CN111675278A - Method for directly treating hexavalent chromium-containing wastewater by using clay raw ore - Google Patents
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- Treatment Of Water By Oxidation Or Reduction (AREA)
- Removal Of Specific Substances (AREA)
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Abstract
The invention provides a method for directly treating hexavalent chromium-containing wastewater by using clay raw ore, and relates to the technical field of sewage purification. The invention comprises the following steps: adding the powder of the clay raw ore into the wastewater containing hexavalent chromium to obtain a mixed solution; adjusting the pH value of the mixed solution to 2-6; heating the mixed solution to ensure that the temperature of the mixed solution is 30-45 ℃; fully stirring for 30-36h, and standing to obtain a mixed solution of solid slag and regenerated water; the solid slag and the regenerated water are separated, and the raw clay ore adopted by the invention contains pyrite, transition metal oxides and other components, and also has a reduction effect on hexavalent chromium in the wastewater. The removal efficiency of the chromium ions is high, and the obtained chromium ions are easily separated from the clay minerals. The applicable range of pH value in the removing process is wide.
Description
Technical Field
The invention relates to the technical field of sewage purification, in particular to a method for directly treating hexavalent chromium-containing wastewater by using clay raw ore.
Background
Chromium is an important metal resource and is widely applied to industries such as tanning, electroplating, mining, chemical engineering, metallurgy and the like. However, the treatment of the waste water containing chromium is difficult due to the large amount of waste water generated in the production process, and particularly, the problem of environmental pollution caused by the toxicity of the waste water is widely worried by people, particularly, the physiological toxicity of hexavalent chromium is 100 times that of trivalent chromium, and the hexavalent chromium belongs to carcinogenic, teratogenic and mutagenic highly toxic substances and is extremely harmful, so the hexavalent chromium is a key concern for environmental management. From the viewpoint of environmental chemistry, chromium exists in various forms, but in actual production wastewater, chromium mainly appears in trivalent chromium form and hexavalent chromium form, and chromium in the two forms is converted along with the change of the environment.
At present, the main methods for treating the chromium-containing wastewater comprise an ion exchange method, an adsorption method, an electrolysis method, a chemical precipitation method and the like; wherein the anion exchange method can be used to exchange CrO4 2-、HCrO4 -Directly exchange, remove and enrich to obtain high-concentration chromium salt, realize recycling; however, in the actual operation process, the repeated adsorption performance of the resin or the adsorption material is often seriously deteriorated due to the complex and various components in the wastewater, so the precondition for being successfully applied in the actual situation is very strict. The adsorption method mainly uses an adsorption material such as activated carbon, and the like, and has high preparation cost and difficulty in effective solid-liquid separation. The electrolysis method is difficult to popularize and apply due to the reasons of large energy consumption, low treatment efficiency and the like. The chemical precipitation method mainly adopts a reducing agent to reduce Cr (VI) and then adds an alkaline substance to remove the precipitate, and has the defects that the pH value of the solution needs to be adjusted, and the medicament cost is high. The methods have certain limitations, so that the development of a new material and a new method for treating the chromium-containing wastewater, which have the advantages of low cost, simple operation, high efficiency and easy separation, is necessary.
Chinese patent CN104310666A discloses a method for restoring heavy metal chromium in underground water, belonging to the field of sewage treatment. Firstly, introducing chromium-containing wastewater into a micro-electrolysis region (2) synthesized by copper (7) and zinc (8) materials for micro-electrolysis; then, the chromium-containing wastewater is introduced into a concentration zone (3) through a water passage I (13), one part of the wastewater is blocked by a water-blocking baffle (10), and the other part of the wastewater loses water under the action of a semipermeable membrane (9), so that the internal chromium is concentrated; after being concentrated, the mixture enters a precipitation zone (4) through a water passage II (14), sulfide is added into the mixture, and the mixture is stirred by a stirrer (11); then enters an ion exchange area (5) through a water passage III (15), and the water is purified by utilizing the exchange adsorption effect of the resin (12) on chromate plasma and the like in the water, and finally is discharged through a water outlet (6). The concentration of the original wastewater of the device is about 114mg/L, the concentration of the chromium-containing wastewater treated by the device is 0.15mg/L, the removal rate reaches 99.87%, and the device is proved to be capable of well purifying the underground water. The purification method used in the application realizes the purification of chromium ions through the membrane permeation and adsorption of a semipermeable membrane, has poor purification speed, has high requirements on pH value, and has a narrow suitable range of pH value.
The chromium ion purification speed in the prior art is slow, and the efficiency of solid-liquid separation treatment is not high.
Disclosure of Invention
In view of the above, the present invention provides a method for directly treating wastewater containing hexavalent chromium by using clay raw ore, wherein the clay raw ore adopted in the method contains pyrite, transition metal oxides and other components, and has a reduction effect on hexavalent chromium in the wastewater. The removal efficiency of the chromium ions is high, and the obtained chromium ions are easily separated from the clay minerals. The applicable range of pH value in the removing process is wide.
A method for directly treating hexavalent chromium-containing wastewater by using clay raw ore comprises the following steps:
adding the powder of the clay raw ore into the wastewater containing hexavalent chromium to obtain a mixed solution; adjusting the pH value of the mixed solution to 2-6; heating the mixed solution to ensure that the temperature of the mixed solution is 30-45 ℃; fully stirring for 30-36h at the stirring speed of 200-260rpm, and standing to obtain a mixed solution of solid slag and regenerated water; separating solid slag and regenerated water; and dropwise adding 3-5M alkali liquor into the solid slag, stirring and soaking for 1-2h for desorption, separating chromium ions adsorbed on clay mineral sites from the clay minerals to realize desorption, dropwise adding 3-5M acid liquor, stirring and soaking for 1-2h, and performing activation and regeneration on the clay raw ores.
The addition amount of the clay raw ore is 3-5g/L, and the clay raw ore is any one or more of montmorillonite, bentonite, rectorite, kaolin, illite, halloysite, palygorskite, sepiolite, attapulgite, vermiculite, chlorite and pyrite.
Wherein, the effective components in the clay raw ore comprise: fe2O3、TiO2、FeS2、Na2O、MnO、ZnO、CuO、Ag2O。
In addition, the particle size of the clay raw ore is 5-15 μm, and the clay raw ore comprises montmorillonite, bentonite, rectorite, kaolin, palygorskite, sepiolite, attapulgite and vermiculite.
The clay raw ore comprises, by weight, 2-4 parts of montmorillonite, 1.5-3 parts of bentonite, 5-7 parts of rectorite, 3-5 parts of kaolin, 1-2 parts of palygorskite, 1.3-2.6 parts of sepiolite, 4.5-6.3 parts of attapulgite and 1-2 parts of vermiculite. The clay raw ore comprises 4 parts of montmorillonite, 3 parts of bentonite, 7 parts of rectorite, 5 parts of kaolin, 2 parts of palygorskite, 2.6 parts of sepiolite, 6.3 parts of attapulgite and 2 parts of vermiculite in parts by weight.
The invention achieves the aim of removing hexavalent chromium ions by directly or indirectly carrying out contact reaction on the clay raw ore and the hexavalent chromium ions. The principle comprises the following two processes:
1. direct adsorption removal: 1) in the process of forming the clay mineral, isomorphous substitution often occurs in a tetrahedron or octahedron structure of the clay mineral, so that charge imbalance occurs, oxygen atoms are exposed on a fracture surface of the clay mineral due to crystal breakage, and permanent negative charges are carried on the crystal surface of the clay mineral due to the characteristics, so that hexavalent chromium ions are attracted, and coordination can be generated to combine and achieve the purpose of removing. 2) Inorganic cations capable of being exchanged freely are contained among clay mineral structures, and part of cations can be exchanged with hexavalent chromium ions in the solution, so that the aim of adsorbing and removing the chromium ions is fulfilled. 3) Most clay minerals have huge specific surface area and interlayer space, and are beneficial to the absorption of hexavalent chromium ions.
2. Reduction-adsorption removal: compared with a simple clay mineral, a raw clay mineral often contains a plurality of associated minerals including iron minerals, rare metal minerals and the like. Hexavalent chromium ions have strong oxidizing property, and are reduced to trivalent chromium ions when contacting reduced substances in the clay raw ore, and can be directly adsorbed.
Compared with the pure clay mineral, the clay raw ore disclosed by the invention has a better removal effect in a wider pH range when used for treating hexavalent chromium, and the reason is mainly that the clay raw ore has associated metal minerals. Generally, the structural unit layers of clay minerals are generally charged and are divided into two forms of structural charge (permanent charge) and surface charge (variable charge), and when adsorption of hexavalent chromium is carried out, the adsorption mainly comes from electrostatic adsorption caused by the structural charge. The structural charge is derived from the excess negative charge generated by isomorphous substitution and lattice defects in the clay mineral lattice, the amount of which is generally not affected by the pH of the environment. When absorbing hexavalent chromium, the clay mineral mainly depends on two forms of electrostatic adsorption and interlayer cation exchange, and the specific pH application range is related to the structure of the clay mineral.
Compared with the pure clay minerals, the clay raw ore used by the invention also contains reductive metal minerals, and reductive components in the metal minerals are easy to react with hexavalent chromium, so that the hexavalent chromium is reduced into trivalent chromium or forms a complex with the hexavalent chromium, and the aim of removing the hexavalent chromium is fulfilled. And the process is not terminated by a change in pH. Therefore, the reducing components in the clay raw ore used by the invention broadens the pH application range when absorbing hexavalent chromium.
The raw clay ore used in the invention is a mixed mineral, and the different components of the mixed mineral have different principles for removing hexavalent chromium. For example, clay minerals have an adsorption effect and an interlayer cation exchange effect on hexavalent chromium, and reducing metal minerals also have a reduction effect and a complexing effect on hexavalent chromium. The treatment effect of the combination on hexavalent chromium is far higher than that of a single component.
The raw clay ore adopted by the invention contains components such as pyrite, transition metal oxide and the like, and has a reduction effect on hexavalent chromium in wastewater. The removal efficiency of the chromium ions is high, and the obtained chromium ions are easily separated from the clay minerals. The applicable range of pH value in the removing process is wide.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
Example 1
A method for directly treating hexavalent chromium-containing wastewater by using clay raw ore comprises the following steps:
adding the powder of the clay raw ore into the wastewater containing hexavalent chromium to obtain a mixed solution; adjusting the pH value of the mixed solution to 2; heating the mixed solution to ensure that the temperature of the mixed solution is 30 ℃; fully stirring for 30 hours at the stirring speed of 200rpm, and standing to obtain a mixed solution of solid slag and reclaimed water; separating solid slag and regenerated water; and dropwise adding 3M alkali liquor into the solid slag, stirring and soaking for 1h for desorption, separating chromium ions adsorbed on clay mineral sites from the clay minerals to realize desorption, dropwise adding 3M acid liquor, stirring and soaking for 1h, and performing activation and regeneration on the clay raw ores.
The addition amount of the clay raw ore is 3g/L, and the clay raw ore is any one or more of montmorillonite, bentonite, rectorite, kaolin, illite, halloysite, palygorskite, sepiolite, attapulgite, vermiculite, chlorite and pyrite.
Wherein, the effective components in the clay raw ore comprise: fe2O3、TiO2、FeS2、Na2O、MnO、ZnO、CuO、Ag2O。
In addition, the particle size of the clay raw ore is 5 μm, and the clay raw ore comprises montmorillonite, bentonite, rectorite, kaolin, palygorskite, sepiolite, attapulgite and vermiculite. The clay raw ore comprises 4 parts of montmorillonite, 3 parts of bentonite, 7 parts of rectorite, 5 parts of kaolin, 2 parts of palygorskite, 2.6 parts of sepiolite, 6.3 parts of attapulgite and 2 parts of vermiculite in parts by weight.
Example 2
A method for directly treating hexavalent chromium-containing wastewater by using clay raw ore comprises the following steps:
adding the powder of the clay raw ore into the wastewater containing hexavalent chromium to obtain a mixed solution; adjusting the pH value of the mixed solution to 6; heating the mixed solution to enable the temperature of the mixed solution to be 45 ℃; fully stirring for 36 hours at the stirring speed of 260rpm, and standing to obtain a mixed solution of solid slag and reclaimed water; separating solid slag and regenerated water; and dropwise adding 5M alkali liquor into the solid slag, stirring and soaking for 2h for desorption, separating chromium ions adsorbed on clay mineral sites from the clay minerals to realize desorption, dropwise adding 5M acid liquor, stirring and soaking for 2h, and performing activation and regeneration on the clay raw ores.
The addition amount of the clay raw ore is 5g/L, and the clay raw ore is any one or more of montmorillonite, bentonite, rectorite, kaolin, illite, halloysite, palygorskite, sepiolite, attapulgite, vermiculite, chlorite and pyrite.
In addition, the particle size of the clay raw ore is 15 μm, and the clay raw ore comprises montmorillonite, bentonite, rectorite, kaolin, palygorskite, sepiolite, attapulgite and vermiculite.
The clay raw ore comprises, by weight, 2 parts of montmorillonite, 1.5 parts of bentonite, 5 parts of rectorite, 3 parts of kaolin, 1 part of palygorskite, 1.3 parts of sepiolite, 4.5 parts of attapulgite and 1 part of vermiculite.
Example 3
A method for directly treating hexavalent chromium-containing wastewater by using clay raw ore comprises the following steps:
adding the powder of the clay raw ore into the wastewater containing hexavalent chromium to obtain a mixed solution; adjusting the pH value of the mixed solution to 2.5; heating the mixed solution to enable the temperature of the mixed solution to be 35 ℃; fully stirring for 33 hours at the stirring speed of 250rpm, and standing to obtain a mixed solution of solid slag and reclaimed water; separating solid slag and regenerated water; and dropwise adding 4.5M acid liquor into the solid slag, stirring and soaking for 1.5h for desorption, separating chromium ions adsorbed on clay mineral sites from the clay minerals to realize desorption, and dropwise adding 4.5M acid liquor, stirring and soaking for 1.5h to activate and regenerate the clay raw ores.
The addition amount of the clay raw ore is 4g/L, and the clay raw ore is any one or more of montmorillonite, bentonite, rectorite, kaolin, illite, halloysite, palygorskite, sepiolite, attapulgite, vermiculite, chlorite and pyrite.
In addition, the particle size of the clay raw ore is 10 μm, and the clay raw ore comprises montmorillonite, bentonite, rectorite, kaolin, palygorskite, sepiolite, attapulgite and vermiculite. The clay raw ore comprises, by weight, 3 parts of montmorillonite, 2 parts of bentonite, 6 parts of rectorite, 4 parts of kaolin, 1.2 parts of palygorskite, 2.0 parts of sepiolite, 5.3 parts of attapulgite and 1.2 parts of vermiculite.
Example 4
A method for directly treating hexavalent chromium-containing wastewater by using clay raw ore comprises the following steps:
adding the powder of the clay raw ore into the wastewater containing hexavalent chromium to obtain a mixed solution; adjusting the pH value of the mixed solution to 4; heating the mixed solution to make the temperature of the mixed solution be 40 ℃; fully stirring for 35 hours at the stirring speed of 200rpm, and standing to obtain a mixed solution of solid slag and reclaimed water; separating solid slag and regenerated water; and dropwise adding 4.5M acid liquor into the solid slag, stirring and soaking for 1.5h for desorption, separating chromium ions adsorbed on clay mineral sites from the clay minerals to realize desorption, and dropwise adding 4.5M acid liquor, stirring and soaking for 1.5h to activate and regenerate the clay raw ores.
The addition amount of the clay raw ore is 5g/L, and the clay raw ore is any one or more of montmorillonite, bentonite, rectorite, kaolin, illite, halloysite, palygorskite, sepiolite, attapulgite, vermiculite, chlorite and pyrite.
In addition, the particle size of the clay raw ore is 10 μm, and the clay raw ore comprises montmorillonite, bentonite, rectorite, kaolin, palygorskite, sepiolite, attapulgite and vermiculite. The clay raw ore comprises, by weight, 3 parts of montmorillonite, 2 parts of bentonite, 5 parts of rectorite, 4.8 parts of kaolin, 1.5 parts of palygorskite, 2.0 parts of sepiolite, 5.3 parts of attapulgite and 2 parts of vermiculite.
Comparative example
The method selects the clay minerals after mineral separation to remove chromium ions, and the specific operation is the same as that in example 4, except that the clay raw ores are replaced by the clay minerals after mineral separation.
The sewage having the chromium ion concentrations of 50mg/L, 75mg/L and 100mg/L was purified by the methods of examples 1, 2, 3 and 4 and comparative example, and the chromium ion removal rate was calculated by measuring the chromium ion concentration after purification, with the following results:
(1) the pure clay mineral adsorbing material has fine granularity, is easy to disperse and pulverize after meeting water, and is easy to cause difficulty in subsequent solid-liquid separation. The raw clay ore used in the invention is not easy to deform after meeting water, has large specific gravity, and is easy to carry out solid-liquid separation after the hexavalent chromium wastewater is treated.
(2) When adsorbing hexavalent chromium, a simple clay mineral is easily affected by environmental conditions, such as pH, and thus a phenomenon of deterioration of treatment effect is likely to occur in practical applications. The raw clay ore used in the invention is more suitable for hexavalent chromium wastewater under different environmental conditions due to various components.
(3) The hexavalent chromium is not adsorbed by a pure clay mineral, and therefore, the hexavalent chromium is often strengthened by various modification methods, which generally include calcination, surface activation, compounding, and the like. These modification processes are complex and require the use of additional resources. The clay raw ore used in the invention can be directly used without excessive treatment processes, and the treatment effect on hexavalent chromium is not inferior to that of the modified clay mineral.
The raw clay ore adopted by the invention contains components such as pyrite, transition metal oxide and the like, and has a reduction effect on hexavalent chromium in wastewater. The removal efficiency of the chromium ions is high, and the obtained chromium ions are easily separated from the clay minerals. The applicable range of pH value in the removing process is wide.
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.
Claims (9)
1. A method for directly treating hexavalent chromium-containing wastewater by using clay raw ore is characterized by comprising the following steps:
adding the powder of the clay raw ore into the wastewater containing hexavalent chromium to obtain a mixed solution; adjusting the pH value of the mixed solution to 2-6; heating the mixed solution to ensure that the temperature of the mixed solution is 30-45 ℃; fully stirring for 30-36h, and standing to obtain a mixed solution of solid slag and regenerated water; separating the solid slag from the regenerated water,
the addition amount of the clay raw ore is 3-5g/L, and the clay raw ore is any one or more of montmorillonite, bentonite, rectorite, kaolin, illite, halloysite, palygorskite, sepiolite, attapulgite, vermiculite, chlorite and pyrite.
2. The method for directly treating hexavalent chromium-containing wastewater by using clay raw ore according to claim 1, wherein the effective components in the clay raw ore comprise: fe2O3、TiO2、FeS2、Na2O、MnO、ZnO、CuO、Ag2O。
3. The method for directly treating hexavalent chromium-containing wastewater using clay raw ore according to claim 2, wherein the particle size of the clay raw ore is 5 to 15 μm.
4. The method for directly treating hexavalent chromium-containing wastewater by using the raw clay ore according to claim 3, wherein the stirring speed of the stirring is 200-260 rpm.
5. The method for directly treating hexavalent chromium-containing wastewater according to claim 4, wherein the clay raw ore comprises montmorillonite, bentonite, rectorite, kaolin, palygorskite, sepiolite, attapulgite and vermiculite.
6. The method of claim 5, wherein the clay raw ore comprises 2-4 parts by weight of montmorillonite, 1.5-3 parts by weight of bentonite, 5-7 parts by weight of rectorite, 3-5 parts by weight of kaolin, 1-2 parts by weight of palygorskite, 1.3-2.6 parts by weight of sepiolite, 4.5-6.3 parts by weight of attapulgite and 1-2 parts by weight of vermiculite.
7. The method for directly treating hexavalent chromium-containing wastewater according to claim 6, wherein the clay raw ore comprises 4 parts by weight of montmorillonite, 3 parts by weight of bentonite, 7 parts by weight of rectorite, 5 parts by weight of kaolin, 2 parts by weight of palygorskite, 2.6 parts by weight of sepiolite, 6.3 parts by weight of attapulgite and 2 parts by weight of vermiculite.
8. The method for directly treating hexavalent chromium-containing wastewater by using clay raw ore according to claim 7, further comprising the steps of: and dropwise adding alkali liquor into the solid slag, stirring and soaking for 0.1-2 h for desorption, dropwise adding acid liquor, stirring and soaking for 0.1-2 h, and performing activation regeneration on the clay raw ore.
9. The method for directly treating hexavalent chromium-containing wastewater by using clay raw ore according to claim 8, wherein the concentration of the alkali solution is 3-5M, and the concentration of the acid solution is 3-5M.
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| CN113461131B (en) * | 2021-07-01 | 2022-06-07 | 中冶南方都市环保工程技术股份有限公司 | Preparation method and application of heavy metal and organic matter composite sewage purifying agent |
| CN114804412A (en) * | 2022-04-15 | 2022-07-29 | 桂林电子科技大学 | Treatment process of mixed waste liquid of water quality online monitoring equipment |
| CN114804412B (en) * | 2022-04-15 | 2023-11-10 | 桂林电子科技大学 | Treatment process of mixed waste liquid of water quality on-line monitoring equipment |
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