CN115043474B - Application of potassium titanium oxalate in removing heavy metals in water - Google Patents
Application of potassium titanium oxalate in removing heavy metals in water Download PDFInfo
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- CN115043474B CN115043474B CN202210605593.9A CN202210605593A CN115043474B CN 115043474 B CN115043474 B CN 115043474B CN 202210605593 A CN202210605593 A CN 202210605593A CN 115043474 B CN115043474 B CN 115043474B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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Abstract
The invention discloses application of potassium titanium oxalate in removing heavy metals in water. The inventor discovers that the titanium potassium oxalate can be rapidly hydrolyzed in natural calcium-containing water, amorphous hydrous titanium oxide with strong adsorption capacity and calcium oxalate crystals which can co-precipitate with heavy metals are generated, the aim of jointly removing various heavy metals is fulfilled by the synergistic effect of the hydrous titanium oxide and the calcium oxalate crystals, and the defect that the existing medicament is single in heavy metal removal type is overcome.
Description
Technical Field
The invention belongs to the field of water pollution treatment, and particularly relates to application of potassium titanium oxalate in removing heavy metals in water.
Background
Heavy metals are of great social interest because of their non-biodegradability, high toxicity, bioaccumulation. Because of industrial development, drinking water in China is threatened by various heavy metal pollution, representative heavy metals comprise cadmium (Cd), lead (Pb), mercury (Hg) and hexavalent chromium (Cr (VI)), arsenic (mainly arsenate ions (As (V)) and arsenite (As (III)), and the standard of the heavy metal indexes of drinking water and sewage discharge is not only related to environmental protection, but also related to the health of people, and is a necessary thing.
The prior art can meet most heavy metal removal requirements without considering cost. For example, ion exchange, membrane separation, adsorption and other technologies can realize high-efficiency removal of heavy metals from water, but the running cost is high for removal of trace heavy metals, so that the application of the technology in daily drinking water treatment technology is less. The coagulation method has simple operation and low cost, and has wide application in the process of removing heavy metals from drinking water and sewage. At present, widely used coagulants mainly comprise ferric salt and aluminum salt, and the coagulants mainly aim at removing turbidity and have poor treatment effect on drinking water with excessive heavy metals. For example, iron and aluminum salts have high removal rates for As (V) anions, but poor removal rates for uncharged As (III), positively charged Cd, pb, hg. The development of a novel coagulant for removing heavy metals is an economic and effective scheme for solving the problems of trace heavy metal pollution of drinking water, excessive heavy metal emission of sewage and the like.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provides application of potassium titanium oxalate in removing heavy metals in water.
The aim of the invention is achieved by the following technical scheme: the application of the titanium potassium oxalate in removing heavy metals in water is based on the discovery by the inventor that the titanium potassium oxalate can be rapidly hydrolyzed in natural calcium-containing water, amorphous hydrous titanium oxide with strong adsorption capacity and calcium oxalate crystals which can co-precipitate with heavy metals are generated, and the aim of removing various heavy metals together is fulfilled through the synergistic effect of the hydrous titanium oxide and the calcium oxalate crystals.
The application of the potassium titanium oxalate in removing heavy metals in water comprises the following steps: adding the potassium titanium oxalate into the water body to perform a coagulation reaction, and obtaining the water body with heavy metal removed after the sediment generated by the coagulation reaction is settled.
The water includes drinking water, industrial waste water and domestic sewage.
The pH of the water is preferably 4-9; more preferably 4 to 7.5.
The heavy metals include As, cd, cr, pb, hg and Cu.
The As includes As (III) and As (V).
The Cr is preferably Cr (VI).
The addition amount of the potassium titanium oxalate is preferably 2-20 mg-Ti/L calculated by titanium.
The potassium titanium oxalate is preferably added into the water body in the form of potassium titanium oxalate solution.
The concentration of the potassium titanium oxalate solution is preferably 1-9% by mass; more preferably 8% by mass.
The time of the coagulation reaction is preferably 5-30 min; more preferably 10min.
The principle of the invention is as follows: the main industrial application of the potassium titanium oxalate is as tanning agent, mordant, metal surface treating agent, analytical reagent and the like, and the potassium titanium oxalate has not been applied in the fields of drinking water, domestic sewage and industrial wastewater. According to a great number of scientific experiments, the invention discovers that the potassium titanium oxalate can be rapidly hydrolyzed in natural calcium-containing water body to generate strongAmorphous hydrous titanium oxide with adsorption capacity and calcium oxalate crystals which can co-precipitate with heavy metals realize the aim of removing various heavy metals together through the synergistic effect of the hydrous titanium oxide and the calcium oxalate crystals. Potassium titanium oxalate is effective for treating anionic heavy metals (X) m- ) For example, cr (VI), as (V), as (III) and the like, and single heavy metals such As Cd, pb, hg and the like and a plurality of heavy metal mixtures thereof have high-efficiency removal capability. The basic principle is shown in chemical reactions (1) - (4). The potassium titanium oxalate hydrolyzes to produce hydrous titanium oxide and calcium oxalate. The hydrated titanium oxide is rich in titanium hydroxyl groups, can form coordination bonds with various heavy metals, and is removed in a coordination adsorption mode. The hydrous titanium oxide colloid has a great amount of negative charges, and can enrich multivalent cation type heavy metals through classical adsorption. In addition, no matter groundwater, river water or lake water contains more natural calcium and magnesium ions (natural hardness), and oxalate ions react with natural calcium and magnesium to generate indissolvable oxalate. In the process, the cationic heavy metal can enter calcium oxalate crystal lattice through coprecipitation and other modes, so that the aim of removing trace heavy metal is fulfilled.
K 2 TiO(C 2 O 4 ) 2 +2H 2 O+2Ca 2+ →TiO(OH) 2 +2CaC 2 O 4 +2K + +2H + (1)；
TiO(OH) 2 +X m- →TiO(OH) 2 (X m- ) Coordination adsorption (2)；
[TiO(OH) 2 ] z- +Y n+ →[TiO(OH) 2 ](Y n+ ) Electrostatic adsorption (3)；
The invention creatively uses the industrial tanning agent, namely the titanium potassium oxalate, as a novel water treatment coagulant for removing various heavy metals, provides a novel water treatment medicament for efficiently removing various heavy metals in water, guaranteeing the safety of drinking water and reducing heavy metal pollution, and belongs to the innovative application of the titanium potassium oxalate.
Compared with the prior art, the invention has the following advantages and effects:
by adopting the titanium potassium oxalate As the coagulant, the coordination adsorption heavy metal performance of the hydrated titanium oxide and the coprecipitation heavy metal removal performance of the calcium oxalate can be comprehensively utilized, and one or more of the heavy metals such As Cd, pb and Hg with positive charges, cr (VI) and As (V) with negative charges and the uncharged As (III) can be simultaneously removed from various water bodies, so that the defect of single heavy metal removal type of the traditional medicament is overcome.
Drawings
FIG. 1 is a graph of the effect of potassium titanyl oxalate dose on As and Cd removal from drinking water.
FIG. 2 is an X-ray diffraction pattern diagram of the removal of As and Cd flocs by the coagulation of potassium titanium oxalate.
FIG. 3 is a scanning electron micrograph of the potassium titanium oxalate coagulated to remove As and Cd flocs and an element distribution diagram.
FIG. 4 is an X-ray photoelectron spectroscopy analysis of the removal of As and Cd flocs by coagulation of potassium titanium oxalate.
FIG. 5 is a graph showing the results of potassium titanyl oxalate in comparison with conventional coagulant iron sulfate and aluminum sulfate in removing As and Cd from drinking water.
FIG. 6 is a graph showing the effect of potassium titanium oxalate on the pH of a water body compared with that of conventional coagulant iron sulfate and aluminum sulfate.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
As (III) and As (V) are measured by adopting an atomic fluorescence spectrometry according to the national industry standard HY/T152-2013; the total As and Hg are measured by adopting an atomic fluorescence spectrometry according to the national standard GB/T33086-2016; cd. Pb, cr and Cu were measured by inductively coupled plasma mass spectrometry (ICP-MS).
EXAMPLE 1 Potassium titanium oxalate for deep removal of As and Cd from drinking Water
Some tap water source water 100L contains As (III) 100 mug/L, cd mug/L, hardness 160mg/L, pH7. An aqueous solution of potassium titanium oxalate having a mass concentration of 8% (wherein K 2 TiO(C 2 O 4 ) 2 The using amount is 6 mg-Ti/L) is taken As a coagulant, the coagulant is added into As/Cd polluted source water, the adding amount is 6mg-Ti/L (calculated by titanium), the coagulation time is 10 minutes, natural sedimentation is carried out for 1 hour, a large amount of white sediment is seen to sink into the water bottom, supernatant liquid is taken As treated water, and the As (III) content of the water is 7.2 mug/L, cd 4.3.3 mug/L, the hardness is 126mg/L, the pH is 6.9, and the water quality reaches the national drinking water quality standard (GB 5749-2006). FIG. 1 shows that the effect of removing Cd and As by the coagulation of the potassium titanium oxalate is good, and the concentration of Cd/As in the effluent can be reduced by more than 90% within 10 minutes, so that the effluent reaches the drinking water standard.
The white precipitate dried at 110℃for 24 hours was taken and examined by an X-ray diffractometer, and the results are shown in FIG. 2. FIG. 2 shows that the flocs formed by the coagulation of potassium titanium oxalate are predominantly amorphous hydrous titanium oxide and calcium oxalate crystals with small amounts of hydrous calcium oxalate (calcium oxalate hydrate) present.
The white precipitate dried at 110℃for 24 hours was examined by a scanning electron microscope, and the results are shown in FIG. 3. FIG. 3 shows that most of the hydrated titanium oxide and calcium oxalate crystals are uniformly mixed into larger flocs, which is beneficial to gravity sedimentation or simple filtration to realize mud-water separation.
The white precipitate dried at 110℃for 24 hours was analyzed by X-ray photoelectron spectroscopy, and the results are shown in FIG. 4. FIG. 4 shows that there are more As and Cd in the potassium titanium oxalate coagulated flocs, where As exists in the form of As (III), indicating that there is no significant redox reaction during flocculation and that the valence state remains stable during heavy metal removal.
The tap water source water is treated by ferric sulfate and aluminum sulfate respectively, and the treatment steps are the same as those of the potassium titanium oxalate, and only the ferric sulfate and the aluminum sulfate are used for replacing the potassium titanium oxalate respectively. For comparison, the coagulant addition amounts are expressed in terms of iron/aluminum/titanium molar concentrations ranging from 0 to 120. Mu. Mol/L. At the end of the experiment, the resulting supernatants were tested for As (V), as (III), cd and pH, respectively, and the results are shown in FIGS. 5 and 6. Fig. 5 shows that potassium titanyl oxalate is superior to conventional coagulants, ferric sulfate and aluminum sulfate in removing uncharged trivalent arsenic and cadmium from drinking water. Fig. 6 shows that compared with ferric sulfate and aluminum sulfate, the influence of potassium titanium oxalate on tap water pH is smaller, because oxalic acid generated by hydrolysis of potassium titanium oxalate is weak acid, and sulfuric acid which is a byproduct of hydrolysis of other reagents is strong acid, the pH of water body can be rapidly reduced, and the process of adjusting pH needs to be additionally increased, which is unfavorable for simplifying operation and reducing cost.
EXAMPLE 2 Potassium titanium oxalate for deep removal of Cr (VI) and Cd in drinking Water
Some tap water source water 100L contains 500 mug/L, cd mug/L Cr (VI), 380mg/L hardness and pH 7.1. Adding an aqueous solution of potassium titanium oxalate with the mass concentration of 8% into Cr (VI)/Cd polluted water source water, wherein the adding amount is 13mg-Ti/L (calculated by titanium), the coagulation time is 10 minutes, natural sedimentation is carried out for 1 hour, a large amount of white sediment can be seen to sink into the water bottom, supernatant liquid is taken as treated water, and the obtained water contains 37.2 mug/L, cd 3.5.5 mug/L of Cr (VI), the hardness is 326mg/L, the pH value is 6.8, and the water quality reaches the national drinking water quality standard.
EXAMPLE 3 Potassium titanium oxalate for deep removal of As, cr and Cd from drinking Water
Some tap water source water 100L contains Cr (VI) 500 mug/L, total As 100 mug/L, cd mug/L, hardness 285mg/L and pH 7.0. Adding an aqueous solution of potassium titanium oxalate with the mass concentration of 8% into water of a Cr (VI)/As/Cd polluted water source, wherein the addition amount is 15mg-Ti/L (calculated by titanium), the coagulation time is 10 minutes, the solution is naturally settled for 1 hour, a large amount of white precipitate can be seen to sink into the water bottom, supernatant liquid is taken As treated water, and the obtained water contains 42.2 mug/L, as 6.8.8 mug/L, cd 3.9.9 mug/L of Cr (VI), has the hardness of 228mg/L and the pH of 6.7, and the water quality reaches the national drinking water quality standard.
EXAMPLE 4 Potassium titanium oxalate for deep removal of As, cr, cd and Pb in drinking Water
Some tap water source water 100L contains Cr (VI) 500 mug/L, total As 100 mug/L, cd mug/L and Pb 100 mug/L, hardness 450mg/L and pH 7.4. Adding 8% by mass of potassium titanium oxalate aqueous solution serving As a coagulant into Cr (VI)/As/Cd/Pb polluted source water, wherein the addition amount is 10mg-Ti/L (calculated by titanium), the coagulation time is 10 minutes, the solution is naturally settled for 1 hour, a large amount of white precipitate can be seen to sink into the water bottom, supernatant liquid is taken As treated water, and the obtained water contains 21.0 mug/L, as 6.6.6 mug/L, cd 2.5.5 mug/L, pb 2.5.5 mug/L of Cr (VI), 402mg/L of hardness and 6.8 of pH, and the water quality reaches the national drinking water quality standard.
EXAMPLE 5 Potassium titanium oxalate for deep drinking Water removal As, cr, cd, pb and Hg
Some tap water source water 100L contains 500 mug/L Cr (VI), 100 mug/L, cd mug/L, pb mug/L total As, 10 mug/L Hg, 370mg/L hardness, pH7.2. Adding an aqueous solution of potassium titanium oxalate with the mass concentration of 8% into water of a Cr (VI)/As/Cd/Pb polluted water source, wherein the addition amount is 20mg-Ti/L (calculated by titanium), the coagulation time is 10 minutes, the solution is naturally settled for 1 hour, a large amount of white precipitate can be seen to sink into the water, supernatant liquid is taken As treated water, and the obtained water contains 15.0 mug/L, as 2.6.6 mug/L, cd 0.8.8 mug/L of Cr (VI), 1.7 mug/L of Pb, the hardness is 291mg/L, the pH is 6.8, and the water quality reaches the national drinking water quality standard.
EXAMPLE 6 use of Potassium titanium oxalate for deep Industrial wastewater removal As, cr, cd, pb and Cu
100L of industrial wastewater contains 530 mug/L of Cr (VI), 25 mug/L, cd mug/L, pb mug/3552 mug/L, cu 1.6.6 mg/L of total As and 88mg-O of COD 2 L, pH 4.1. Adding 8% by mass of aqueous solution of potassium titanium oxalate As coagulant into Cr (VI)/As/Cd/Pb polluted source water, wherein the addition amount is 20mg-Ti/L (calculated by titanium), the coagulation time is 10 minutes, natural sedimentation is carried out for 1 hour, a large amount of gray precipitate can be seen to sink into the water, the pH of effluent is regulated to be 6.7 by adding 20% sodium hydroxide solution, supernatant is taken As treated effluent, and the content of Cr (VI) in the effluent is measured to be 13 mug/L, as 0.5 mug/L, cd 2.2.2 mug/L, pb 8.4.4 mug/L, cu 0.337mg/L, COD 32mg-O 2 and/L, pH6.8, and the water quality reaches the national first-class A standard of domestic sewage discharge (GB 8978-1996).
EXAMPLE 7 application of Potassium titanium oxalate to advanced removal of As, cd, pb in domestic Sewage
100L of effluent water from a municipal sewage plant contains 16 mug/L, cd mug/L, pb mug/L of total As, 208mg/L of hardness and 38mg-O of COD 2 L, pH 6.8. Adding 8% by mass of aqueous solution of potassium titanium oxalate into As/Cd/Pb standard-exceeding domestic sewage, adding 2mg-Ti/L (calculated As titanium), coagulating for 10min, naturally settling for 1 hr, allowing a small amount of gray precipitate to sink into the water bottom, collecting supernatant As treated water, and measuring As content of 7.6 μg/L, cd 3.8.8 μg/LPb 5.7 mug/L, hardness 198mg/L, COD 28mg-O 2 and/L, pH6.7, and the water quality reaches the national first-class A standard of domestic sewage discharge (GB 8978-1996).
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (5)
1. The application of the potassium titanium oxalate in removing heavy metals in water is characterized by comprising the following steps: adding an aqueous solution of potassium titanium oxalate with the mass concentration of 8% into a calcium-containing water body for coagulation reaction, wherein the coagulated flocs mainly comprise amorphous hydrated titanium oxide and calcium oxalate crystals, and a small amount of hydrated calcium oxalate is present; obtaining a water body for removing heavy metals after precipitation generated by the coagulation reaction is settled;
the pH of the water is 4.1-9;
the adding amount of the potassium titanium oxalate is 2-20 mg-Ti/L calculated by titanium;
the heavy metals include As, cd, cr, pb, hg and Cu.
2. The use of potassium titanium oxalate for removing heavy metals from water according to claim 1, wherein: the water includes drinking water, industrial waste water and domestic sewage.
3. The use of potassium titanium oxalate for removing heavy metals from water according to claim 1, wherein: the pH of the water is 4.1-7.5.
4. The use of potassium titanium oxalate for removing heavy metals from water according to claim 1, wherein:
the As comprises As (III) and As (V);
cr is Cr (VI).
5. The use of potassium titanium oxalate for removing heavy metals from water according to claim 1, wherein: the coagulation reaction time is 5-30 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10290986A (en) * | 1997-04-18 | 1998-11-04 | Toyobo Co Ltd | Treatment of antimony-containing waste water |
| JP2002249471A (en) * | 2000-12-19 | 2002-09-06 | Sanyo Chem Ind Ltd | Production method of ester |
| CN110282779A (en) * | 2019-07-05 | 2019-09-27 | 南京中微纳米功能材料研究院有限公司 | A kind of heavy metal-polluted water treatment technology |
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| US7491335B2 (en) * | 2005-05-13 | 2009-02-17 | The Board Of Regents Of The University Of Texas System | Removal of arsenic from water with oxidized metal coated pumice |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10290986A (en) * | 1997-04-18 | 1998-11-04 | Toyobo Co Ltd | Treatment of antimony-containing waste water |
| JP2002249471A (en) * | 2000-12-19 | 2002-09-06 | Sanyo Chem Ind Ltd | Production method of ester |
| CN110282779A (en) * | 2019-07-05 | 2019-09-27 | 南京中微纳米功能材料研究院有限公司 | A kind of heavy metal-polluted water treatment technology |
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