-butyl alcohol, and when the composite extractant is applied to the waste aluminum material chemical polishing solution, P=O in tributyl phosphate and C-OH in n-butyl alcohol can form hydrogen bonds with protons in waste acid in waste liquid, so that waste acid molecules in the waste aluminum material chemical polishing solution are extracted into an organic phase, waste acid is effectively recovered, the stripping rate of H 3PO4 reaches 94.5-95.6%, and the stripping rate of H 2SO4 reaches 91.11-92.38%; meanwhile, by regulating and controlling the volume ratio of tributyl phosphate to n-butanol, waste acid and impurity aluminum ions are effectively separated, beta (H 3PO4/Al3+) reaches 9.68-11.58, beta (H 2SO4/Al3+) reaches 4.81-5.86, and further the extracted and recovered waste acid can be recycled to use the aluminum chemical polishing solution.
Drawings
FIG. 1 is a schematic diagram of the application flow of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
The extraction rate, the back extraction rate, the separation coefficient and the distribution ratio of the invention are respectively determined by adopting the following formulas. Extraction rate: stripping rate: /(I) Distribution ratio: /(I)Separation coefficient: /(I)C 0 -the concentration of each component in the waste aluminum polishing solution and mol/L; v 0 -volume of waste aluminum polishing solution, L;
C aq -concentration of each component in raffinate, mol/L; v aq -raffinate volume, L;
C org -concentration of each component in the loaded organic phase, mol/L; v org -loaded organic phase volume, L;
C s -concentration of each component of the water phase after back extraction, mol/L; v s -volume of aqueous phase after stripping, L.
Example 1
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps (shown in figure 1):
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out primary extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 1:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out primary extraction, and separating phases to obtain an organic phase and a stripping liquid, wherein the volume ratio of the organic phase to the water phase is 1:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
the composite extractant consists of tributyl phosphate and n-butyl alcohol, wherein the volume ratio of the tributyl phosphate to the n-butyl alcohol is 9:1 respectively, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 373.96g/L,H2SO4 254.76g/L,Al3 + 24.90.90 g/L.
Example 2
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out primary extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 1:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out primary extraction, and separating phases to obtain an organic phase and a stripping liquid, wherein the volume ratio of the organic phase to the water phase is 1:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
the composite extractant consists of tributyl phosphate and n-butyl alcohol, wherein the volume ratio of the tributyl phosphate to the n-butyl alcohol is 8:2 respectively, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 373.96g/L,H2SO4 254.76g/L,Al3 + 24.90.90 g/L.
Example 3
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out primary extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 1:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out primary extraction, and separating phases to obtain an organic phase and a stripping liquid, wherein the volume ratio of the organic phase to the water phase is 1:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
The composite extractant consists of tributyl phosphate and n-butyl alcohol, wherein the volume ratio of the tributyl phosphate to the n-butyl alcohol is 7:3 respectively, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 373.96g/L,H2SO4 254.76g/L,Al3 + 24.90.90 g/L.
Example 4
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out primary extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 1:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out primary extraction, and separating phases to obtain an organic phase and a stripping liquid, wherein the volume ratio of the organic phase to the water phase is 1:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
The composite extractant consists of tributyl phosphate and n-butyl alcohol, wherein the volume ratio of the tributyl phosphate to the n-butyl alcohol is 6:4 respectively, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 373.96g/L,H2SO4 254.76g/L,Al3 + 24.90.90 g/L.
Example 5
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
S1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out 5-stage intermittent multistage countercurrent extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 2:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
s2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out 2-stage interstage multistage countercurrent extraction, and obtaining an organic phase and a stripping liquid after phase separation, wherein the volume ratio of the organic phase to the water phase is 2:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
the composite extractant consists of tributyl phosphate and n-butyl alcohol, the volume ratio of the tributyl phosphate to the n-butyl alcohol is 7:3, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 378.73g/L,H2SO4246.67g/L,Al3+ 25.95.95 g/L.
The above raffinate and strip extract were tested and the extraction and strip rates obtained are shown in Table 1.
TABLE 1
| Component (A) | H3PO4 | H2SO4 | Al3+ |
| Extraction rate | 70％-75％ | 52％-55％ | ＜10％ |
| Back extraction rate | 95.6％ | 92.38％ | / |
Example 6
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
S1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out 4-stage intermittent multistage countercurrent extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 4:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out 2-stage interstage multistage countercurrent extraction, and obtaining an organic phase and a stripping liquid after phase separation, wherein the volume ratio of the organic phase to the water phase is 5:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
wherein the composite extractant consists of tributyl phosphate and n-butyl alcohol, and the volume ratio of the tributyl phosphate to the n-butyl alcohol is 7:3; the main component content of the waste aluminum material chemical polishing solution is H 3PO4 377.48g/L,H2SO4260.56g/L,Al3+ 24.54.54 g/L.
The above raffinate and strip extract were tested and the extraction and strip rates obtained are shown in Table 2.
TABLE 2
| Component (A) | H3PO4 | H2SO4 | Al3+ |
| Extraction rate | 76％-79％ | 52％-55％ | ＜5％ |
| Back extraction rate | 94.5％ | 91.11％ | / |
Comparative example 1
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out primary extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 1:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out primary extraction, and separating phases to obtain an organic phase and a stripping liquid, wherein the volume ratio of the organic phase to the water phase is 1:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
The composite extractant consists of tributyl phosphate and n-butyl alcohol, wherein the volume ratio of the tributyl phosphate to the n-butyl alcohol is 9.8:0.2, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 373.96g/L,H2SO4 254.76g/L,Al3+ 24.90.90 g/L.
Comparative example 2
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out primary extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 1:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out primary extraction, and separating phases to obtain an organic phase and a stripping liquid, wherein the volume ratio of the organic phase to the water phase is 1:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
The composite extractant consists of tributyl phosphate and n-butyl alcohol, wherein the volume ratio of the tributyl phosphate to the n-butyl alcohol is 1:1, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 373.96g/L,H2SO4 254.76g/L,Al3+ 24.90.90 g/L.
Comparative example 3
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out primary extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 1:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out primary extraction, and separating phases to obtain an organic phase and a stripping liquid, wherein the volume ratio of the organic phase to the water phase is 1:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
the composite extractant consists of tributyl phosphate and n-octanol, wherein the volume ratio of the tributyl phosphate to the n-octanol is 9:1 respectively, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 373.96g/L,H2SO4 254.76g/L,Al3 + 24.90.90 g/L.
Comparative example 4
The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution comprises the following steps:
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device, fully mixing, carrying out primary extraction, and separating phases to obtain a loaded organic phase and a raffinate, wherein the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is 1:1, the extraction temperature is 30 ℃, and the extraction time is 10min;
S2, adding the loaded organic phase and water in the S1 into an extraction device for full mixing, carrying out primary extraction, and separating phases to obtain an organic phase and a stripping liquid, wherein the volume ratio of the organic phase to the water phase is 1:1, the back extraction temperature is 30 ℃, and the back extraction time is 10min;
The composite extractant consists of tributyl phosphate and methyl isobutyl ketone, wherein the volume ratio of the tributyl phosphate to the methyl isobutyl ketone is 9:1, and the main component content of the waste aluminum material chemical polishing solution is H 3PO4 373.96g/L,H2SO4254.76g/L,Al3+ 24.90.90 g/L.
TABLE 3 separation coefficient (. Beta.) and partition ratio (D) of the respective components in examples 1 to 4 and comparative examples 1 to 4
| Numbering device | β(H3PO4/Al3+) | β(H2SO4/Al3+) | D(H3PO4) | D(H2SO4) | D(Al3+) |
| Example 1 | 9.81 | 5.17 | 0.3603 | 0.1898 | 0.0367 |
| Example 2 | 9.68 | 4.81 | 0.3697 | 0.1838 | 0.0382 |
| Example 3 | 11.58 | 5.86 | 0.3598 | 0.1820 | 0.0311 |
| Example 4 | 10.64 | 5.04 | 0.3854 | 0.1826 | 0.0362 |
| Comparative example 1 | 7.71 | 4.06 | 0.3598 | 0.1895 | 0.0467 |
| Comparative example 2 | 9.07 | 5.36 | 0.3441 | 0.2036 | 0.0380 |
| Comparative example 3 | 8.13 | 4.26 | 0.3175 | 0.1662 | 0.0391 |
| Comparative example 4 | 9.35 | 4.26 | 0.3307 | 0.1506 | 0.0354 |
The partition ratio (D) is the ratio of the total concentration of the extracted substances in the organic phase to the total concentration in the aqueous phase after the extraction system reaches equilibrium, and the higher the partition ratio of phosphoric acid to sulfuric acid is, the stronger the acid extraction capability of the extractant is. The separation coefficient (beta) is the ratio of the distribution ratio of the two substances in the extraction process, and the greater the separation coefficient, namely the higher the separation degree, the more thoroughly the H 3PO4 or H 2SO4 is separated from the Al 3+. Comprehensively considering the partition ratio and the separation coefficient, selecting a composite extractant to be composed of tributyl phosphate and n-butyl alcohol, wherein the volume ratio of tributyl phosphate to n-butyl alcohol is not (6-9): in the case of (1-4), the extraction and separation effects are optimal.
The above examples of the present invention are merely illustrative of the present invention and are not intended to limit the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (4)
1. The application of the composite extractant in recycling waste acid in the waste aluminum chemical polishing solution is characterized by comprising the following steps:
s1, adding a composite extractant and a waste aluminum material chemical polishing solution into an extraction device for fully mixing, and extracting and phase-separating to obtain a load organic phase and raffinate; the volume ratio of the composite extractant to the waste aluminum material chemical polishing solution is (1-4) 1;
S2, adding the loaded organic phase and water in the S1 into an extraction device for fully mixing, and carrying out back extraction to obtain an organic phase and a back extraction liquid; wherein the strip liquor in S2 is a mixed solution of H 3PO4 and H 2SO4;
the composite extractant consists of tributyl phosphate and n-butyl alcohol, wherein the volume ratio of the tributyl phosphate to the n-butyl alcohol is (6-7): (3-4);
The concentration of H 3PO4、H2SO4 and Al 3+,H3PO4 in the waste aluminum material chemical polishing solution is 373.96-378.73 g/L, H 2SO4, the concentration of 246.67-268.56 g/L, al 3+ and the concentration of 24.54-25.95 g/L.
2. The use of the composite extractant for recycling waste acid in chemical polishing liquid of waste aluminum materials as claimed in claim 1, wherein the volume ratio of the loaded organic phase to water in S2 is (2-7): 1.
3. The use of the composite extractant for recycling waste acid in chemical polishing liquid of waste aluminum materials as claimed in claim 1, wherein the temperature of the extraction in S1 is 10-50 ℃, and the temperature of the back extraction in S2 is 10-50 ℃.
4. The application of the composite extractant in recycling waste aluminum product chemical polishing liquid as claimed in claim 1, wherein the extraction stage number of the extraction in S1 is 1-8; and S2, the extraction stage number of the back extraction is 1-8.
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