CN114684903A - Preparation method of inorganic-organic enhanced phosphorus removal flocculating agent and wastewater treatment method - Google Patents
Preparation method of inorganic-organic enhanced phosphorus removal flocculating agent and wastewater treatment method Download PDFInfo
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- CN114684903A CN114684903A CN202210365641.1A CN202210365641A CN114684903A CN 114684903 A CN114684903 A CN 114684903A CN 202210365641 A CN202210365641 A CN 202210365641A CN 114684903 A CN114684903 A CN 114684903A
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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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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention belongs to the technical field of flocculating agents for water treatment, and particularly relates to a preparation method of an inorganic-organic enhanced phosphorus removal flocculating agent and a wastewater treatment method, which comprises 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 adjusting the pH value to be 1.5-4.2 to obtain the phosphorus removal 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; adding the modified polymeric ferric sulfate into diatomite, performing ultrasonic treatment and water bath heating treatment to obtain a diatomite solution loaded with the modified polymeric ferric sulfate; by using the phosphorus removal flocculant, the removal rate of suspended matters and the removal rate of total phosphorus are both high, the settling velocity of the suspended matters is higher, and the sewage treatment effect is better.
Description
Technical Field
The invention belongs to the technical field of flocculants for water treatment, and particularly relates to a preparation method of an inorganic-organic enhanced phosphorus removal flocculant and a wastewater treatment method.
Background
The industrial development brings about a serious problem of water eutrophication, and phosphorus is a main reason causing the water eutrophication, so that the phosphorus removal from wastewater is one of the most challenging problems in the field of human water resource management, the phosphorus in the wastewater is partially derived from chemical fertilizers and agricultural wastes, and meanwhile, the content of the phosphorus in the domestic wastewater is remarkably increased due to the large use of phosphorus-containing detergents in life.
At present, one of the most effective methods for removing phosphorus from wastewater is to use a flocculating agent to remove phosphorus chemically, but because the total phosphorus content in some wastewater is higher, the total phosphorus content cannot be reduced sufficiently by using a traditional flocculating agent to reach the national discharge standard, or the total phosphorus content in effluent can be reduced by using a large amount of flocculating agent, which often means that the production cost of an enterprise is increased.
The patent application number 201910311682.0 discloses a solid inorganic-organic covalent bond type hybrid flocculant and a preparation method and application thereof, wherein the inorganic-organic covalent bond type hybrid flocculant is mainly prepared by polymerizing an organic silicon coupling agent and aluminum salt or ferric salt through 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) 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 the silicon-iron ratio (molar ratio) of 0.001-200, and stirring and reacting for 0.5-24 hours at the temperature of 5-85 ℃; (3) and 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 removal rate of nitric and nitrogen is 40-90%, and the removal rate of total phosphorus is 90-99%.
The patent application number of 201911307611.X discloses a papermaking sewage treatment agent, a preparation method and an application thereof, wherein the flocculant comprises the following components in parts by weight: 5-10 parts of polymeric ferric sulfate, 10-15 parts of polysilicate iron, 10-15 parts of chitosan, 20-30 parts of sodium alginate, 5-10 parts of hydrated 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 water solution to obtain chitosan solution, and adding 28 parts of sodium alginate into the chitosan solution to obtain a first mixed solution. (2) Adding absolute ethyl alcohol with the mass 9 times of that of the 4 raw materials into 8 parts of polymeric ferric sulfate, 13 parts of ferric polysilicate, 6 parts of hydrated lime and 8 parts of polyacrylamide, and performing ultrasonic treatment at 85 ℃ for 50min with the ultrasonic power of 850W to obtain an ultrasonic treatment mixture; (2) and mixing the first mixed solution and the second mixed solution, performing high-temperature microwave treatment at 180 ℃ for 2-6 hours, drying, grinding and sieving to obtain the flocculant. It mainly treats heavy metal ions in the papermaking wastewater.
Disclosure of Invention
The invention aims to solve the technical problems of providing an inorganic-organic enhanced phosphorus removal flocculant, a preparation method and a wastewater treatment method.
The invention relates to a preparation method of an inorganic-organic enhanced phosphorus removal flocculating agent, which comprises the following steps,
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 (preferably 0.5-1h), and adjusting the pH value to be 1.5-4.2 (preferably adjusting the pH value by using sodium bicarbonate) to obtain an inorganic-organic enhanced phosphorus removal 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 3-5h) to obtain the modified polymeric ferric sulfate; and adding the modified polyferric sulfate into the diatomite, performing ultrasonic treatment and water bath heating treatment to obtain the diatomite solution loaded with the modified polyferric sulfate.
The mass volume ratio of the diatomite to the modified polymeric ferric sulfate is 1-3g: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 vinyltrimethoxysilane, vinyltriethoxysilane, vinyltris (2-methoxyethoxy) silane and vinyltriacetoxysilane.
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 into the diatomite solution loaded with the modified polymeric ferric sulfate in a dropwise manner.
Preferably, the mass fraction of the polyacrylamide solution is 0.5%.
Preferably, the mass ratio of the iron element in the polyacrylamide and polyferric sulfate solution is 0.2-0.6: 100.
The invention provides a wastewater treatment method which comprises the step of adding the inorganic-organic enhanced phosphorus removal flocculating agent obtained by the preparation method into wastewater to be treated.
The invention has the advantages that the silane oxygen group 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 an inorganic interface and an organic interface, a bonding layer of an organic matrix-the silane coupling agent-an inorganic matrix can be formed.
The diatomite carrier has an adsorption and agglomeration effect, and various metal substances in the diatomite can interact with the polyferric sulfate to form a three-dimensional network macromolecular polymer with various valence bond structures, so that the composite flocculant can perform the functions of adsorption bridging and rolling sweeping, and the adhesion bridging capacity of the modified polyferric sulfate loaded with the diatomite is improved.
The synthesized inorganic-organic enhanced phosphorus removal flocculant not only has the characteristics of high-density positive charges carried by the inorganic flocculant and high molecular weight of the organic flocculant, but also enhances the functions of integral adsorption bridging and sweeping by loading diatomite, and has the applicable pH range of 4-11.
According to the method, the pH value is adjusted to be between 1.5 and 4.2 by using the sodium bicarbonate, the basicity of the target product can be controlled to be between 6 and 8 percent, phosphate in the wastewater can easily react with free iron ions to generate iron phosphate precipitates, and the iron ions are combined with more hydroxide ions to form ferric hydroxide when the basicity is too high, so that less free iron ions are generated, and the phosphorus removal effect is poor.
The inorganic-organic enhanced phosphorus removal flocculant synthesized by the method has removal rates of 95.96% and 98.82% for suspended matters and phosphorus elements in urban, industrial and domestic sewage respectively.
Detailed Description
The invention provides an inorganic-organic enhanced phosphorus removal flocculating agent and a preparation method thereof, which aim to solve the problems of cost and effect of phosphorus removal. 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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Mixing 100mL of liquid polymeric ferric sulfate with 10% of total iron content and 100mL of distilled water, adding 3g of silane coupling agent (vinyl trimethoxy silane), stirring at room temperature for reaction for 3h, adding 2g of diatomite, transferring to an ultrasonic cleaning instrument, turning on ultrasonic to adjust the ultrasonic power to 300W, raising the water bath temperature to 50 ℃, and carrying out load reaction for 0.5 h. Slowly dropwise adding the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to the 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
Mixing 100mL of liquid polymeric ferric sulfate with 10% of total iron content and 100mL of distilled water, adding 3.1g of silane coupling agent (vinyl trimethoxy silane), stirring at room temperature for reaction for 4 hours, adding 2g of diatomite, transferring to an ultrasonic cleaning instrument, turning on ultrasonic to adjust the ultrasonic power to 300W, raising the water bath temperature to 55 ℃, and carrying out load reaction for 1 hour. Slowly dropwise adding the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to the 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
Mixing 100mL of liquid polymeric ferric sulfate with 10% of total iron content and 100mL of distilled water, adding 3.2g of silane coupling agent (vinyl trimethoxy silane), stirring at room temperature for reaction for 4 hours, adding 2.5g of diatomite, transferring to an ultrasonic cleaning instrument, turning on ultrasonic to adjust the ultrasonic power to 300W, raising the water bath temperature to 50 ℃, and carrying out load reaction for 1 hour. Slowly and dropwise adding the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to iron element in the liquid polyferric 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
100mL of liquid polymeric ferric sulfate having 10% total iron content was mixed with 100mL of distilled water, 2g of diatomaceous earth was added, and the temperature of the water bath was raised to 50 ℃. Slowly and dropwise adding the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to iron element in the liquid polyferric sulfate is 0.3:100, controlling the temperature at 60 ℃, reacting at constant temperature for 0.5h, adjusting the pH value to 2.0 by using sodium bicarbonate, and standing at room temperature for 2h to obtain the target product.
Comparative example 2
Mixing 100mL of liquid polymeric ferric sulfate with 10% of total iron content and 100mL of distilled water, then adding 3g of silane coupling agent (vinyl trimethoxy silane), stirring at room temperature for reaction for 3h, adding 2g of diatomite and 0.5% of PAM aqueous solution by mass fraction, wherein the mass ratio of PAM to iron element in the liquid polymeric ferric sulfate is 0.3: 100. Transferring the mixture into an ultrasonic cleaning instrument, turning on the ultrasonic to adjust the ultrasonic power to 300W, heating the water bath to 60 ℃, carrying out load reaction for 1h, adjusting the pH value to 2.0 by using sodium bicarbonate, and standing the mixture at room temperature for 2h to obtain the target product. The mass ratio of PAM to iron is 0.3: 100.
Comparative example 3
Mixing 100mL of liquid polymeric ferric sulfate with 10% of total iron content and 100mL of distilled water, adding 3g of silane coupling agent (vinyl trimethoxy silane), stirring at room temperature for reaction for 3h, adding 2g of diatomite, transferring to an ultrasonic cleaning instrument, turning on ultrasonic to adjust the ultrasonic power to 300W, raising the water bath temperature to 50 ℃, and carrying out load reaction for 0.5 h. Slowly dropwise adding the prepared PAM aqueous solution with the mass fraction of 0.5%, wherein the mass ratio of PAM to the 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.
Phosphorus removal-flocculation performance evaluation was performed using the phosphorus removal flocculants prepared in examples 1-3 and comparative examples 1-3 described above.
1 per mill of inorganic-organic enhanced phosphorus removal flocculating agent is added into a certain amount of phosphorus-containing industrial sewage under slow stirring, then the solution is continuously and slowly stirred for 2min, the solution is kept stand for 20min, the flocculating agent formation speed, the floc size and the sinking speed are observed, suspended matter and phosphorus content in supernatant are measured by a gravimetric method and an ammonium molybdate spectrophotometry respectively, and meanwhile, comparison is carried out under the same experimental conditions, and the results are shown in table 1.
TABLE 1 certain effect of treating Industrial wastewater
Experimental process shows that when 1 per mill of the inorganic-organic enhanced phosphorus removal flocculating agent in the embodiment 1-3 is added into certain industrial sewage respectively, the volume of alum floc in the sewage is large, and the water quality of supernatant becomes clear and bright after 20min of sedimentation.
As can be seen from Table 1, the phosphorus removal flocculant synthesized by the above example can have a remarkable removal effect on suspended matters and phosphorus, the removal rate of the suspended matters can reach 95.96%, and the removal rate of the total phosphorus can reach 98.82%. Although comparative examples 1-2 also have a certain effect of removing suspended matters and phosphorus, alum floc volume is small, the settling speed of suspended matters is slow, and after settling for 50min, the supernatant still has fine flocs which are difficult to settle. Comparative example 1 compared with example 1, the silane coupling agent is not added, the system is a simple mixed solution, and the removal rates of suspended matters and phosphorus elements are respectively 76.85% and 77.40%; compared with the example 1, the diatomite and the PAM are simultaneously added with the modified polyferric solution and then subjected to the ultrasonic reaction, the reaction effect is poor, and the removal rates of suspended matters and phosphorus elements are respectively 85.43% and 88.03%, which are obviously lower than that of the phosphorus removal flocculant synthesized by the invention. Comparative example 3 with respect to example 1, the PH was adjusted to 5.0 with sodium bicarbonate to exceed 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 suspension and phosphorus removal rates of 91.05% and 89.58%, respectively.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to imply that the scope of the application is limited to these examples; within the context of the present application, features from the above embodiments or from different embodiments may also be combined, steps may be implemented in any order, and there are many other variations of different aspects of one or more embodiments in the present application as described above, which are not provided in detail for the sake of brevity.
The one or more embodiments of the present application are intended to embrace all such alternatives, modifications and variances that fall within the broad scope of the present application. Therefore, any omissions, modifications, substitutions, improvements, and the like that may be made without departing from the spirit and principles of one or more embodiments of the present application are intended to be included within the scope of the present application.
Claims (10)
1. A preparation method of inorganic-organic enhanced phosphorus removal flocculating agent is characterized by comprising the following steps,
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 adjusting the pH value to be 1.5-4.2 to obtain an inorganic-organic enhanced phosphorus removal 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; and adding the modified polyferric sulfate into the diatomite, performing ultrasonic treatment and water bath heating treatment to obtain the diatomite solution loaded with the modified polyferric sulfate.
2. The method according to claim 1, wherein the polyferric sulfate solution is a mixture of liquid polyferric sulfate and water, and the volume ratio of the liquid polyferric sulfate to the water is 1-3: 1.
3. The method according to claim 1, wherein the mass ratio of the silane coupling agent to the iron element in the polymeric ferric sulfate solution is 1-3: 6.
4. The method according to claim 1, wherein the silane coupling agent is one or more selected from the group consisting of vinyltrimethoxysilane, vinyltriethoxysilane, vinyltris (2-methoxyethoxy) silane, and vinyltriacetoxysilane.
5. The method according to claim 1, wherein the ultrasonic power of the ultrasonic treatment is 300W to 600W.
6. The method according to claim 1, wherein the temperature of the water bath heating treatment is 40 to 60 ℃.
7. The method according to claim 1, wherein the polyacrylamide solution is added dropwise to the modified polyferric sulfate-loaded diatomaceous earth solution.
8. The method according to claim 1, wherein the mass fraction of the polyacrylamide solution is 0.5%.
9. The method according to claim 1, wherein the mass ratio of iron in the polyacrylamide and polyferric sulfate solution is 0.2-0.6: 100.
10. A wastewater treatment method, characterized in that the inorganic-organic enhanced phosphorus removal flocculant obtained by the preparation method of any one of claims 1 to 9 is added into wastewater to be treated.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117986902A (en) * | 2024-01-11 | 2024-05-07 | 佛山市中瑞工业材料有限公司 | Long-acting antibacterial antiviral formaldehyde-removing powder and preparation method thereof |
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