CN109455748A - A method of recycling aluminum nitrate from waste acid liquor - Google Patents
A method of recycling aluminum nitrate from waste acid liquor Download PDFInfo
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- CN109455748A CN109455748A CN201811543879.9A CN201811543879A CN109455748A CN 109455748 A CN109455748 A CN 109455748A CN 201811543879 A CN201811543879 A CN 201811543879A CN 109455748 A CN109455748 A CN 109455748A
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- Prior art keywords
- nitric acid
- aluminium
- solution
- added
- acid
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- 239000002253 acid Substances 0.000 title claims abstract description 59
- 239000002699 waste material Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 40
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 title claims abstract description 34
- 238000004064 recycling Methods 0.000 title claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 65
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 58
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 42
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000004411 aluminium Substances 0.000 claims abstract description 34
- 230000001376 precipitating effect Effects 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000013049 sediment Substances 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 12
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- 239000006166 lysate Substances 0.000 claims abstract description 4
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000013078 crystal Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 5
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 238000013517 stratification Methods 0.000 claims description 4
- GTTYPHLDORACJW-UHFFFAOYSA-N nitric acid;sodium Chemical compound [Na].O[N+]([O-])=O GTTYPHLDORACJW-UHFFFAOYSA-N 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- 235000010210 aluminium Nutrition 0.000 abstract description 46
- 229910052751 metal Inorganic materials 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 10
- 239000000047 product Substances 0.000 abstract description 8
- 239000002351 wastewater Substances 0.000 abstract description 7
- 239000005030 aluminium foil Substances 0.000 abstract description 4
- 238000000866 electrolytic etching Methods 0.000 abstract description 4
- 230000003628 erosive effect Effects 0.000 abstract description 4
- 239000012776 electronic material Substances 0.000 abstract description 2
- 235000021110 pickles Nutrition 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 76
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 52
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 25
- 239000004317 sodium nitrate Substances 0.000 description 25
- 235000010344 sodium nitrate Nutrition 0.000 description 25
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 21
- 235000011121 sodium hydroxide Nutrition 0.000 description 20
- 239000000203 mixture Substances 0.000 description 19
- 229910001388 sodium aluminate Inorganic materials 0.000 description 19
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 18
- 239000006227 byproduct Substances 0.000 description 17
- 239000007788 liquid Substances 0.000 description 16
- 239000012528 membrane Substances 0.000 description 16
- 238000001556 precipitation Methods 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 13
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 12
- 239000011734 sodium Substances 0.000 description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 238000007127 saponification reaction Methods 0.000 description 10
- 229910052708 sodium Inorganic materials 0.000 description 10
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical class [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000011259 mixed solution Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000428 dust Substances 0.000 description 8
- 238000009292 forward osmosis Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 6
- 239000011888 foil Substances 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- -1 aluminum ions Chemical class 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229940037003 alum Drugs 0.000 description 2
- 229960005363 aluminium oxide Drugs 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001679 gibbsite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910000474 mercury oxide Inorganic materials 0.000 description 1
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000000802 nitrating effect Effects 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000405 sodium aluminium phosphate Inorganic materials 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/66—Nitrates, with or without other cations besides aluminium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/04—Preparation with liquid nitric acid
-
- 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
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/445—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by forward osmosis
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Agronomy & Crop Science (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The method that the present invention provides a kind of to recycle aluminum nitrate from waste acid liquor, comprising the following steps: 1) sodium hydroxide stirring a period of time is added into waste acid liquor containing aluminium；2) nitric acid is added, pH value is adjusted to 6-7, generates precipitating；3) supernatant and lower sediment are obtained after filtering the substance that step 2) obtains, addition nitric acid dissolution in lower sediment；4) lysate in step 3) after condensing crystallizing to get.This method handles waste water and the valuable chemical products of recycling by being specifically applied to the combination of inorganic chemistry and physical chemistry relevant knowledge in the acid pickle of electronic material aluminium foil.The Aluminums such as corrode for other aluminium electroloysis and aluminium, while also providing Technical Reference for industries such as other electrolytic etching of metal and metal erosion.
Description
Technical field
The present invention relates to chemical fields, and in particular to a method of aluminum nitrate is recycled from waste acid liquor.
Background technique
Acid aluminum-cleaning wastewater refers mainly to refer to the waste acid water that electric aluminum foil generates in burn into acid cleaning process.In order to remove
Micro impurity is such as in aluminium foil: copper, iron metal, using nitric acid oxidation and handles its surface area, while to generate a large amount of useless
Acid solution.In fact, a considerable amount of aluminium salts are contained in this kind of " spent acid ".Such as untreated any discharge, not only corrode downcomer
Road, powerhouse foundation, it is in line also to will cause water pollution.The waste liquid of waste nitric acid containing aluminium is mainly derived from pickling oxidation section, is ring
Protect the important indicator of department's strict control total nitrogen, ammonia nitrogen in border.
In the corrosion process of electric aluminum foil, corrosive liquid is mainly configured by nitric acid by a certain percentage, in certain temperature
Under degree and current condition, aluminium foil is corroded, then becomes the semi-finished product (etched foil) of Waste Acid From Hua Cheng Foil through nitric acid solution reaming, by change
At obtaining electrode foil (Waste Acid From Hua Cheng Foil).Corrosion and reaming process have very high requirement to corrosive liquid each component, it is therefore desirable to constantly add
Add new liquid, the acid solution overflowed just becomes waste acid liquor.This waste acid liquor contain be corroded out from aluminium foil it is big
Aluminium ion is measured, needs further to be recycled.
In view of this, the present invention is specifically proposed.
Summary of the invention
The method that the purpose of the present invention is to provide a kind of to recycle aluminum nitrate from waste acid liquor, by handling waste acid liquor
And recycling wherein valuable chemical products, obtain the aluminum nitrate crystal of high-purity, at the same output as byproduct sodium nitrate and
Pure water provides Technical Reference for the Aluminums such as aluminium electroloysis and aluminium corrosion and the industries such as other electrolytic etching of metal and metal erosion.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
The method that the present invention provides a kind of to recycle aluminum nitrate from waste acid liquor, comprising the following steps:
1) sodium hydroxide stirring a period of time is added into waste acid liquor containing aluminium；
2) nitric acid is added, pH value is adjusted to 6-7, generates precipitating；
3) supernatant and lower sediment are obtained after filtering the substance that step 2) obtains, addition nitric acid is molten in lower sediment
Solution；
4) lysate in step 3) after condensing crystallizing to get.
Further, as a kind of enforceable scheme, in step 1), speed of agitator 80-120rad/min, stirring
Time controls between 30-60min.
Further, as a kind of enforceable scheme, in step 1), reaction temperature is 60-90 DEG C.
Further, as a kind of enforceable scheme, in step 2), reaction temperature is increased to addition at 90 DEG C or more
Nitric acid.
Further, as a kind of enforceable scheme, in step 2), the concentration that nitric acid is added is 1-3mol/L.
Further, as a kind of enforceable scheme, in step 2), the compounding substances generated after precipitating are continued to stir
The rear stratification of 10min or more is mixed, time of repose is no less than 20min.
Further, as a kind of enforceable scheme, in step 2), nitric acid is added dropwise into the clarified solution after standing,
Until occurring without precipitating.
Further, nitric acid is added in lower sediment in step 3) as a kind of enforceable scheme, until heavy
Shallow lake is completely dissolved.
It further, as a kind of enforceable scheme, further include adding water into the solution after being completely dissolved in step 3)
Dilution, filtering.
Further, obtained filtrate is stirred continuously in step 4) as a kind of enforceable scheme, it is cooling, make nitre
Sour sodium crystal is precipitated, filter to get.
The characteristics of present invention is according to the waste liquid of waste nitric acid containing aluminium, the recycling to aluminum nitrate mainly includes four steps: 1) using
Aluminium ion in sodium hydroxide and waste acid liquor carries out saponification and generates tetrahydroxy conjunction sodium aluminate；2) by closing aluminium in tetrahydroxy
A small amount of nitric acid is added in acid sodium solution, aluminium ion is discharged from mixed solution in the form of aluminum hydroxide precipitation, the step
Notice that certain added nitric acid cannot be excessive, adds its pH after nitric acid to maintain between 6-7, more preferably between 6.2-6.5, most
It excellently is 6.3, practice discovery control precipitates more complete within the scope of this pH；3) nitric acid is added in aluminum hydroxide precipitation,
The molten reaction of acid is carried out, aluminum nitrate solution, condensing crystallizing recycling are generated；4) byproduct sodium nitrate is handled using forward osmosis membrane method, together
When obtain pure water.The method of nitric acid alum recovery is taken and is not destroyed based on nitrate anion, it is whole that nitrate anion is transferred to byproduct
In sodium nitrate, to reach nine Heshui aluminum nitrates of recycling high quality and the production purpose of by-product sodium nitrate.
This method is by being specifically applied to electronic material aluminium for the combination of inorganic chemistry and physical chemistry relevant knowledge
In the acid pickle of foil, waste water and the valuable chemical products of recycling are handled.The Aluminums such as corrode for other aluminium electroloysis and aluminium, while being also it
The industries such as its electrolytic etching of metal and metal erosion provide Technical Reference.
Compared with the prior art, the advantages of the present invention are as follows:
1) aluminium ion removal rate is up to 99.5% in waste water, and primary recovery is up to 70%；
2) byproduct sodium nitrate is prepared using the processing of forward osmosis membrane method, while obtains pure water, reach waste acid liquor containing aluminium
Environmentally protective, environmental-friendly is effectively treated.
3) Determination of Total Nitrogen in Waste Water is controlled, the concentration of ammonia nitrogen is not exceeded, reaches whole effective wastewater treatment.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
The process flow diagram of the method for aluminum nitrate is recycled in the slave waste acid liquor that Fig. 1 provides for the embodiment of the present invention 1.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation,
It is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
The method that the present invention provides a kind of to recycle aluminum nitrate from waste acid liquor, comprising the following steps:
1) sodium hydroxide stirring a period of time is added into waste acid liquor containing aluminium；
2) nitric acid is added, pH value is adjusted to 6-7, generates precipitating；
3) supernatant and lower sediment are obtained after filtering the substance that step 2) obtains, addition nitric acid is molten in lower sediment
Solution；
4) lysate in step 3) after condensing crystallizing to get.
The characteristics of present invention is according to the waste liquid of waste nitric acid containing aluminium, the recycling to aluminum nitrate mainly includes four steps: 1) using
Aluminium ion in sodium hydroxide and waste acid liquor carries out saponification and generates tetrahydroxy conjunction sodium aluminate；2) by closing aluminium in tetrahydroxy
A small amount of nitric acid is added in acid sodium solution, and aluminium ion is discharged from mixed solution in the form of aluminum hydroxide precipitation；3) in hydrogen
Nitric acid is added in precipitation of alumina, carries out the molten reaction of acid, generates aluminum nitrate solution, condensing crystallizing recycling；4) forward osmosis membrane is used
Method handles byproduct sodium nitrate, while obtaining pure water.
Aluminum nitrate is white clear crystal as a kind of important chemical products, there is a hygroscopy, soluble easily in water and ethyl alcohol,
It is atomic to be dissolved in acetone, it is practically insoluble in ethyl acetate and pyridine.Aqueous solution reacts acid, and 73 DEG C of fusing point (decomposes) at 135 DEG C,
It is oxidizing, cause to burn with organic matter friction or impact energy.
It is mainly used in the production of kinescope, is also used for manufacture nature electric lamp filament, mordant.Meanwhile aluminum nitrate is also dividing
It plays an important role on analysis reagent, the extraction of uranium, nitrating agent, corrosion inhibitor and petroleum refinement catalyst.
During the preparation process, the production principle taken predominantly passes through aluminium or aluminium hydroxide and nitric acid reaction, generates nitric acid
Aluminium is detailed in following formulas:
A1+4HNO3→Al(NO3)3+NO+2H2O
A1(OH)3+3H NO3→Al(NO3)3+3H2O
In traditional industrial production, the technique mainly used is as follows:
Metal aluminum sheet is cleaned with 10% soda bath after removing surface and oil contaminant, then rinsed with tap water, is then placed in anti-
It answers in device, a small amount of (2kg is about added in every 100kg aluminium flake) mercury oxide is added as oxidant, then be slowly added into dust technology (concentration is about
38%), reaction process makes aluminium keep excessive, so that reaction temperature is maintained at 110~115 DEG C with steam heating, about after 2h, reaction
It finishes.Clarified, filtering, clear liquid is sent to evaporator to be evaporated under reduced pressure, is put into natural cooling crystallization in crystallizer, taking-up is smashed to pieces
Afterwards, it is dehydrated with centrifuge, without drying, direct barrelling is as finished product.
Mother liquor send evaporator to be recycled, ability venting when iron content in finished product or unqualified content of beary metal.Reaction
When the nitrogen dioxide gas released, by-product NaNO can be obtained by being pumped into lye Chi Zhongyong Alkali absorption through vacuum3Or NaNO2。
In the present invention, by handling the waste acid liquor containing aluminium generated in the production of electric aluminum foil, after treatment
Under the premise of waste water meets total nitrogen, ammonia-nitrogen content requirement, can aluminium ion effectively in waste acid recovery solution, converting it into has
The aluminum nitrate of economic value, in the form of nine Heshui aluminum nitrates of high quality recycle, and during processing by-product sodium nitrate and
Pure water.While making to there is the waste acid liquor of very big destroying infection to be effectively addressed environment, one kind is also opened up and has not destroyed
Nitrate anion in solution, by its global transfer and in conjunction with aluminium ion in solution produce aluminum nitrate preparation new process.
In specific production, saponification is carried out using the aluminium ion in sodium hydroxide and waste acid liquor first and generates tetrahydroxy
Sodium aluminate is closed, tetrahydroxy closes sodium aluminate and is although commonly called as sodium metaaluminate, but its basic structure is a kind of complex.Saponification
Reaction carries out under stiring, speed of agitator 80-120rad/min, and mixing time controls between 30-60min.Preferably, it stirs
Mixing revolving speed is 100rad/min, mixing time 45min.It is 60-90 DEG C, preferably 80 DEG C that the step, which is in reaction temperature, simultaneously
Under the conditions of carry out.The saponification that stirring can be such that the aluminium ion in the sodium hydroxide and waste acid liquor that are added occurs more is filled
Point, in this step, the sodium hydroxide of addition be it is excessive, aluminium ion under the action of hydroxyl, first production aluminium hydroxide
Precipitating, then aluminium hydroxide dissolves after reacting with excessive sodium hydroxide, generates sodium metaaluminate, and sodium metaaluminate is dissolved in aqueous solution
In practical composition i.e. transform into tetrahydroxy close sodium aluminate.Intermediate product tetrahydroxy close sodium aluminate can make the aluminium in solution from
Son is totally converted, it is therefore intended that improves the aluminum ions rate of recovery in waste acid liquor.Further, in the revolving speed of 100rad/min
Under, it can guarantee that aluminium ion reacts more abundant with sodium hydroxide, help to improve the aluminum ions rate of recovery, can more make to mix
It closes solution and constitutes metastable uniform state.In the present invention, on the one hand the reaction temperature for improving saponification can effectively improve
On the other hand reaction rate promotes temperature and is more advantageous to the ionization of water, it is well known that water power from rear generation hydroxyl and hydrogen from
Son, and hydroxyl then has an effect with aluminium ion and generates precipitating, aluminum hydroxide precipitation alkali soluble under sodium hydroxide effect, hydrogen ion
Then neutralized with excessive sodium hydroxide.Aluminium ion is finally improved by combined reaction above-mentioned in solution to be changed into the solution
Tetrahydroxy closes the conversion ratio of sodium aluminate, has been ensured to the greatest extent to effective recycling aluminum ions in waste acid liquor.
It is actually two kinds of compounds that sodium metaaluminate and tetrahydroxy, which close sodium aluminate, has different the Nomenclature Composition and Structure of Complexes.
NaAlO2It is the ingredient being present in solid crystals, is substantially considered as ionic crystals, i.e., by the tightly packed shape of zwitterion
At compound.Aluminium oxide, which is dissolved in the caustic soda of melting, can be obtained the substance.Na[Al(OH)4] it is to come across in aqueous solution
Ingredient, that is, metallic aluminium is dissolved in the true composition of product obtained in NaOH by we.
In acid condition, tetrahydroxy closes sodium aluminate and can react with a small amount of acid, generates aluminum hydroxide precipitation and phase
Answer the sodium salt of acid group；But if the excessive acid being added, acidolysis reaction can occur to precipitating, generate corresponding acid ion
Aluminium salt and sodium salt.In the present invention, tetrahydroxy closes sodium aluminate and a small amount of nitric acid reaction, generates aluminum hydroxide precipitation and nitric acid
Sodium.Corresponding reaction equation is as follows:
Na[Al(OH)4]+HNO3(a small amount of) → Al (OH)3↓+NaNO3+H2O
Above-mentioned reaction is solution under conditions of close to boiling, is in solution specifically by being stirred continuously progress
Temperature when being increased to 90 DEG C or more, then closed in sodium aluminate solution to tetrahydroxy and add nitric acid.The raised purpose of temperature also helps
It is sufficiently discharged in tetrahydroxy is closed the aluminium component in sodium aluminate, is converted into aluminum hydroxide precipitation, while after temperature raising, Neng Gouzeng
The big solubility of sodium nitrate in water；In the above description, it is indicated that the raising of temperature facilitates the ionization of water, comprehensively considers,
Improving reaction temperature can promote reaction towards positive direction progress, and tetrahydroxy is effectively ensured and closes sodium aluminate to the greatest extent to aluminum ions
Release, is fully converted into aluminum hydroxide precipitation, reduces the impurity content in subsequent byproduct sodium nitrate.In this step, it adds
The concentration of nitric acid is 1-3mol/L, and preferred concentration is the nitric acid of 2mol/L.It is generally acknowledged that the nitric acid that concentration is 14mol/L or more is
Concentrated nitric acid, as pointed out in above-mentioned reaction mechanism, need to be added a small amount of nitric acid in this step, the dust technology for adding 2mol/L has
Help prevent that nitric acid is excessive to be happened to reaction preferably control.
According in process flow, as the pH=6.3 of solution, aluminium ion precipitating is complete, C [Al in solution3+]=1.3 ×
10-12mol/L；Under usual conditions, Ksp [Al (OH)3]=1.3 × 10-33.Then in alkali soluble, (i.e. step 1 generates tetrahydroxy and closes aluminic acid
Sodium) pH=7 that adjusts solution afterwards, it is added solution tune pH=6.3 after nitric acid.Such purpose is to guarantee that aluminium ion has precipitated
Entirely, it is calculated according to dissolution and the solubility product formula of sedimentation equilibrium；
Then think that the aluminium ion precipitating in solution is complete.Certainly, the solution after precipitating also is needed to carry out further
Detection, usually by the mixture of pH=6.3 continue stir 10min after stratification, stand be no less than 20min after mixture
It is layered as supernatant liquid and lower sediment.Part clarified solution is taken out, nitric acid is added dropwise into clarified solution, if not precipitating production
It is raw, then illustrate fully reacting, carries out subsequent filter and realize separation of solid and liquid；But if there are also precipitatings to generate, need further
Nitric acid is added, until occurring without precipitating.Such purpose also for greatest extent to the aluminium in waste acid liquor from
Son is recycled, and the rate of recovery is improved.
After determining that aluminium ion is fully converted to aluminum hydroxide precipitation, mixture is filtered, obtain supernatant and under
Layer precipitating adds the molten reaction of acid that nitric acid carries out aluminium hydroxide into lower sediment.Reaction equation is as follows:
Al(OH)3+3HNO3→Al(NO3)3+3H2O
It after being completely dissolved precipitating, is diluted with water, filtering filters out insoluble matter, improves the recycling quality of aluminum nitrate.At this
In step, the molten reaction of acid that nitric acid carries out aluminium hydroxide is added into precipitating, precipitating can be made to complete to be converted into aluminum nitrate, and
Form the solution of certain nitric acid aluminium content.Certainly, solution temperature is also in a higher level at this time, and aluminum nitrate is in the solution
Solubility it is higher, also ensure that the yield of aluminum nitrate from another angle.
By filtered aluminum nitrate solution under conditions of being stirred continuously cooling down, make aluminum nitrate crystal in the solution by
It is gradually precipitated, after being fully cooled, the mixed liquor containing aluminum nitrate crystal is filtered, drains, obtains nine Heshui nitric acid of high quality
Aluminium crystal.It needs to be noted that also storage has the undecomposed aluminum nitrate component in part in solution after aluminum nitrate crystal is precipitated,
The aluminum nitrate solution that the part needs further to produce recycles output, to guarantee the recycling quality of nine Heshui aluminum nitrate crystal.
Containing sodium nitrate as by-product in supernatant after filtering aluminum hydroxide precipitation, by forward osmosis membrane technology into
The recycling of row byproduct sodium nitrate, positive infiltration are the membrane process of concentration drive type, it relies on the infiltration of permoselective membrane two sides
Pressure difference is transmitting of the spontaneous realization water of driving force in film.Placing two kinds respectively in the two sides with permselectivity membrane has not
It is a kind of for the material liquid compared with Hyposmolality with the solution of osmotic pressure, another kind for the driving solution compared with hyperosmosis,
The permeable pressure head that positive infiltration exactly applies film two sides solution just allows the water to spontaneously saturating from material liquid side as driving force
It crosses permoselective membrane and reaches driving liquid-side.It is positive to permeate compared to pressure-actuated membrane separating process such as micro-filtration, hyperfiltration technique
Membrane process has low pressure or without series of advantages such as press operation, low energy consumption and low fouling membranes.In the present invention, it is seeped by using positive
Permeable membrane finally obtains sodium nitrate and pure water.
Need to stress has, and the present invention, which takes the method for nitric acid alum recovery, not to be destroyed based on nitrate anion, and entirety will
Nitrate anion is transferred in byproduct sodium nitrate, to reach the production of the nine Heshui aluminum nitrates and by-product sodium nitrate of recycling high quality
Purpose.Byproduct sodium nitrate is prepared by using forward osmosis membrane method processing, while obtaining pure water, realizes waste acid liquor containing aluminium
Environmentally protective, environmental-friendly treatment effect makes also to bring certain economy while Determination of Total Nitrogen in Waste Water, ammonia-nitrogen content are up to standard
Benefit, is the Aluminums such as other aluminium electroloysis and aluminium corrosion, and the industries such as other electrolytic etching of metal and metal erosion provide Technical Reference.
The technical solution in the present invention is further illustrated in the form of specific embodiment below:
Embodiment 1
A certain amount of waste acid liquor containing aluminium is heated to 60 DEG C, in the case where revolving speed is the stirring condition of 80rad/min with uniform
Amount addition sodium hydroxide solution, adjusts pH value=7 of mixed solution, makes aluminium ion and sodium hydroxide in waste acid liquor that soap occur
Change reaction, mixing time 30min sufficiently generates tetrahydroxy after reaction and closes sodium aluminate.It is persistently stirred after saponification, and right
Mixed solution heating adds the dust technology that concentration is 1mol/L into solution, adjusts mixture when temperature is increased to 90 DEG C
PH value=6 make tetrahydroxy close sodium aluminate and are fully converted into aluminum hydroxide precipitation.It has added dust technology to continue after stirring 10min, stop
It only stirs to mixture stratification.Mixture is divided into supernatant liquid and lower sediment after standing 20min, takes out part and clarifies
Liquid, is added dropwise whether nitric acid detection aluminium hydroxide precipitates completely into clarified solution.But it if there are also precipitatings to generate, needs into one
It walks and adds nitric acid into mixture, until occurring in the clarified solution after standing without precipitating.Then mixture was carried out
Filter, obtained filtrate is filtered by forward osmosis membrane technology, obtains sodium nitrate solution and pure water, continuous to sodium nitrate solution
Stirring, cooling, are precipitated nitric acid sodium crystal, and suction filtration obtains byproduct sodium nitrate；It is molten that nitric acid is added in obtained aluminium hydroxide
Liquid is diluted with water until precipitating is completely dissolved into the solution after being completely dissolved, filtering removal impurity, and the nitric acid that will be obtained
Aluminum solutions crystallisation by cooling, is obtained by filtration nine Heshui aluminum nitrate crystal, and specific embodiment is as shown in Figure 1.
Embodiment 2
A certain amount of waste acid liquor containing aluminium is heated to 90 DEG C, in the case where revolving speed is the stirring condition of 120rad/min with uniform
Amount addition sodium hydroxide solution, adjusts pH value=6 of mixed solution, makes aluminium ion and sodium hydroxide in waste acid liquor that soap occur
Change reaction, mixing time 60min sufficiently generates tetrahydroxy after reaction and closes sodium aluminate.It is persistently stirred after saponification, and right
Mixed solution heating adds the dust technology that concentration is 3mol/L into solution, tetrahydroxy is made to close aluminium when temperature is increased to 95 DEG C
Sour sodium is fully converted into aluminum hydroxide precipitation.It has added dust technology to continue after stirring 15min, has stopped stirring to mixture standing point
Layer.Mixture is divided into supernatant liquid and lower sediment after standing 30min, takes out part clarified solution, nitre is added dropwise into clarified solution
Whether acid detection aluminium hydroxide precipitates completely.But it if there are also precipitatings to generate, needs further to add nitre into mixture
Acid, until stand after clarified solution in without precipitating occur until.Then mixture is filtered, obtained filtrate is passed through
Forward osmosis membrane technology is filtered, and obtains sodium nitrate solution and pure water, is stirred continuously, is cooled down to sodium nitrate solution, makes sodium nitrate
Crystal is precipitated, and suction filtration obtains byproduct sodium nitrate；Nitric acid solution is added in obtained aluminium hydroxide, until precipitating is completely molten
Solution, is diluted with water into the solution after being completely dissolved, filtering removal impurity, and the aluminum nitrate solution crystallisation by cooling that will be obtained, mistake
Filter obtains nine Heshui aluminum nitrate crystal.
Embodiment 3
A certain amount of waste acid liquor containing aluminium is heated to 80 DEG C, in the case where revolving speed is the stirring condition of 100rad/min with uniform
Amount addition sodium hydroxide solution, adjusts pH value=6.5 of mixed solution, and aluminium ion and sodium hydroxide in waste acid liquor occurs
Saponification, mixing time 40min sufficiently generate tetrahydroxy after reaction and close sodium aluminate.It is persistently stirred after saponification, and
Mixed solution is heated, when temperature is increased to 93 DEG C, the dust technology that concentration is 2mol/L is added into solution, closes tetrahydroxy
Sodium aluminate is fully converted into aluminum hydroxide precipitation.It has added dust technology to continue after stirring 20min, has stopped stirring and mixture is stood
Layering.Mixture is divided into supernatant liquid and lower sediment after standing 25min, takes out part clarified solution, is added dropwise into clarified solution
Whether nitric acid detection aluminium hydroxide precipitates completely.But it if there are also precipitatings to generate, needs further to add into mixture
Nitric acid, until stand after clarified solution in without precipitating occur until.Then mixture is filtered, it is logical to obtained filtrate
It crosses forward osmosis membrane technology to be filtered, obtains sodium nitrate solution and pure water, sodium nitrate solution is stirred continuously, is cooled down, nitric acid is made
Sodium crystal is precipitated, and suction filtration obtains byproduct sodium nitrate；Nitric acid solution is added in obtained aluminium hydroxide, until precipitating is completely molten
Solution, is diluted with water into the solution after being completely dissolved, filtering removal impurity, and the aluminum nitrate solution crystallisation by cooling that will be obtained, mistake
Filter obtains nine Heshui aluminum nitrate crystal.
Experimental example 1
Using the concrete technology method of embodiment 3, the pH value of mixed solution is controlled according to following table difference group different
In numberical range, the precipitation status of solution is tested, specific test result is as follows:
From the result of above-mentioned experimental example as can be seen that when adding nitric acid, the amount for adding nitric acid is between needs and pH
Be mutually adapted, add nitric acid amount is too big or the too small effect that can all influence actual process, if the step does not have
It controls, also will affect continuing for follow-up test.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, but those skilled in the art should understand that: its
It is still possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features
It is equivalently replaced；And these are modified or replaceed, various embodiments of the present invention skill that it does not separate the essence of the corresponding technical solution
The range of art scheme.
Claims (10)
1. a kind of method for recycling aluminum nitrate from waste acid liquor, comprising the following steps:
1) sodium hydroxide stirring a period of time is added into waste acid liquor containing aluminium；
2) nitric acid is added, pH value is adjusted to 6-7, generates precipitating；
3) supernatant and lower sediment are obtained after filtering the substance that step 2) obtains, addition nitric acid dissolution in lower sediment；
4) lysate in step 3) after condensing crystallizing to get.
2. the method according to claim 1, wherein in step 1), speed of agitator 80-120rad/min,
Mixing time controls between 30-60min.
3. according to the method described in claim 2, it is characterized in that, reaction temperature is 60-90 DEG C in step 1).
4. the method according to claim 1, wherein in step 2), when reaction temperature is increased to 90 DEG C or more
Add nitric acid.
5. according to the method described in claim 4, it is characterized in that, the concentration that nitric acid is added is 1-3mol/L in step 2).
6. according to the method described in claim 4, it is characterized in that, in step 2), compounding substances after precipitating will be generated after
Stratification after continuous stirring 10min or more, time of repose are no less than 20min.
7. according to the method described in claim 4, it is characterized in that, nitre is added dropwise into the clarified solution after standing in step 2)
Acid, until occurring without precipitating.
8. the method according to claim 1, wherein nitric acid is added in lower sediment in step 3), until
Precipitating is completely dissolved.
9. according to the method described in claim 8, it is characterized in that, further including in step 3), to the solution after being completely dissolved
In be diluted with water, filter.
10. cold according to the method described in claim 9, it is characterized in that, be stirred continuously obtained filtrate in step 4)
But, make nitric acid sodium crystal be precipitated, filter to get.
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| CN114314912A (en) * | 2021-12-23 | 2022-04-12 | 茂名鲁华新材料有限公司 | Method for treating carbon five resin wastewater |
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