CN114853109B - Deep defluorination medicament and preparation method and use method thereof - Google Patents

Deep defluorination medicament and preparation method and use method thereof Download PDF

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CN114853109B
CN114853109B CN202210791944.XA CN202210791944A CN114853109B CN 114853109 B CN114853109 B CN 114853109B CN 202210791944 A CN202210791944 A CN 202210791944A CN 114853109 B CN114853109 B CN 114853109B
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oxide
fluorine
deep
mixed solution
carbonate
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CN114853109A (en
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刘湘雄
刘承斌
唐海芳
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Hunan University
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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
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention discloses a deep defluorination medicament and a preparation method and a use method thereof. The deep defluorination medicament comprises 1-5% of yttrium oxide or yttrium carbonate, 1-5% of aluminum oxide or aluminum hydroxide, 1-5% of cerium oxide or cerium carbonate, 1-5% of ferric oxide or ferric sulfate, 1-5% of samarium oxide or samarium carbonate, 0.5-2% of calcium oxide or calcium hydroxide, 1-3% of sulfuric acid and deionized water in preset percentage content; wherein the sum of the percentage contents of all the components is 100%. The deep fluorine removal medicament provided by the invention can enable inlet water fluorine ions to reach the standard that outlet water fluorine ions are less than 5 mg/L after being treated under the condition that inlet water fluorine ions are less than 300 mg/L; the pH application range is wide; the novel defluorinating agent has the advantages of simple chemical dosing, high defluorinating rate, small sludge yield, low treatment cost, wide application range and the like under the condition of the same water inlet concentration and water outlet concentration, and can be rapidly settled without adding a flocculating agent.

Description

Deep defluorination medicament and preparation method and use method thereof
Technical Field
The invention relates to the technical field of fluorine-containing wastewater treatment, in particular to a deep defluorination medicament and a preparation method and a use method thereof.
Background
In recent years, with the rapid development of economy in China, the fluorination industry has become the backbone industry for the development of modern industrial technology, and plays a significant role in industrial production of military industry, aviation industry, automobile manufacturing industry, photovoltaic industry and the like. The fluorine ion content in the fluorine-containing wastewater is greatly different due to different production characteristics of various industries. Numerous production enterprises bring great potential and economic prospect to the market and also cause certain damage to the ecological environment.
Strict control standards are established for the safety of the concentration of the fluorine ions in water in China, and the sanitary standard for drinking water (GB 5749-2006) cannot exceed 1 mg/L of the concentration of the fluorine ions in the drinking water. The A-level standard of the wastewater discharge town sewer water quality standard (GB/T31962-2015) can not exceed 10 mg/L of the fluorine ion concentration in the discharged fluorine-containing wastewater. If the waste water is directly discharged into natural water body without being treated to reach the standard, serious pollution is caused to the ecological environment, and the life safety of people is threatened.
The prior method for treating the fluorine-containing wastewater mainly comprises an adsorption method, an electrocoagulation method, a reverse osmosis method, an ion exchange method, a chemical precipitation method, a coagulation sedimentation method and the like. The treatment methods have the advantages and the disadvantages, wherein the ion exchange method has higher cost, strict requirements on the quality of wastewater and complex regeneration operation; the electrocoagulation method and the reverse osmosis method have the disadvantages of complex device, expensive equipment, large power consumption and high operation level requirement, so the electrocoagulation method and the reverse osmosis method are rarely adopted; the chemical precipitation method has simple process and small investment, and is the most widely applied method for treating the fluorine-containing wastewater at present.
At present, common chemical precipitation methods comprise a calcium salt precipitation method, an aluminum salt precipitation method, a water glass fluorine removal method and the like, wherein the fluorine removal by calcium salt is difficult to reduce the concentration of fluorine ions to be below 20 mg/L; the defluorination of aluminum salt requires that the PH range is 6-7, the PH application range is narrow, pipeline equipment and the like are easy to scale, the defluorination cost is high, an aluminum fluorine complex can be generated and continuously exists in a water body, and fluorine ions are not really removed; the fluorine removal from the water glass also generates fluorine complexes which continue in the water body and do not really remove the fluorine.
Therefore, a new deep fluorine removal agent, a preparation method and a use method thereof are researched and developed to solve the technical problems.
Disclosure of Invention
The invention aims to provide a deep fluorine removal agent, which is used for solving the technical problems of low fluorine removal efficiency and narrow pH application range in the related art.
In order to solve the technical problems, the deep defluorinating medicament provided by the invention comprises 1-5% of yttrium oxide or yttrium carbonate, 1-5% of aluminum oxide or aluminum hydroxide, 1-5% of cerium oxide or cerium carbonate, 1-5% of ferric oxide or ferric sulfate, 1-5% of samarium oxide or samarium carbonate, 0.5-2% of calcium oxide or calcium hydroxide, 1-3% of sulfuric acid and deionized water in preset percentage; wherein the sum of the percentage contents of the components is 100%.
In order to solve the technical problems, the invention also provides a preparation method of the deep fluorine removal agent, which comprises the following steps:
heating and stirring deionized water, yttrium oxide or yttrium carbonate, aluminum oxide or aluminum hydroxide, cerium oxide or cerium carbonate, iron oxide or ferric sulfate, samarium oxide or samarium carbonate to form a mixed solution, wherein when the temperature of the mixed solution reaches a first preset temperature range, the heating and the stirring are stopped;
adding the deionized water into the mixed solution again, and then stirring and adding sulfuric acid until the pH value of the mixed solution is less than 1;
adding calcium oxide or calcium hydroxide into the mixed solution by stirring until the pH value of the mixed solution reaches 3; it can be understood that the user can fine-tune the PH value here according to practical situations, and only needs to satisfy that the PH of the mixed liquor reaches about 3, for example, PH =3.5 or PH = 2.8.
And cooling the mixed solution to a second preset temperature range, and filtering to remove sediments in the mixed solution to obtain the deep fluorine removal medicament.
Preferably, the sulfuric acid is commercially available in industrial grade in liquid form.
Preferably, any one of the yttrium oxide or yttrium carbonate, the aluminum oxide or aluminum hydroxide, the cerium oxide or cerium carbonate, the iron oxide or iron sulfate, the samarium oxide or samarium carbonate, and the calcium oxide or calcium hydroxide is commercially available in a solid state.
Preferably, the first preset temperature range is 70 ℃ to 100 ℃.
Preferably, the temperature rises by no more than 5 ℃ per minute during the heating and stirring.
Preferably, the stirring speed is 1500 rpm during the heating and stirring.
Preferably, the second preset temperature range is 20 ℃ to 30 ℃.
Preferably, in the step of adding the deionized water into the mixed solution again, and then adding the sulfuric acid with stirring until the pH value of the mixed solution is less than 1, the pH value needs to be kept below 1, and the next step is not started until the mixed solution is stirred for 10-15 minutes.
In order to solve the technical problems, the invention also provides a use method of the deep fluorine removal agent, which comprises the following steps:
weighing the deep defluorinating agent in a corresponding proportion according to the concentration of fluorine ions in the wastewater to be treated;
adding the deep defluorination agent into the wastewater, uniformly stirring and mixing to obtain a treatment solution, and standing the treatment solution within a preset time;
taking supernatant in the treatment liquid, and measuring the concentration of fluorine ions in the supernatant;
and when the concentration of the fluorine ions in the supernatant reaches the discharge requirement, discharging the filtered treatment liquid outwards.
The deep defluorination medicament provided by the invention mainly takes a composite adsorption material medicament, and a cation group and fluorine ions in the composite adsorption material in the medicament form a precipitate which is difficult to dissolve in water and are removed by standing and settling. The cationic groups in the composite adsorption material have a certain synergistic effect, residual fluoride ions in the combined water body can be efficiently adsorbed, the overall sedimentation speed is improved, the sedimentation time is shortened, and the defluorination efficiency is improved.
The agent can enable the fluoride ions in the inlet wastewater to reach the standard that the fluoride ions in the outlet water are less than 5 mg/L after being treated under the condition that the fluoride ions in the inlet wastewater are less than 300 mg/L; the pH application range is wide, and the pH is not required to be adjusted for multiple times; the sludge is quickly settled after the reaction is finished, and no flocculating agent is required to be added additionally, so that the method has the advantages of simple chemical dosing, high defluorination rate, small sludge yield, low treatment cost, wide application range and the like.
The basic reaction principle of the deep fluorine removal agent provided by the invention for fluorine removal is as follows:
Y 2 O 3 +Al 2 O 3 +Ce 2 O 3 +Fe 2 O 3 +Sm 2 O 3 +CaO+H 2 o (Heat)
→Y 2 O 3 +Y(OH) 3 +Al 2 O 3 +Ce 2 O 3 +Ce(OH) 3 +Fe 2 O 3 +Sm 2 O 3 +Sm(OH) 3 +Ca(OH) 2 +H 2 O （1-1）
Or
Y 2 (CO 3 ) 3 +Al 2 O 3 +Ce 2 (CO 3 ) 3 +Fe 2 O 3 +Sm 2 (CO 3 ) 3 +CaO+H 2 O (Heat)
→Y 2 (CO 3 ) 3 +Y(OH) 3 +Al 2 O 3 +Ce 2 (CO 3 ) 3 +Ce(OH) 3 +Fe 2 O 3 +Sm 2 (CO 3 ) 3 +Sm(OH) 3 +Ca(OH) 2 +H 2 O （1-2）
Y 2 O 3 +Y(OH) 3 +Al 2 O 3 +Ce 2 O 3 +Ce(OH) 3 +Fe 2 O 3 +Sm 2 O 3 +Sm(OH) 3 +Ca(OH) 2 +H 2 O+H 2 SO 4
→(Y 3+ +Al 3+ +Ce 3+ +Fe 3+ +Sm 3+ +Ca 2+ )+H 2 O+SO 4 2- Ca (part) (SO) 4 )↓ （2-1）
Or
Y 2 (CO 3 ) 3 +Y(OH) 3 +Al 2 O 3 +Ce 2 (CO 3 ) 3 +Ce(OH) 3 +Fe 2 O 3 +Sm 2 (CO 3 ) 3 +Sm(OH) 3 +Ca(OH) 2 +H 2 O+
H 2 SO 4 →(Y 3+ +Al 3+ +Ce 3+ +Fe 3+ +Sm 3+ +Ca 2+ )+H 2 O+SO 4 2- +CO 2 ℃ + (part) Ca (SO) 4 )↓ （2-2）
n(Y 3+ +Al 3+ +Ce 3+ +Fe 3+ +Sm 3+ +Ca 2+ )+H 2 O+m(F - )
→(Y 3+ +Al 3+ +Ce 3+ +Fe 3+ +Sm 3+ +Ca 2+ ) n (F - ) m ·xH 2 O↓ （3）。
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1 (preparation of an agent for deep fluorine removal)
Adding 3g of yttrium carbonate, 1g of aluminum oxide, 3g of cerium oxide, 2g of ferric sulfate and 5g of samarium carbonate into 100ml of deionized water, slowly heating to 75 ℃ while stirring for about 40 minutes;
then adding 100ml of deionized water, slowly adding 5ml of sulfuric acid while stirring until the pH is less than 1, and continuing to stir for about 15 minutes;
adding about 1.5g of calcium hydroxide to adjust the pH value to about 3, continuously stirring at a slow speed until the temperature is reduced to below 30 ℃, and stopping stirring;
filtering to remove a small amount of sediments and obtaining the deeply defluorinating agent which is mixed evenly.
Example 2 (wastewater defluorination)
Adding 17.1 mg of sodium fluoride into 200 mL of water, detecting fluorine ions by using a thunder magnetic portable selective electrode, (adding 10mL of the prepared fluorine-containing liquid into 90 mL of deionized water, namely diluting by 10 times, wherein the pH value is 7), wherein the reading of a fluorine ion detection ion meter is 3.7 mg/L, and the actual fluorine ion concentration of the prepared fluorine-containing liquid is 37 mg/L;
adding 0.6 mL of prepared deep defluorinating medicament into the residual 190 mL of fluorine-containing liquid, magnetically stirring at a low speed for 5 min, and standing for 15 min;
taking 100mL of supernatant to detect the concentration of the fluoride ions, wherein the reading is 2.5 mg/L.
After the fluorine-containing liquid prepared by the method is added with the deep fluorine removal agent provided by the invention, the fluorine ion concentration is reduced to 2.5 mg/L from 37 mg/L.
Example 3 (waste water defluorination)
Taking 10mL of waste acid solution (the PH of the waste acid solution is less than 1, the liquid contains a plurality of heavy metals and high-concentration fluorine ions and chloride ions) of a large-scale nonferrous smelting plant in a certain country, adding 190 mL of deionized water, and detecting that the concentration of the fluorine ions in the diluted liquid is 38.4 mg/L;
adding 1 mL of the prepared deep defluorinating agent into the solution, magnetically stirring for 5 min at a slow speed, standing for 15 min, and taking the supernatant to detect that the concentration of fluorine ions is 3.5 mg/L.
After the fluorine-containing liquid with the configuration is added with the deep fluorine removal agent provided by the invention, the fluorine ion concentration is reduced from 38.4 mg/L to 3.5 mg/L.
Example 4 (waste water defluorination)
Taking 15 mL of fluorine-containing waste acid solution, adding into 185 mL of water, detecting fluorine ions by using a thunder magnetic portable selective electrode, (taking 10mL of the prepared fluorine-containing liquid, adding into 90 mL of deionized water, namely diluting by 10 times to detect the concentration of the fluorine ions), wherein the reading of a fluorine ion detection ion meter is 5.5 mg/L, and the actual concentration of the fluorine ions in the prepared fluorine-containing liquid is 55 mg/L;
and (3) directly adding 2mL of prepared deep defluorination agent into the residual 190 mL of fluorine-containing liquid with the pH value less than 1, magnetically stirring for 5 min at a slow speed, standing for 15 min, taking 100mL of supernatant, detecting the concentration of fluorine ions, and reading to be 4.4 mg/L.
After the fluorine-containing liquid with the configuration is added with the deep fluorine removal agent provided by the invention, the fluorine ion concentration is reduced from 55 mg/L to 4.4 mg/L.
Example 5 (wastewater defluorination)
Taking 10mL of fluorine-containing waste acid solution, adding the fluorine-containing waste acid solution into 190 mL of water, and detecting fluorine ions by using a thunder magnetic portable selective electrode, (taking 10mL of the prepared fluorine-containing liquid, adding the prepared fluorine-containing liquid into 90 mL of deionized water, namely diluting the prepared fluorine-containing liquid by 10 times to detect the concentration of the fluorine ions), wherein the reading of a fluorine ion detection ion meter is 3.9 mg/L, and the actual concentration of the fluorine ions of the prepared fluorine-containing liquid is 39 mg/L;
and adding an alkali liquor into the residual 190 mL of fluorine-containing liquid to adjust the pH value to about 10, adding 2mL of a prepared deep fluorine removal agent, stirring for 5 min at a slow speed by magnetic force, standing for 15 min, taking 100mL of supernatant to detect the concentration of fluorine ions, and reading to be 4.6 mg/L.
The fluorine-containing liquid prepared by the method has the advantage that under the alkaline condition, after the deep fluorine removal agent provided by the invention is added, the fluorine ion concentration is reduced from 39 mg/L to 4.6 mg/L.
Example 6 (wastewater defluorination)
Adding 130 mg of sodium fluoride into 200 mL of water, detecting fluorine ions by using a thunder magnetic portable selective electrode, (10 mL of the prepared fluorine-containing liquid is added into 90 mL of deionized water, namely diluted by 100 times, and the pH value is 6-7), the reading of a fluorine ion detection ion meter is 2.8 mg/L, and the actual fluorine ion concentration of the prepared fluorine-containing liquid is 280 mg/L;
and adding 5mL of prepared deep defluorination agent into 190 mL of fluorine-containing liquid left after sampling, magnetically stirring for 5 min at a slow speed, standing for 15 min, taking 100mL of supernatant to detect the concentration of fluorine ions, and reading to be 1.9 mg/L.
After the fluorine-containing liquid with the configuration is added with the deep fluorine removal agent provided by the invention, the fluorine ion concentration is reduced from 280 mg/L to 1.9 mg/L.
Example 7 (wastewater defluorination)
Adding 6 mg of sodium fluoride into 200 mL of water (pH is about 7), and directly detecting fluorine ions in the liquid by using a thunder magnetic portable selective electrode, wherein the reading of a fluorine ion detection ion meter is 12.8 mg/L;
then 0.4 mL of prepared deep defluorination agent is added into the fluorine-containing liquid, the mixture is magnetically stirred for 5 min at a slow speed, and after standing for 15 min, 100mL of supernatant is taken to detect the concentration of fluorine ions, and the reading is 0.5 mg/L.
After the fluorine-containing liquid with the configuration is added with the deep fluorine removal agent provided by the invention, the fluorine ion concentration is reduced from 12.8 mg/L to 0.5 mg/L.
Example 8 (wastewater defluorination)
In a sulfuric acid workshop of a super-huge type copper smelting plant, 400 mL of water sample (pH is about 6) of desulfurized gypsum post-liquid is taken, the detected fluorine ion is 5.022 mg/L, 0.2mL of prepared deep defluorination medicament is added into the fluorine-containing liquid, the mixture is stirred slowly for 5 min by magnetic force, and after standing for 15 min, the supernatant is taken to detect the fluorine ion concentration to be 3.080 mg/L.
The fluorine-containing liquid is illustrated that after the deep fluorine removal agent provided by the invention is added, the concentration of fluorine ions is reduced from 5.022 mg/L to 3.080 mg/L.
Example 9 (wastewater defluorination)
In a sulfuric acid workshop of a super-huge type copper smelting plant, taking 400 mL of water sample (pH is about 6) of desulfurized gypsum post-liquid, detecting that the fluorine ion is 5.022 mg/L, and using sulfuric acid (H) 2 SO 4 ) Adjusting the pH value of the liquid to 3, adding 0.2mL of prepared deep defluorination agent into the acidic fluorine-containing liquid, magnetically stirring for 5 min at a slow speed, standing for 15 min, and taking supernatant to detect that the concentration of fluorine ions is 3.444 mg/L.
The fluorine-containing liquid is illustrated that after the deep fluorine removal agent provided by the invention is added, the fluorine ion concentration is reduced from 5.022 mg/L to 3.444 mg/L.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications, equivalents and direct/indirect applications in the technical field related to the present invention are included in the scope of the present invention.

Claims (10)

1. The deep defluorination medicament is characterized by comprising 1-5% of yttrium oxide or yttrium carbonate, 1-5% of aluminum oxide or aluminum hydroxide, 1-5% of cerium oxide or cerium carbonate, 1-5% of ferric oxide or ferric sulfate, 1-5% of samarium oxide or samarium carbonate, 0.5-2% of calcium oxide or calcium hydroxide, 1-3% of sulfuric acid and deionized water in preset percentage content; wherein the sum of the percentage contents of all the components is 100%.
2. A method for preparing the deep fluorine removal agent of claim 1, comprising the steps of:
heating and stirring deionized water, yttrium oxide or yttrium carbonate, aluminum oxide or aluminum hydroxide, cerium oxide or cerium carbonate, iron oxide or ferric sulfate, samarium oxide or samarium carbonate to form a mixed solution, wherein when the temperature of the mixed solution reaches a first preset temperature range, the heating and the stirring are stopped;
adding the deionized water into the mixed solution again, and then adding sulfuric acid into the mixed solution under stirring until the pH value of the mixed solution is less than 1;
adding calcium oxide or calcium hydroxide into the mixed solution under stirring until the pH value of the mixed solution reaches 3;
and cooling the mixed solution to a second preset temperature range, and filtering to remove sediments in the mixed solution to obtain the deep fluorine removal medicament.
3. The method for preparing a deep fluorine chemical according to claim 2, wherein the sulfuric acid is commercially available in the form of liquid.
4. The method according to claim 2, wherein any one of the yttrium oxide or the yttrium carbonate, the aluminum oxide or the aluminum hydroxide, the cerium oxide or the cerium carbonate, the iron oxide or the iron sulfate, the samarium oxide or the samarium carbonate, and the calcium oxide or the calcium hydroxide is commercially available in industrial grade and in solid form.
5. The method of claim 2, wherein the first predetermined temperature range is 70 ℃ to 100 ℃.
6. The method of claim 5 wherein the temperature is raised to a level not exceeding 5 ℃ per minute during the heating and stirring.
7. The method of claim 5 wherein the stirring speed during the heating and stirring is 1500 rpm.
8. The method of claim 2, wherein the second predetermined temperature is in a range of 20 ℃ to 30 ℃.
9. The method for preparing the deep fluorine removal agent as claimed in claim 2, wherein the deionized water is added into the mixed solution again, then the sulfuric acid is added with stirring until the pH value of the mixed solution is less than 1, the pH value is required to be kept below 1, and the next step is not carried out until the mixed solution is stirred for 10-15 minutes.
10. A method of using the deep fluorine removal agent as claimed in claim 1, comprising the steps of:
weighing the deep defluorinating agent in a corresponding proportion according to the concentration of fluorine ions in the wastewater to be treated;
adding the deep defluorination agent into the wastewater, uniformly stirring and mixing to obtain a treatment solution, and standing the treatment solution within a preset time;
taking supernatant in the treatment liquid, and measuring the concentration of fluorine ions in the supernatant;
and when the concentration of the fluorine ions in the supernatant reaches the discharge requirement, discharging the filtered treatment liquid outwards.
CN202210791944.XA 2022-07-07 2022-07-07 Deep defluorination medicament and preparation method and use method thereof Active CN114853109B (en)

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