CN114684903B - Preparation method of inorganic-organic reinforced dephosphorization flocculant and wastewater treatment method - Google Patents
Preparation method of inorganic-organic reinforced dephosphorization flocculant and wastewater treatment method Download PDFInfo
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- CN114684903B CN114684903B CN202210365641.1A CN202210365641A CN114684903B CN 114684903 B CN114684903 B CN 114684903B CN 202210365641 A CN202210365641 A CN 202210365641A CN 114684903 B CN114684903 B CN 114684903B
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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
- C02F1/52—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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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Abstract
The application belongs to the technical field of flocculating agents for water treatment, and particularly relates to a preparation method of an inorganic-organic reinforced dephosphorization flocculating agent and a wastewater treatment method, comprising the following steps of adding a polyacrylamide solution into a diatomite solution loaded with modified polymeric ferric sulfate, controlling the temperature to be 50-90 ℃, reacting for a period of time, and regulating the pH value to be 1.5-4.2 to obtain the dephosphorization flocculating agent; the preparation method of the diatomite solution loaded with the modified polymeric ferric sulfate comprises the steps of mixing the polymeric ferric sulfate solution with a silane coupling agent, and reacting to obtain the modified polymeric ferric sulfate; then adding the modified polymeric ferric sulfate into diatomite, carrying out ultrasonic treatment, and carrying out water bath heating treatment to obtain a diatomite solution loaded with the modified polymeric ferric sulfate; the dephosphorization flocculant has the advantages of higher suspended matter removal rate and total phosphorus removal rate, higher suspended matter sedimentation speed and better sewage treatment effect.
Description
Technical Field
The application belongs to the technical field of flocculating agents for water treatment, and particularly relates to a preparation method of an inorganic-organic reinforced dephosphorization flocculating agent and a wastewater treatment method.
Background
The development of industry brings about serious water eutrophication problem, and phosphorus is the main cause of water eutrophication, so wastewater dephosphorization is one of the most challenging problems facing the field of human water resource management, phosphorus in sewage is partially sourced from chemical fertilizers and agricultural wastes, and meanwhile, the content of phosphorus in domestic sewage is obviously increased due to the large-scale use of phosphorus-containing detergents in life.
At present, one of the most effective methods for removing phosphorus in wastewater is to use a flocculant for chemical phosphorus removal, but due to the fact that the total phosphorus content in some wastewater is high, the total phosphorus content cannot be sufficiently reduced by using a traditional flocculant to reach national emission standards, or a large amount of flocculant is needed to reduce the total phosphorus content of effluent, which also tends to increase the production cost of enterprises.
The patent application number 201910311682.0 discloses a solid inorganic-organic covalent bond type hybrid flocculant, a preparation method and application thereof, wherein the inorganic-organic covalent bond type hybrid flocculant is mainly prepared by polymerizing an organosilicon coupling agent and aluminum salt or ferric salt by adding alkali. The preparation method comprises the following steps: (1) Dissolving aluminum salt or ferric salt in a reaction kettle to obtain a solution with the concentration (mass ratio) of less than or equal to 30%; (2) Then, adding a silane coupling agent into the solution obtained in the step (1) according to the silicon-aluminum ratio or silicon-iron ratio (molar ratio) of 0.001-200, and stirring and reacting for 0.5-24h at the temperature of 5-85 ℃; (3) Finally, adding sodium hydroxide according to the hydroxyl aluminum ratio (OH/Al molar ratio) or hydroxyl iron ratio (OH/Fe molar ratio) of 0-2.5, stirring and reacting for 0.5-24h to obtain the liquid inorganic-organic covalent bond type hybrid flocculant, wherein the nitrate nitrogen removal rate is 40-90%, and the total phosphorus removal rate is 90-99%.
The patent application number 201911307611.X discloses a papermaking sewage treatment agent, a preparation method and application thereof, wherein the flocculant comprises the following components in parts by weight: 5-10 parts of polymeric ferric sulfate, 10-15 parts of polymeric ferric silicate, 10-15 parts of chitosan, 20-30 parts of sodium alginate, 5-10 parts of slaked lime, 5-10 parts of polyacrylamide and 1-2 parts of acetic acid.
The preparation method comprises (1) dissolving 8 parts of chitosan in 2 parts of acetic acid aqueous solution to obtain chitosan solution, and adding 28 parts of sodium alginate into the chitosan solution to obtain a first mixed solution. (2) Adding 9 times of absolute ethyl alcohol with the mass being the 4 raw materials into 8 parts of polymeric ferric sulfate, 13 parts of polymeric ferric silicate, 6 parts of slaked lime and 8 parts of polyacrylamide, and carrying out ultrasonic treatment at 85 ℃ for 50min with the ultrasonic power being 850W to obtain an ultrasonic treatment mixture; (2) Mixing the first mixed solution and the second mixed solution, performing high-temperature microwave treatment for 2-6 h at 180 ℃, drying, grinding and sieving to obtain the flocculant. It is mainly used for treating heavy metal ions in papermaking wastewater.
Disclosure of Invention
The application aims to solve the technical problems of providing an inorganic-organic reinforced dephosphorization flocculant, a preparation method and a wastewater treatment method.
The application relates to a preparation method of an inorganic-organic reinforced dephosphorization flocculant, which comprises the following steps,
adding polyacrylamide solution into diatomite solution loaded with modified polymeric ferric sulfate, controlling the temperature to be 50-90 ℃, reacting for a period of time (preferably 0.5-1 h), and adjusting the pH value to be 1.5-4.2 (preferably adjusting the pH value by adopting sodium bicarbonate) to obtain an inorganic-organic reinforced dephosphorizing flocculant;
the preparation method of the diatomite solution loaded with the modified polymeric ferric sulfate comprises the steps of mixing the polymeric ferric sulfate solution with a silane coupling agent, and reacting (the reaction time is preferably 3-5 h) to obtain the modified polymeric ferric sulfate; then adding the modified polymeric ferric sulfate into diatomite, carrying out ultrasonic treatment and water bath heating treatment to obtain the diatomite solution loaded with the modified polymeric ferric sulfate.
The mass volume ratio of the diatomite to the modified polymeric ferric sulfate is 1-3 g/100 ml.
Preferably, the polymeric ferric sulfate solution is a mixture of liquid polymeric ferric sulfate and water, and the volume ratio of the liquid polymeric ferric sulfate to the water is 1-3:1.
Preferably, the mass ratio of the silane coupling agent to the iron element in the polymeric ferric sulfate solution is 1-3:6.
Preferably, the silane coupling agent is one or more of vinyl trimethoxy silane, vinyl triethoxy silane, vinyl tri (2-methoxyethoxy) silane and vinyl triacetoxy silane.
Preferably, the ultrasonic power of the ultrasonic treatment is 300W-600W.
Preferably, the temperature of the water bath heating treatment is 40-60 ℃ (the water bath time is generally 0.5-1 h).
Preferably, the polyacrylamide solution is added dropwise to the modified polymeric ferric sulfate loaded diatomite solution.
Preferably, the mass fraction of the polyacrylamide solution is 0.5%.
Preferably, the mass ratio of the polyacrylamide to the iron element in the polymeric ferric sulfate solution is 0.2-0.6:100.
The application provides a wastewater treatment method, which comprises the steps of adding the inorganic-organic reinforced dephosphorization flocculant obtained by the preparation method into wastewater to be treated.
The application has the beneficial effects that the silicon alkoxy of the silane coupling agent has reactivity to inorganic matters, and the organic functional group has reactivity or compatibility to organic matters, so that when the silane coupling agent is between inorganic and organic interfaces, a bonding layer of an organic matrix, the silane coupling agent and the inorganic matrix can be formed.
The diatomite carrier has adsorption agglomeration effect, and various metal substances in the diatomite can interact with the polymeric ferric sulfate to form a three-dimensional reticular macromolecular polymer with various valence bond structures, so that the composite flocculant is beneficial to exerting adsorption bridging and rolling sweeping functions, and the adhesion bridging capacity of the modified polymeric ferric sulfate loaded with the diatomite is improved.
The synthesized inorganic-organic reinforced dephosphorizing flocculant not only has the characteristics of high-density positive charge carried by the inorganic flocculant and high molecular weight of the organic flocculant, but also enhances the functions of integral adsorption bridging and rolling sweeping through loading diatomite, and the applicable pH range is between 4 and 11.
According to the application, sodium bicarbonate is selected to adjust the pH value to be between 1.5 and 4.2, the basicity of a target product can be controlled to be between 6 and 8 percent, phosphate in wastewater is easy to react with free iron ions to generate ferric phosphate precipitates, and if the basicity is too high, more hydroxide ions are combined with the iron ions to form ferric hydroxide, so that the free iron ions are less, and the dephosphorization effect is poor.
The inorganic-organic reinforced dephosphorizing flocculant synthesized by the application has the removal rate of suspended matters and phosphorus elements in urban, industrial and domestic sewage as high as 95.96 percent and 98.82 percent respectively.
Detailed Description
The application provides an inorganic-organic reinforced dephosphorization flocculant and a preparation method thereof, which are used for solving the problems of dephosphorization cost and effect. The following description of the embodiments of the present application will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
100mL of liquid polymeric ferric sulfate with 10% total iron content is mixed with 100mL of distilled water, 3g of silane coupling agent (vinyl trimethoxy silane) is added, then stirring reaction is carried out for 3 hours at room temperature, 2g of diatomite is added, then the mixture is transferred to an ultrasonic cleaning instrument, ultrasonic power is adjusted to 300W by opening ultrasonic, the water bath temperature is increased to 50 ℃, and load reaction is carried out for 0.5 hour. Slowly dripping the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to iron element in the liquid polymeric ferric sulfate is 0.3:100, controlling the temperature at 60 ℃, reacting for 0.5h at constant temperature, adjusting the pH value to 2.0 by using sodium bicarbonate, and standing for 2h at room temperature to obtain the target product.
Example 2
After 100mL of liquid polymeric ferric sulfate with 10% total iron content is mixed with 100mL of distilled water, 3.1g of silane coupling agent (vinyl trimethoxy silane) is added, then stirring reaction is carried out for 4 hours at room temperature, 2g of diatomite is added, the mixture is transferred to an ultrasonic cleaning instrument, ultrasonic power is adjusted to 300W by opening ultrasonic, the water bath temperature is raised to 55 ℃, and load reaction is carried out for 1 hour. Slowly dripping the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to iron element in the liquid polymeric ferric sulfate is 0.35:100, controlling the temperature at 65 ℃, reacting for 1h at constant temperature, adjusting the pH value to 2.5 by using sodium bicarbonate, and standing for 2h at room temperature to obtain the target product.
Example 3
100mL of liquid polymeric ferric sulfate with 10% total iron content is mixed with 100mL of distilled water, 3.2g of silane coupling agent (vinyl trimethoxy silane) is added, then the mixture is stirred at room temperature for reaction for 4 hours, 2.5g of diatomite is added, the mixture is transferred to an ultrasonic cleaning instrument, ultrasonic power is adjusted to 300W by opening ultrasonic waves, the water bath temperature is increased to 50 ℃, and load reaction is carried out for 1 hour. Slowly dripping the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to iron element in the liquid polymeric ferric sulfate is 0.4:100, controlling the temperature at 75 ℃, reacting for 1h at constant temperature, adjusting the pH value to 3.0 by using sodium bicarbonate, and standing for 2h at room temperature to obtain the target product.
Comparative example 1
After mixing 100mL of 10% total iron content liquid polymeric ferric sulfate with 100mL of distilled water, 2g of diatomaceous earth was added and the water bath temperature was raised to 50 ℃. Slowly dripping the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to iron element in the liquid polymeric ferric sulfate is 0.3:100, controlling the temperature at 60 ℃, reacting for 0.5h at constant temperature, adjusting the pH value to 2.0 by using sodium bicarbonate, and standing for 2h at room temperature to obtain the target product.
Comparative example 2
After 100mL of liquid polymeric ferric sulfate with 10% total iron content is mixed with 100mL of distilled water, 3g of silane coupling agent (vinyl trimethoxysilane) is added, then stirring is carried out at room temperature for 3h, 2g of kieselguhr and 0.5% mass fraction of PAM aqueous solution are added, and the mass ratio of PAM to iron element in the liquid polymeric ferric sulfate is 0.3:100. Transferring to an ultrasonic cleaning instrument, opening ultrasonic to adjust ultrasonic power to 300W, heating the water bath temperature to 60 ℃, carrying out load reaction for 1h, adjusting the pH value to 2.0 by using sodium bicarbonate, and standing at room temperature for 2h to obtain a target product. The mass ratio of PAM to iron is 0.3:100.
Comparative example 3
100mL of liquid polymeric ferric sulfate with 10% total iron content is mixed with 100mL of distilled water, 3g of silane coupling agent (vinyl trimethoxy silane) is added, then stirring reaction is carried out for 3 hours at room temperature, 2g of diatomite is added, then the mixture is transferred to an ultrasonic cleaning instrument, ultrasonic power is adjusted to 300W by opening ultrasonic, the water bath temperature is increased to 50 ℃, and load reaction is carried out for 0.5 hour. Slowly dripping the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to iron element in the liquid polymeric ferric sulfate is 0.3:100, controlling the temperature at 60 ℃, reacting for 0.5h at constant temperature, adjusting the pH value to 5.0 by using sodium bicarbonate, and standing for 2h at room temperature to obtain the target product.
The dephosphorization-flocculation performance evaluation was performed using the dephosphorization flocculants prepared in examples 1 to 3 and comparative examples 1 to 3 described above.
Adding 1%inorganic-organic reinforced dephosphorizing flocculant into a certain amount of phosphorus-containing industrial sewage under slow stirring, then continuously stirring the solution slowly for 2min, standing for 20min, observing the formation speed, the size of flocs and the sinking speed of the flocs, measuring suspended matters and phosphorus content in supernatant by a gravimetric method and an ammonium molybdate spectrophotometry respectively, and comparing under the same experimental conditions, wherein the result is shown in table 1.
TABLE 1 effect of treating industrial wastewater
The experimental process shows that when 1 per mill of the inorganic-organic reinforced dephosphorization flocculant of the examples 1-3 is respectively added into certain industrial sewage, the volume of alum blossom in the sewage is larger, and the supernatant water quality becomes clear and bright after 20 minutes of sedimentation.
As shown in Table 1, the dephosphorization flocculant synthesized by the above example has remarkable removal effect on suspended matters and phosphorus, the suspended matters removal rate can reach 95.96%, and the total phosphorus removal rate can reach 98.82%. Although comparative examples 1 to 2 also had a certain effect of removing suspended matters and phosphorus, the volume of alum blossom was small, the settling rate of suspended matters was slow, and after settling for 50 minutes, the supernatant still had fine flocs which were difficult to settle. Comparative example 1 was conducted in a simple mixed solution without adding a silane coupling agent, and the suspended matter and phosphorus element removal rates were 76.85% and 77.40%, respectively; compared with the example 1, the comparative example 2 has the advantages that diatomite and PAM are simultaneously added with the modified polyferric solution and then subjected to ultrasonic reaction, the reaction effect is poor, and the measured suspended matters and the phosphorus element removal rate are respectively 85.43% and 88.03%, which are obviously lower than the phosphorus removal flocculant synthesized by the application. Comparative example 3 in comparison with example 1, the pH was adjusted to 5.0 with sodium bicarbonate to a value exceeding 1.5-4.2, under which conditions the iron ions of the product combined with more hydroxide ions to form ferric hydroxide, resulting in less free iron ions and poor phosphorus removal, with suspended solids and phosphorus removal rates of 91.05% and 89.58%, respectively.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of protection of the application is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the application, the steps may be implemented in any order and there are many other variations of the different aspects of one or more embodiments of the application as described above, which are not provided in detail for the sake of brevity.
One or more embodiments of the present application are intended to embrace all such alternatives, modifications and variations as fall within the broad scope of the present application. Accordingly, any omissions, modifications, equivalents, improvements and others which are within the spirit and principles of the one or more embodiments of the application are intended to be included within the scope of the application.
Claims (8)
1. A preparation method of an inorganic-organic reinforced dephosphorization flocculant is characterized by comprising the following steps,
adding polyacrylamide solution into diatomite solution loaded with modified polymeric ferric sulfate, controlling the temperature to be 50-90 ℃, reacting for a period of time, and adjusting the pH value to be 1.5-4.2 to obtain an inorganic-organic reinforced dephosphorizing flocculant;
the preparation method of the diatomite solution loaded with the modified polymeric ferric sulfate comprises the steps of mixing the polymeric ferric sulfate solution with a silane coupling agent, and reacting to obtain the modified polymeric ferric sulfate; then adding the modified polymeric ferric sulfate into diatomite, carrying out ultrasonic treatment, and carrying out water bath heating treatment to obtain a diatomite solution loaded with the modified polymeric ferric sulfate; the mass ratio of the silane coupling agent to the iron element in the polymeric ferric sulfate solution is 1-3:6; the mass ratio of the iron element in the polyacrylamide to the polymeric ferric sulfate solution is 0.2-0.6:100; the regulator for regulating the pH value is sodium bicarbonate.
2. The method of claim 1, wherein the polymeric ferric sulfate solution is a mixture of liquid polymeric ferric sulfate and water in a volume ratio of 1-3:1.
3. The method of claim 1, wherein the silane coupling agent is one or more of vinyltrimethoxysilane, vinyltriethoxysilane, vinyltris (2-methoxyethoxy) silane, vinyltriacetoxysilane.
4. The method of claim 1, wherein the ultrasonic power of the ultrasonic treatment is 300W to 600W.
5. The method according to claim 1, wherein the water bath heating treatment is carried out at a temperature of 40 to 60 ℃.
6. The method of claim 1, wherein the polyacrylamide solution is added dropwise to the modified polymeric ferric sulfate loaded diatomaceous earth solution.
7. The preparation method as claimed in claim 1, wherein the mass fraction of the polyacrylamide solution is 0.5%.
8. A wastewater treatment method, characterized in that the inorganic-organic reinforced dephosphorization flocculant obtained by the preparation method according to any one of claims 1 to 7 is added into wastewater to be treated.
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| US20090107919A1 (en) * | 2007-10-31 | 2009-04-30 | Chevron U.S.A. Inc. | Apparatus and process for treating an aqueous solution containing chemical contaminants |
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