CN112158935A - Inorganic polymer phosphorus removal agent and preparation method and application thereof - Google Patents
Inorganic polymer phosphorus removal agent and preparation method and application thereof Download PDFInfo
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- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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Abstract
The invention relates to an environmental pollution treatment material, and particularly discloses an inorganic polymer phosphorus removal agent, and a preparation method and application thereof. According to the invention, by selecting raw materials and optimizing a preparation process, an inorganic polymer phosphorus removal agent with the Ala content of more than 70% and the Alc content of less than 15% is developed and obtained, and the inorganic polymer phosphorus removal agent can be applied to the field of water phosphorus removal. The inorganic polymer phosphorus removing agent provided by the invention has a prefabricated polymerization form, and cannot be rapidly hydrolyzed after being added into a water body, so that the influence on the pH value of the water body is reduced, and the problems of serious corrosion of the existing phosphorus removing agent on equipment and the like are solved. Meanwhile, the inorganic polymer phosphorus removal agent provided by the invention also has the advantages of high phosphorus removal efficiency, stable effluent turbidity, small influence on water chromaticity and the like, and has good popularization and application prospects.
Description
Technical Field
The invention relates to an environmental pollution treatment material, in particular to an inorganic polymer dephosphorizing agent and a preparation method and application thereof.
Background
The aluminum-based inorganic polymer water treatment functional material is a novel inorganic polymer material which is rapidly developed in recent years, has the advantages of wide application, low toxicity, low corrosivity and the like, and is widely applied to various links of water treatment and sludge treatment at present.
According to the research, the aluminum has different occurrence forms of hydrolytic polymerization, wherein the Al2-Al8The low-hydrolysis polymerization forms are called Ala and Al9-Al30The moderately hydrolyzed polymeric forms are referred to as Alb, and the more highly hydrolyzed polymeric forms are referred to as Alc.
It has been found that aluminum-based polymer materials having different forms of occurrence can correspond to different water treatment functions, and therefore, aluminum-based polymer materials having different forms of occurrence can be developed for different water treatment purposes.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide an inorganic polymer phosphorus removal agent, and a preparation method and application thereof.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
in a first aspect, the invention provides a preparation method of an inorganic polymer dephosphorizing agent, which comprises the following steps:
(1) adding aluminum-containing acid solution into a pre-reactor, and adding Ca (OH) into the pre-reactor2Or CaO is reacted;
standing, discharging 40-75% of liquid in the upper part by volume, and adding the rest solid-liquid mixture into a first reactor (reactor 1);
adding industrial hydrochloric acid or a mixed acid of the industrial hydrochloric acid and sulfuric acid into a reactor 1, wherein the adding amount of the industrial hydrochloric acid or the mixed acid is 40-100% (v/v), preferably 45-50% (v/v) of the adding amount of the aluminiferous acid solution;
sealing the reactor 1, heating to 110-130 ℃, and reacting for 2-3 hours;
(2) when the temperature of the reaction liquid obtained in the step (1) is reduced to below 40 ℃, injecting the reaction liquid into a first purification device (purification device 1) through a slurry pump, carrying out diaphragm filter pressing, and adding the liquid obtained after filter pressing into a second reactor (reactor 2);
(3) heating the reactor 2 to 80 ℃, adding caustic alkali or sodium carbonate in batches under the condition of continuous heat preservation, wherein the mass of the total added sodium element is 40-75% (m/m), preferably 60-65% (m/m) of the mass of the aluminum element in the aluminiferous solution, the adding process needs to last for 1.5-2 hours, and the adding is continuously stirred and reacts for more than 1 hour after the adding is finished;
(4) and (4) cooling the reaction liquid obtained in the step (3) to below 40 ℃, injecting the reaction liquid into a second purification device (purification device 2) through a slurry pump, and performing diaphragm filter pressing to obtain a liquid product, namely the inorganic polymer phosphorus removal agent.
Further, in the step (1), Ca (OH) is charged2Or the molar ratio of CaO to aluminum in the aluminiferous acid solution is 1.5: 1-1.8: 1.
Further, in the step (1), the reaction temperature is controlled to be not higher than 80 ℃, and if the reaction is too violent, the addition can be divided into 2-3 times; after all the solid-liquid mixture is added, standing for 30min, discharging liquid with the volume of 40-75% of the upper part, and adding the remaining solid-liquid mixture into the reactor 1 through a slurry pump.
Further, in the step (1), the aluminiferous acid solution is PO with the aluminum content of more than 30g/L4 3-Acid solution accounting for more than 50% of anions.
Further, in the step (1), the concentration of the industrial hydrochloric acid is 25%, and the sulfuric acid proportion in the mixed acid of the industrial hydrochloric acid and the sulfuric acid is less than 10%.
Further, according to specific requirements, in step (1), FeCl can be added into the reactor 13The ferric sulfate or the ferrate-containing acid is used as a reaction additive, the mass of the iron element is controlled not to exceed 20 percent (m/m) of the total mass of the aluminum element in the aluminiferous solution, and the binding capacity of the inorganic polymer phosphorus removal agent and the phosphorus in the water body can be improved to a certain degree. Meanwhile, it should be noted that the inorganic polymer phosphorus removal agent prepared without introducing the reaction additive in the preparation method can be applied to working conditions with special requirements or conditions (for example, Fe cannot be introduced).
Further, in the step (2), after the temperature of the reaction solution obtained in the step (1) is reduced to below 40 ℃, the reaction solution is injected into the purification device 1 through a slurry pump, the reaction solution is squeezed for more than 30 minutes in a diaphragm pressure filtration mode, and the liquid obtained after pressure filtration is added into the reactor 2.
Further, in the step (2), the solid part after pressure filtration by the purification device 1 can be used as a raw material of a phosphate fertilizer, and is conveyed to other processes by a belt for reprocessing or direct application.
Preferably, in the step (3), caustic alkali or sodium carbonate is added in batches, and the mass of the added sodium element is 60-65% (m/m) of the mass of the aluminum element in the aluminiferous solution.
Further, in the step (4), a liquid product is obtained by squeezing for more than 60 minutes in a diaphragm filter pressing mode, the liquid product is cured for more than 2 hours at normal temperature, secondary filter pressing can be performed if precipitates are generated, and the liquid product after filter pressing is the inorganic high-molecular phosphorus removal agent.
In a second aspect, the invention provides an inorganic polymer dephosphorizing agent prepared by the preparation method, and through detection, Al in the inorganic polymer dephosphorizing agent2-Al8The content of Ala in lower hydrolyzed polymeric form is more than 70% of the total content of Al, while the content of Alc in higher hydrolyzed polymeric form is less than 15% of the total content of Al.
In a third aspect, the invention provides an application of the inorganic polymer phosphorus removal agent in phosphorus removal of a water body.
The application is specifically characterized in that the inorganic polymer phosphorus removal agent is added into the phosphorus-containing sewage/wastewater, and the addition amount of the inorganic polymer phosphorus removal agent is 20-200 times of the phosphorus concentration in the water body (the inorganic polymer phosphorus removal agent is related to the initial concentration of phosphorus and the controlled target concentration).
The inorganic polymer phosphorus removal agent provided by the invention can effectively play a role in phosphorus removal, has small influence on the pH and the chromaticity of a water body, and has stable effluent turbidity.
The raw materials or reagents involved in the invention are all common commercial products, and the operations involved are all routine operations in the field unless otherwise specified.
The above-described preferred conditions may be combined with each other to obtain a specific embodiment, in accordance with common knowledge in the art.
The invention has the beneficial effects that:
according to the invention, by selecting raw materials and optimizing a preparation process, an inorganic polymer phosphorus removal agent with the Ala content of more than 70% and the Alc content of less than 15% is developed and obtained, and the inorganic polymer phosphorus removal agent can be applied to the field of water phosphorus removal. The inorganic polymer phosphorus removing agent provided by the invention has a prefabricated polymerization form, and cannot be rapidly hydrolyzed after being added into a water body, so that the influence on the pH value of the water body is reduced, and the problems of serious corrosion of the existing phosphorus removing agent on equipment and the like are solved. Meanwhile, the inorganic polymer phosphorus removal agent provided by the invention also has the advantages of high phosphorus removal efficiency, stable effluent turbidity, small influence on water chromaticity and the like, has good popularization and application prospects, and leads the development progress of the industrial technology.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present disclosure, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a flow chart of a preparation process of the inorganic polymer phosphorus removal agent of the present invention.
FIG. 2 is an Al-Ferron standard curve.
FIG. 3 is a working curve of the Al-Ferron time-by-time complexation colorimetry.
Detailed Description
Preferred embodiments of the present invention will be described in detail with reference to the following examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and alterations of this invention will become apparent to those skilled in the art without departing from the spirit and scope of this invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
This example is intended to illustrate the preparation method of the inorganic polymeric phosphorus removal agent and the inorganic polymeric phosphorus removal agent obtained by the preparation method.
As shown in the process flow diagram of fig. 1, the specific preparation method comprises the following steps:
(1) adding PO with aluminum content greater than 30g/L4 3-Occupy anionMore than 50 percent of aluminiferous acid solution (raw material 1) is injected into a pre-reactor, and then Ca (OH) is added2The reaction is carried out by adding Ca (OH)2The molar ratio of the aluminum to the aluminum in the aluminum-containing acid solution is 1.5: 1. When in adding, the reaction temperature is controlled not to be higher than 80 ℃, if the reaction is too violent, the adding is divided into 2-3 times; after the solid-liquid mixture is completely added, standing for 30min, discharging liquid with the volume of 60% of the upper part, and adding the remaining solid-liquid mixture into the reactor 1 through a slurry pump;
adding 25% industrial hydrochloric acid (raw material 2) to the reactor 1 in an amount of 45% (v/v) based on the amount of the aluminiferous solution;
adding FeCl to reactor 13Ferric sulfate or ferrate-containing acid is taken as a reaction additive, and the adding amount of iron is controlled to be 10 percent (m/m) of the mass of aluminum in the aluminiferous acid solution;
sealing the reactor 1, heating to 110-130 ℃, and reacting for 2-3 hours;
(2) when the temperature of the reaction liquid obtained in the step (1) is reduced to below 40 ℃, the reaction liquid is injected into the purification device 1 through a slurry pump, the reaction liquid is subjected to filter pressing for more than 30 minutes in a diaphragm filter pressing mode, and the liquid obtained after the filter pressing is added into the reactor 2;
(3) heating the reactor 2 to 80 ℃, adding caustic alkali (raw material 3) in batches under the condition of continuous heat preservation, wherein the mass of the total added sodium element is 60 percent (m/m) of the mass of the aluminum element in the aluminiferous solution, the adding process needs to last for 1.5 hours, and the adding is continuously stirred and reacts for more than 1 hour after the adding is finished;
(4) and (4) cooling the reaction liquid obtained in the step (3) to below 40 ℃, injecting the reaction liquid into the purification device 2 through a slurry pump, squeezing for more than 60 minutes in a diaphragm filter pressing mode to obtain a liquid product, and curing at normal temperature for more than 2 hours (no precipitation occurs), thus obtaining the inorganic polymer phosphorus removal agent.
Example 2
This example differs from example 1 in that Ca (OH)2The molar ratio of the added CaO to the aluminum in the aluminiferous solution was 1.5:1 instead of CaO.
Example 3
The difference between this example and example 1 is that the industrial hydrochloric acid was replaced with a mixed acid of industrial hydrochloric acid and sulfuric acid, and the sulfuric acid ratio in the mixed acid was less than 10%. In the reaction step (1), the adding amount of the acid liquor is adjusted to 50% of the volume of the aluminiferous acid liquor.
Example 4
This example differs from example 1 in the Ca (OH) charged2The molar ratio of the aluminum to the aluminum in the aluminum-containing acid solution is 1.8: 1.
Example 5
This example differs from example 1 in that sodium carbonate is used instead of caustic soda, and the mass of sodium element added is 65% (m/m) of the mass of aluminum element in the aluminiferous solution.
Example 6
This example differs from example 1 in that in step (1), no FeCl is added to reactor 13And a reaction additive such as ferric sulfate or ferrate, and the other steps are the same as the steps in the example 1.
Experimental example 1
In this experimental example, the inorganic polymer phosphorous removal agent prepared in examples 1 to 6 was subjected to an Al-Ferron time-by-time colorimetric method to determine the occurrence of aluminum, and the detection method was as follows:
1) preparation of Ferron colorimetric solution
And mixing the following reagent A, reagent B and reagent C according to the ratio of 2.5:2:1 (adding the reagent A at last) to obtain the Ferron colorimetric solution. The pH of the solution after preparation was about 5.2, and the solution was stored in a refrigerator (4 ℃ C.).
Reagent a [ 0.2% (m/v) Ferron aqueous solution ]: to 1000mL of deionized water boiled and cooled to room temperature was added 2.0g of analytically pure Ferron reagent, the Ferron was dissolved by magnetic stirring, and insoluble impurities were filtered, and then transferred to a 1L volumetric flask for storage in a refrigerator.
Reagent B [ 20% (m/v) NaAc solution ]: 50g of analytically pure anhydrous NaAc is dissolved in a proper amount of deionized water, and the solution is filtered and then transferred into a 250mL volumetric flask to be diluted to a scale mark for constant volume.
Reagent C [ 10% dilute hydrochloric acid ]: 100mL of analytically pure concentrated hydrochloric acid is dissolved in a proper amount of water, and then the solution is transferred into a 1000mL volumetric flask to be diluted to a constant volume of a scale mark.
2) Preparation of standard stock solutions for aluminum
Soaking a certain amount of pure aluminum sheet in dilute hydrochloric acid for 2-4h, taking out, quickly drying with nitrogen, accurately weighing 1.35g (accurate to 0.0002g), adding HCl solution (1:1) for dissolving, and fixing the volume to 500mL, wherein the concentration is 0.1000M.
3) Preparation of Standard Curve
10mL of aluminum stock solution was diluted into a 1.0L volumetric flask to prepare a 10. sup. th concentration-3mol/L Al standard solution. 0.5 mL, 1.0 mL, 1.5 mL, 2.0 mL and 2.5mL of Al standard solution are respectively added into a 25mL colorimetric tube, 5.5mL of colorimetric solution is added, and the absorbance is determined after the volume is constant to 25 mL. The absorbance values of samples with different concentrations at the position of 366nm are plotted into a standard curve, and an Al-Ferron standard curve is shown in figure 2.
4) Time-by-time colorimetric method of Al-Ferron
Adding 5.5mL of prepared Ferron colorimetric solution into a 25mL colorimetric tube, diluting deionized water to a constant volume of 25mL, and adding a trace amount of solution to be detected (the addition amount is related to the total aluminum concentration of the solution to be detected, and the amount of aluminum added into the colorimetric tube is controlled to be 0.5-2.5 x 10-6mol), timing, quickly shaking, placing the cuvette containing the sample in a spectrophotometer, and measuring the absorbance value (i.e. Ala component) at 2 min; the absorbance values (i.e. the components of Ala + Alb) were measured fixed-point at 2 h; the Alc values were calculated as AlT ═ Ala + Alb + Alc. The working curve of the Al-Ferron time-lapse complexation colorimetry is shown in FIG. 3.
According to the above detection method, the inorganic polymer phosphorus removing agent prepared in examples 1 to 6 was subjected to an Al-Ferron time-by-time colorimetry to determine the occurrence form of aluminum, and the detection results are shown in table 1:
TABLE 1 occurrence of aluminum in inorganic polymer phosphorus removing agents prepared in examples 1 to 6
| Ala(％) | Alb(％) | Alc(％) | |
| Example 1 | 75.4 | 16.1 | 8.5 |
| Example 2 | 75.1 | 16.6 | 8.3 |
| Example 3 | 79.3 | 17.8 | 2.9 |
| Example 4 | 70.8 | 14.3 | 14.9 |
| Example 5 | 76.8 | 17.4 | 5.8 |
| Example 6 | 77.3 | 12.9 | 9.8 |
It can be seen from the above table that the addition of raw materials 2 and 3 will seriously affect the appearance of Al in the final product.
Experimental example 2
In this example, the inorganic polymer phosphorous removal agent prepared in examples 3 to 6 and FeCl used in common were used3And taking aluminum sulfate solid as a phosphorus removing agent and taking sewage with the phosphorus concentration of 1.8mg/L as a to-be-treated object, and respectively carrying out phosphorus removing treatment.
The processing method comprises the following steps:
1000mL of raw water sample is taken, and the reagents are respectively added according to the dosage of 50mg/L, 80mg/L, 100mg/L and 150mg/L for coagulation experiments, wherein the coagulation conditions are as follows:
1. stirring at the speed of 250rmp for 1min, and adding a phosphorus removal agent according to the dosage after stirring;
2. stirring at 200rmp for 2 min;
3. stirring at 40rmp for 20 min;
4. standing for precipitation for 30 min. Standing and precipitating after full coagulation, and taking supernatant for detection.
The detection method adopts a conventional method in the field (refer to a corresponding monitoring method in the water and wastewater monitoring and analyzing method (fourth edition)), and the detection indexes comprise the TP content of the effluent (namely the TP content of the supernatant), the pH value of the effluent (namely the pH value of the supernatant), the turbidity of the effluent (namely the turbidity of the supernatant) and the properties of the effluent (namely the properties of the supernatant).
The results are shown in table 2:
TABLE 2 treatment effect of different phosphorus removing agents on phosphorus-containing sewage
Note: the point > 1.14 is due to the upper limit of the P assay of 1.14mg/L without dilution of the working curve.
From the comparison of the above experimental data, it can be seen that:
(1) the inorganic polymer phosphorus removal agent prepared in the embodiments 3-6 of the invention has good phosphorus removal effect, has smaller influence on the pH and the chromaticity of the water body compared with the conventionally used aluminum sulfate and ferric chloride, and has more stable effluent turbidity;
(2) although the aluminum occurrence form of the aluminum sulfate is detected to be the complete Ala form, the aluminum sulfate does not have the pre-polymerization form, and can be rapidly hydrolyzed after entering a water body, so that the alkalinity in the water body is consumed, and the phosphorus removal and the turbidity reduction are not facilitated;
(3) ferric chloride (FeCl)3) Although the phosphorus removal agent has continuous phosphorus removal capability, the phosphorus removal agent has serious influence on the pH and the chromaticity of a water body, and also has the problems of serious corrosion on equipment and the like.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A preparation method of an inorganic polymer dephosphorizing agent comprises the following steps:
(1) adding aluminum-containing acid solution into a pre-reactor, and adding Ca (OH) into the pre-reactor2Or CaO is reacted;
standing, discharging liquid with the volume of 40-75% of the upper part, and adding the rest solid-liquid mixture into the first reactor;
adding industrial hydrochloric acid or mixed acid of the industrial hydrochloric acid and sulfuric acid into a first reactor, wherein the addition amount of the industrial hydrochloric acid or mixed acid is 40-100% of the addition amount of the aluminiferous acid solution;
sealing the first reactor, heating to 110-130 ℃, and reacting for 2-3 hours;
(2) when the temperature of the reaction liquid obtained in the step (1) is reduced to below 40 ℃, injecting the reaction liquid into a first purification device through a slurry pump, carrying out diaphragm filter pressing, and adding the liquid obtained after filter pressing into a second reactor;
(3) heating the second reactor to 80 ℃, adding caustic alkali or sodium carbonate in batches under the condition of continuous heat preservation, wherein the mass of the total added sodium element is 40-75% of the mass of the aluminum element in the aluminiferous solution, the adding process needs to last for 1.5-2 hours, and the adding is carried out for more than 1 hour by continuous stirring reaction;
(4) and (4) cooling the reaction liquid obtained in the step (3) to below 40 ℃, injecting the reaction liquid into a second purification device through a slurry pump, and carrying out diaphragm filter pressing to obtain a liquid product, namely the inorganic polymer phosphorus removal agent.
2. The method according to claim 1, wherein in the step (1), Ca (OH) is charged2Or the molar ratio of CaO to aluminum in the aluminiferous acid solution is 1.5: 1-1.8: 1.
3. The preparation method according to claim 1, wherein in the step (1), the aluminiferous acid solution is PO with an aluminum content of more than 30g/L4 3-Acid solution accounting for more than 50% of anions.
4. The production method according to any one of claims 1 to 3, wherein in the step (1), the concentration of the industrial hydrochloric acid is 25%, and the sulfuric acid proportion in the mixed acid of the industrial hydrochloric acid and the sulfuric acid is less than 10%.
5. The method according to any one of claims 1 to 3, wherein in step (1), FeCl is further added to the first reactor3And ferric sulfate or ferrate is used as a reaction additive, and the mass of the iron element is controlled to be not more than 20% of the total mass of the aluminum element in the aluminiferous acid solution.
6. The preparation method according to any one of claims 1 to 3, wherein in the step (2), after the temperature of the reaction solution obtained in the step (1) is reduced to below 40 ℃, the reaction solution is injected into the first purification device through a slurry pump, is pressed for more than 30 minutes in a diaphragm pressure filtration mode, and the liquid obtained after the pressure filtration is added into the second reactor.
7. The preparation method of claim 6, wherein in the step (4), the inorganic polymer phosphorus removal agent is obtained by squeezing for more than 60 minutes in a diaphragm filter pressing mode, and the liquid product is aged for more than 2 hours at normal temperature.
8. An inorganic polymer dephosphorizing agent, which is characterized by being prepared by the preparation method of any one of claims 1 to 7.
9. The inorganic polymer phosphorus removal agent of claim 8, wherein the content of low hydrolyzed polymeric form Ala in the inorganic polymer phosphorus removal agent is more than 70% of the total content of Al, and the content of high hydrolyzed polymeric form Alc is less than 15% of the total content of Al.
10. The inorganic polymer phosphorus removal agent of claim 8 or 9, which is used for removing phosphorus in water.
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