CN111547804A - Composite defluorinating agent for industrial wastewater, preparation method and method for defluorinating industrial wastewater - Google Patents
Composite defluorinating agent for industrial wastewater, preparation method and method for defluorinating industrial wastewater Download PDFInfo
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- CN111547804A CN111547804A CN202010411251.4A CN202010411251A CN111547804A CN 111547804 A CN111547804 A CN 111547804A CN 202010411251 A CN202010411251 A CN 202010411251A CN 111547804 A CN111547804 A CN 111547804A
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F1/56—Macromolecular 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
- 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
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a composite defluorinating agent for industrial wastewater, a preparation method thereof and a method for defluorinating industrial wastewater, belonging to the technical field of defluorination of industrial wastewater. The defluorinating agent comprises 40-60 wt.% of silicate, 20-30 wt.% of aluminum salt dopant and the balance of divalent cation salt, wherein the silicate is taken as a defluorinating space framework, partial aluminum atoms are introduced to replace silicon atoms to form aluminum silicon oxygen tetrahedrons, and divalent cations such as calcium ions and magnesium ions are introduced, so that the fluorine ions can be effectively locked in the framework structure, the solubility product of formed precipitates is greatly reduced, and deep defluorination is realized; by using the defluorinating agent and the defluorinating method of the invention and adopting a one-step precipitation method, the fluorine ions of the inlet water are treated under the condition of less than 100mg/L to reach the fluorine ions of the outlet water of less than 1 mg/L; when the water inlet concentration and the water outlet concentration are the same, the amount of sludge generated by using the defluorinating agent is more than 30 percent less than that generated by using the traditional calcium salt method.
Description
Technical Field
The invention relates to a defluorinating agent and a defluorinating method, in particular to a composite defluorinating agent for industrial wastewater, a preparation method and a method for defluorinating industrial wastewater, belonging to the technical field of defluorination of industrial wastewater.
Background
The existing defluorination technology can be divided into two major categories in principle, one category is through a precipitation method, namely, an ionic bond is formed between a defluorination agent and fluorine ions to generate a substance with a small solubility product, for example, the defluorination agent adopts calcium salt or magnesium salt to precipitate the fluorine ions; the other is that the concentration of fluorine ions in water is reduced by an adsorption method such as using alumina, bone char, resin or the like as a fluorine removing agent, which is itself a solid, and adsorbing fluorine ions on the solid of the fluorine removing agent by the attraction between anions and cations.
The first type of precipitation method described above has problems in that: at present, a precipitator with high cost performance is difficult to find, and the cost is low while deep fluorine removal is realized. Although the traditional calcium salt or magnesium salt is low in price, the solubility product is not small enough, and the requirement of deep fluorine removal cannot be met.
The second adsorption method has problems in that: although most of the adsorption materials can realize deep fluorine removal, the adsorption materials are regenerated and waste liquid treatment is carried out after regeneration, the regeneration times of the adsorption materials are limited and are usually not more than ten times, so that in actual use, the investment cost is high, and the fluorine removal process is complicated.
Therefore, it is required to find a fluorine removing agent which can combine the advantages of the first precipitation method and the second adsorption method, and a fluorine removing method which is simple in fluorine removing process.
Disclosure of Invention
In order to solve the technical problems, the invention provides a composite defluorinating agent for industrial wastewater, a preparation method and a method for defluorinating industrial wastewater.
The technical scheme of the invention is as follows:
a composite defluorinating agent for industrial wastewater comprises the following components in percentage by mass: 40-60 wt.% silicate, 20-30 wt.% aluminum salt dopant, and balance divalent cation salt.
The further technical scheme is as follows:
the silicate is at least one of sodium silicate, potassium silicate, magnesium silicate, calcium silicate and aluminum silicate.
The further technical scheme is as follows:
the aluminum salt dopant is at least one of aluminum sulfate, aluminum chloride, polyaluminum sulfate, polyaluminum chloride, aluminum nitrate, aluminum hydroxide, alumina, aluminum potassium sulfate, sodium metaaluminate and potassium metaaluminate.
The further technical scheme is as follows:
the divalent cation salt is at least one of magnesium chloride, magnesium sulfate, magnesium nitrate, magnesium carbonate, magnesium oxide, magnesium bicarbonate, calcium sulfate, calcium chloride, calcium nitrate, calcium carbonate, calcium bicarbonate, calcium oxide and calcium bisulfate.
The invention also discloses a preparation method of the composite defluorinating agent for industrial wastewater, which mainly comprises the following steps:
1) weighing the following components in percentage by mass based on the total mass of the fluorine removing agent: 40-60 wt.% silicate, 20-30 wt.% aluminum salt dopant, and balance divalent cation salt;
2) firstly adding silicate into a mixing reactor, then adding an aluminum salt dopant into the mixing reactor, stirring the mixture for 5 to 10 minutes by using a stirring device, adding a divalent cation salt, and continuously stirring the mixture until the mixture is fully mixed to obtain the composite defluorinating agent for industrial wastewater.
The invention also discloses a method for removing fluorine from industrial wastewater by using the composite fluorine removing agent for industrial wastewater, which mainly comprises the following steps:
s1, adjusting the pH value of the wastewater to be treated to be weakly acidic or weakly alkaline;
s2, mixing the defluorinating agent with water to form defluorinating agent/water mixed solution;
s3, adding the defluorinating agent/water mixed solution obtained in the S2 step into the wastewater to be treated obtained in the S1 step, and then adjusting the pH value to 6-7 again; wherein the mass ratio of the fluorine removing agent to the fluorine ions in the wastewater to be treated is (0.5-6.0): 100;
and S4, adding a flocculant aqueous solution into the wastewater to be treated obtained by the step S3 for reaction for 10-15min, filtering and precipitating, and discharging the supernatant liquid which can reach the standard.
The further technical scheme is as follows:
in the step S1, the pH value of the wastewater to be treated is 5-6 when the wastewater to be treated is weakly acidic, and the pH value of the wastewater to be treated is 7-8.5 when the wastewater to be treated is weakly alkaline.
The further technical scheme is as follows:
the mass percentage of the fluorine removing agent in the fluorine removing agent/water mixed solution is 1.0-2.0 wt.%.
The further technical scheme is as follows:
the flocculant aqueous solution is 0.1-0.2 wt.% polyacrylamide aqueous solution, and the mass ratio of polyacrylamide to fluorine ions in wastewater to be treated in the flocculant aqueous solution is (0.4-1.0): 1000.
The further technical scheme is as follows:
the flocculant aqueous solution is a mixture of 0.1-0.2 wt.% polyacrylamide aqueous solution and 5-6 wt.% polyaluminum chloride aqueous solution, wherein the mass ratio of polyacrylamide in the polyacrylamide aqueous solution to fluoride ions in the wastewater to be treated is (0.4-1.0):1000, and the mass ratio of polyaluminum chloride in the polyaluminum chloride aqueous solution to fluoride ions in the wastewater to be treated is (0.1-0.2): 1.
The design principle of the defluorinating agent is as follows: in order to deeply remove the fluorine ions, a strong chemical bond must be formed between the fluorine removing agent and the fluorine ions, and a certain spatial binding effect is constructed, which is similar to a chelate bond formed between a chelating agent and a metal ion, so that after one fluorine ion and the fluorine removing agent act, a plurality of chemical bonds can be formed, and thus, after a certain spatial structure is satisfied, the fluorine ions are difficult to escape from the embedded sites.
The defluorinating agent designed by the invention is silicate (MSiO)3) As a space skeleton for removing fluorine, a certain proportion of aluminum atoms are introduced to replace silicon atoms to form an aluminum-silicon-oxygen tetrahedron (MAL)xSiYO3). Because the aluminum has a valence of +4 and the aluminum has a valence of +3, a cation vacancy is formed in the aluminum-silicon-oxygen tetrahedron, namely a negative charge is generated, and because a stronger bonding effect exists between the aluminum-fluorine and the silicon-aluminum, the density of the negative charge in the framework is further improved along with the adsorption of fluorine ions, so that the aluminum-fluorine-silicon-aluminum composite material is full ofThe charge balance of the whole body is satisfied, and divalent cations such as calcium and magnesium ions are introduced, so that the requirement that the whole framework reaches electric neutrality (MCa) can be metxAlYSizO3Or MMgxAlYSizO3) On the other hand, fluorine ions can be effectively locked in the framework structure, so that the solubility product of the formed precipitate is greatly reduced, and the aim of deeply removing fluorine is fulfilled, wherein the formed precipitate contains Si-F bonds, Al-F bonds, Ca-F bonds or Mg-F bonds.
In addition, in the present application, the concentrations of the adopted agents are calculated according to the mass percentage, for example, the concentration units of the defluorinating agent/water mixed solution, the polyacrylamide aqueous solution and the polyaluminum chloride aqueous solution are wt.%; the concentrations of the contaminants mentioned are all calculated in mg/L, as concentration of the fluoride ion content. Wherein the density of the various liquids in the process is, unless specified or specified, in the order of 1g/cm3The evaluation is carried out as a routine operation in industrial applications by the person skilled in the art and is not described in any more detail in this application.
The beneficial technical effects of the invention are as follows: by using the defluorinating agent and the defluorinating method of the invention and adopting a one-step precipitation method, the fluoride ions in the inlet water can reach the standard that the fluoride ions in the outlet water are less than 1mg/L after being treated under the condition that the fluoride ions in the inlet water are less than 100 mg/L; under the condition of the same water inlet concentration and water outlet concentration, the amount of sludge generated by using the novel defluorinating agent is more than 30 percent less than that generated by using a calcium salt method.
Detailed Description
In order to clearly understand the technical means of the present invention and to implement the technical means according to the content of the specification, the following embodiments are further described in detail in the following with reference to the specific examples, which are used for illustrating the present invention and are not intended to limit the scope of the present invention.
In the following specific embodiments of the present application, the concentrations of the adopted agents are calculated according to mass percentages, for example, the concentration units of the defluorinating agent/water mixed solution, the polyacrylamide aqueous solution and the polyaluminum chloride aqueous solution are wt.%;the concentrations of the contaminants mentioned are all calculated in mg/L, as concentration of the fluoride ion content. Wherein the density of the various liquids in the process is, unless specified or specified, in the order of 1g/cm3The evaluation is carried out as a routine operation in industrial applications for a person skilled in the art, and is not described in particular in the following specific examples of the application.
Detailed description of the preferred embodiment 1
100ml of fluorine-containing wastewater of a certain pickling enterprise is taken, wherein the content of fluorine ions is 5.2 mg/L.
The fluorine removing agent is adopted to remove fluorine ions in wastewater:
s1, adjusting the pH value of the wastewater to be treated to be weakly acidic to 5-6;
s2, mixing the fluorine removing agent and water to form a fluorine removing agent/water mixed solution with the concentration of 1.0 wt.%;
s3, adding 2.5ml of the defluorinating agent/water mixed solution obtained in the S2 step into the wastewater to be treated obtained in the S1 step, and then adjusting the pH value to 6-7 again;
s4, adding 0.5ml of polyacrylamide aqueous solution with the concentration of 0.1 wt.% into the wastewater to be treated obtained by the step S3, reacting for 10min, filtering and precipitating, and measuring the concentration of the fluorine ions in the supernatant to be 0.6mg/L, wherein the supernatant can reach the standard and be discharged.
Specific example 2
100ml of fluorine-containing wastewater of an electronic enterprise is taken, wherein the fluorine ion content is 18.6 mg/L.
The fluorine removing agent is adopted to remove fluorine ions in wastewater:
s1, adjusting the pH value of the wastewater to be treated to be weakly acidic to 5-6;
s2, mixing the fluorine removing agent and water to form a fluorine removing agent/water mixed solution with the concentration of 1.0 wt.%;
s3, adding 10ml of the defluorinating agent/water mixed solution obtained in the S2 step into the wastewater to be treated obtained in the S1 step, and then adjusting the pH value to 6-7 again;
s4, adding 1ml of polyacrylamide aqueous solution with the concentration of 0.1 wt.% into the wastewater to be treated obtained by the step S3, reacting for 10min, filtering and precipitating, and measuring the concentration of the fluorine ions in the supernatant to be 0.8mg/L, wherein the supernatant can reach the standard and be discharged.
Specific example 3
100ml of fluorine-containing wastewater subjected to lime treatment in a certain photovoltaic enterprise is taken, wherein the content of fluorine ions is 8.3 mg/L.
The fluorine removing agent is adopted to remove fluorine ions in wastewater:
s1, adjusting the pH value of the wastewater to be treated to be weakly acidic and 5.0;
s2, mixing the fluorine removing agent and water to form a fluorine removing agent/water mixed solution with the concentration of 1.0 wt.%;
s3, adding 0.5ml of the defluorinating agent/water mixed solution obtained in the S2 step into the wastewater to be treated obtained in the S1 step, and then adjusting the pH value to 7 again;
s4, adding 3ml of polyaluminum chloride aqueous solution with the concentration of 5 wt.% into the wastewater to be treated obtained by the step S3, adding 0.4ml of polyacrylamide aqueous solution with the concentration of 0.1 wt.% into the wastewater, reacting for 10min, filtering and precipitating, and measuring the concentration of fluorine ions in the supernatant to be 0.7mg/L, wherein the supernatant can reach the standard and be discharged.
By using the defluorinating agent and the defluorinating method of the invention and adopting a one-step precipitation method, the fluoride ions in the inlet water can reach the standard that the fluoride ions in the outlet water are less than 1mg/L after being treated under the condition that the fluoride ions in the inlet water are less than 100 mg/L; under the condition of the same water inlet concentration and water outlet concentration, the amount of sludge generated by using the novel defluorinating agent is more than 30 percent less than that generated by using a calcium salt method.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The composite defluorinating agent for industrial wastewater is characterized by comprising the following components in percentage by mass: 40-60 wt.% silicate, 20-30 wt.% aluminum salt dopant, and balance divalent cation salt.
2. The composite fluorine removing agent for industrial wastewater according to claim 1, wherein: the silicate is at least one of sodium silicate, potassium silicate, magnesium silicate, calcium silicate and aluminum silicate.
3. The composite fluorine removing agent for industrial wastewater according to claim 1, wherein: the aluminum salt dopant is at least one of aluminum sulfate, aluminum chloride, polyaluminum sulfate, polyaluminum chloride, aluminum nitrate, aluminum hydroxide, alumina, aluminum potassium sulfate, sodium metaaluminate and potassium metaaluminate.
4. The composite fluorine removing agent for industrial wastewater according to claim 1, wherein: the divalent cation salt is at least one of magnesium chloride, magnesium sulfate, magnesium nitrate, magnesium carbonate, magnesium oxide, magnesium bicarbonate, calcium sulfate, calcium chloride, calcium nitrate, calcium carbonate, calcium bicarbonate, calcium oxide and calcium bisulfate.
5. A preparation method of the composite fluorine removing agent for industrial wastewater as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
1) weighing the following components in percentage by mass based on the total mass of the fluorine removing agent: 40-60 wt.% silicate, 20-30 wt.% aluminum salt dopant, and balance divalent cation salt;
2) firstly adding silicate into a mixing reactor, then adding an aluminum salt dopant into the mixing reactor, stirring the mixture for 5 to 10 minutes by using a stirring device, adding a divalent cation salt, and continuously stirring the mixture until the mixture is fully mixed to obtain the composite defluorinating agent for industrial wastewater.
6. A method for removing fluorine from industrial wastewater by using the composite fluorine removing agent for industrial wastewater as defined in any one of claims 1 to 4, comprising the steps of:
s1, adjusting the pH value of the wastewater to be treated to be weakly acidic or weakly alkaline;
s2, mixing the defluorinating agent with water to form defluorinating agent/water mixed solution;
s3, adding the defluorinating agent/water mixed solution obtained in the S2 step into the wastewater to be treated obtained in the S1 step, and then adjusting the pH value to 6-7 again; wherein the mass ratio of the fluorine removing agent to the fluorine ions in the wastewater to be treated is (0.5-6.0): 100;
and S4, adding a flocculant aqueous solution into the wastewater to be treated obtained by the step S3 for reaction for 10-15min, filtering and precipitating, and discharging the supernatant liquid which can reach the standard.
7. The method for performing fluorine removal from industrial wastewater according to claim 6, characterized in that: in the step S1, the pH value of the wastewater to be treated is 5-6 when the wastewater to be treated is weakly acidic, and the pH value of the wastewater to be treated is 7-8.5 when the wastewater to be treated is weakly alkaline.
8. The method for performing fluorine removal from industrial wastewater according to claim 6, characterized in that: the mass percentage of the fluorine removing agent in the fluorine removing agent/water mixed solution is 1.0-2.0 wt.%.
9. The method for performing fluorine removal from industrial wastewater according to claim 6, characterized in that: the flocculant aqueous solution is 0.1-0.2 wt.% polyacrylamide aqueous solution, and the mass ratio of polyacrylamide to fluorine ions in wastewater to be treated in the flocculant aqueous solution is (0.4-1.0): 1000.
10. The method for performing fluorine removal from industrial wastewater according to claim 6, characterized in that: the flocculant aqueous solution is a mixture of 0.1-0.2 wt.% polyacrylamide aqueous solution and 5-6 wt.% polyaluminum chloride aqueous solution, wherein the mass ratio of polyacrylamide in the polyacrylamide aqueous solution to fluoride ions in the wastewater to be treated is (0.4-1.0):1000, and the mass ratio of polyaluminum chloride in the polyaluminum chloride aqueous solution to fluoride ions in the wastewater to be treated is (0.1-0.2): 1.
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Cited By (9)
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| CN112624388A (en) * | 2020-10-23 | 2021-04-09 | 北京朗新明环保科技有限公司 | Circulating fluidization induced crystallization silicon and fluorine removal method |
| CN112794420A (en) * | 2020-12-23 | 2021-05-14 | 武汉理工大学 | Efficient low-cost fluorine removal agent and deep fluorine removal method |
| CN112850867A (en) * | 2021-01-22 | 2021-05-28 | 北京华德创业环保设备有限公司 | Deep defluorination medicament and preparation method thereof |
| CN113499756A (en) * | 2021-07-23 | 2021-10-15 | 同济大学 | Defluorinating agent based on metal organic framework material |
| CN113511714A (en) * | 2021-06-17 | 2021-10-19 | 苏州福硼科技发展有限公司 | Compound medicament for removing fluoride ions and use method thereof |
| CN114477564A (en) * | 2022-03-17 | 2022-05-13 | 中国矿业大学(北京) | Defluorination medicament, preparation method and method for defluorination of hydrofluoric acid wastewater |
| CN114835232A (en) * | 2022-05-23 | 2022-08-02 | 中国科学院生态环境研究中心 | Defluorination agent for waste acid wastewater, application and defluorination method |
| CN115636493A (en) * | 2022-11-16 | 2023-01-24 | 中科润蓝环保技术(北京)股份有限公司 | Sewage fluorine removal agent and preparation and application methods thereof |
| CN117509810A (en) * | 2024-01-05 | 2024-02-06 | 深圳市盘古环保科技有限公司 | Efficient reaction industrial wastewater defluorination treatment method and equipment |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112624388A (en) * | 2020-10-23 | 2021-04-09 | 北京朗新明环保科技有限公司 | Circulating fluidization induced crystallization silicon and fluorine removal method |
| CN112624388B (en) * | 2020-10-23 | 2022-11-08 | 国能朗新明环保科技有限公司 | Circulating fluidization induced crystallization silicon and fluorine removal method |
| CN112794420A (en) * | 2020-12-23 | 2021-05-14 | 武汉理工大学 | Efficient low-cost fluorine removal agent and deep fluorine removal method |
| CN112794420B (en) * | 2020-12-23 | 2023-11-28 | 武汉理工大学 | Efficient low-cost defluorination medicament and deep defluorination method |
| CN112850867A (en) * | 2021-01-22 | 2021-05-28 | 北京华德创业环保设备有限公司 | Deep defluorination medicament and preparation method thereof |
| CN113511714A (en) * | 2021-06-17 | 2021-10-19 | 苏州福硼科技发展有限公司 | Compound medicament for removing fluoride ions and use method thereof |
| CN113499756A (en) * | 2021-07-23 | 2021-10-15 | 同济大学 | Defluorinating agent based on metal organic framework material |
| CN114477564B (en) * | 2022-03-17 | 2023-08-25 | 中国矿业大学(北京) | Defluorination medicament, preparation method and defluorination method for hydrofluoric acid wastewater |
| CN114477564A (en) * | 2022-03-17 | 2022-05-13 | 中国矿业大学(北京) | Defluorination medicament, preparation method and method for defluorination of hydrofluoric acid wastewater |
| CN114835232A (en) * | 2022-05-23 | 2022-08-02 | 中国科学院生态环境研究中心 | Defluorination agent for waste acid wastewater, application and defluorination method |
| CN115636493B (en) * | 2022-11-16 | 2023-03-10 | 中科润蓝环保技术(北京)股份有限公司 | Sewage fluorine removal agent and preparation and application methods thereof |
| CN115636493A (en) * | 2022-11-16 | 2023-01-24 | 中科润蓝环保技术(北京)股份有限公司 | Sewage fluorine removal agent and preparation and application methods thereof |
| CN117509810A (en) * | 2024-01-05 | 2024-02-06 | 深圳市盘古环保科技有限公司 | Efficient reaction industrial wastewater defluorination treatment method and equipment |
| CN117509810B (en) * | 2024-01-05 | 2024-03-22 | 深圳市盘古环保科技有限公司 | Efficient reaction industrial wastewater defluorination treatment method and equipment |
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