CN111115795A - Ion response biofilm formation material for sewage treatment and preparation method thereof - Google Patents
Ion response biofilm formation material for sewage treatment and preparation method thereof Download PDFInfo
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- C02F3/00—Biological treatment of water, waste water, or sewage
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- C02F3/302—Nitrification and denitrification treatment
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- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses an ion response biofilm formation material for sewage treatment and a preparation method thereof. Firstly, preparing interpenetrating network hydrogel with ion responsiveness, and then loading a carbon source to the interpenetrating network hydrogel with ion responsiveness to obtain the ion responsiveness biofilm formation material for sewage treatment. The film forming material has high mechanical strength and good tensile property, and can be used for preparing film forming materials with different shapes by changing the mould, thereby meeting the requirements of sewage treatment on the film forming materials. The biofilm formation material has the ion strength responsiveness and can generate NO according to the nitrification process in sewage treatment3 ‑Or NO2 ‑To control the release rate of the carbon source required for the denitrification process. The carbon source release with response to the ionic strength avoids the reduction of denitrification efficiency or the over-release of the carbon source caused by insufficient release of the carbon sourceSecondary pollution is often caused.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to an ion response biofilm formation material for sewage treatment and a preparation method thereof.
Background
In recent years, with the rural economic development and the improvement of the rural living standard of China, more and more rural domestic sewage is generated and enters a water circulation system, so that the water environment is polluted. Denitrification in rural domestic sewage treatment is one of important purposes, and the conventional biological denitrification mode is mainly used at presentBy nitration of NH4 +By oxidation to NO3 -Or NO2 -And then NO is converted by denitrification3 -Or NO2 -Reduction to N2And is discharged to the atmosphere. A large amount of organic carbon sources need to be consumed in the denitrification process, but the C/N of the current rural domestic sewage is generally low, so that the carbon sources needed in the denitrification process are insufficient, and the denitrification efficiency is low.
Many scholars promote the denitrification process by adding carbon sources. However, the adding amount of liquid carbon sources such as methanol and glucose is difficult to control, and the problem of secondary pollution is prominent. Cellulose solid carbon source is easy to be utilized by microorganism, but the carbon releasing period is short, and the carbon releasing amount in the former period is high, thus easily causing secondary pollution. The artificially synthesized biodegradable polymer solid carbon source usually has a longer carbon release period but a small carbon release amount. Therefore, the carbon source adding technology in the existing sewage treatment is improved, so that the high-efficiency denitrification of the low-C/N rural domestic sewage is necessary.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide an ion response biofilm formation material for sewage treatment and a preparation method thereof. The prepared material has high mechanical strength and good tensile property, and meets the requirements of sewage treatment on the film forming material. The biofilm formation material is loaded with a carbon source, has ionic strength responsiveness and can generate NO according to the nitrification process in sewage treatment3 -Or NO2 -The concentration of the carbon source controls the release rate of the carbon source, and the carbon source is properly supplemented for the treatment system of the rural domestic sewage with low C/N.
In order to solve the technical problem, the technical scheme adopted by the invention is as follows:
preparing the ion-responsive interpenetrating network hydrogel, and loading a carbon source to obtain the ion-responsive biofilm formation material for sewage treatment. The method comprises the following steps:
(1) adding carboxyl nano-cellulose into water, and carrying out ultrasonic treatment for 2-30 minutes to prepare 1-3.5 wt% carboxyl nano-cellulose suspension;
(2) mixing the raw materials in a mass ratio of 80-120 g: 0.5-0.7: 0.15-0.25: 6-9 of N-vinyl pyrrolidone, a photoinitiator, a cross-linking agent and a terminal amino polyethylene glycol mixture are added into 700ml of water with 500-; introducing nitrogen into the mixed solution 1 for bubbling for 5-30 min;
(3) adding 80-100ml of 1-3.5 wt% carboxyl nano cellulose suspension into the mixed solution 1 to form a mixed solution 2, adjusting the pH to 7.5-9, and stirring the mixed solution 2 for 5-30min to uniformly disperse the mixed solution; adding the obtained mixed solution 2 into a mold, heating to 30-50 ℃ and maintaining for 5-60 min; then gradually cooling the mixed solution 2 to room temperature, and standing for 15-50min to obtain an intermediate product 1;
(4) placing the intermediate product 1 under 254nm or 365nm ultraviolet rays for irradiating for 1-5h, taking out the intermediate product from a mold after the irradiation is finished, soaking the intermediate product in deionized water for 2-5 days, and changing water every 8-24 hours to remove unreacted monomers; after soaking, washing with deionized water to obtain interpenetrating network hydrogel with ion responsiveness;
(5) preparing a carbon source into a saturated carbon source aqueous solution, soaking the interpenetrating network hydrogel with the ion responsiveness in the carbon source aqueous solution for 1-60 days, and changing the carbon source aqueous solution every 1-10 days; and washing the soaked product with deionized water to obtain the ion-responsive interpenetrating network hydrogel loaded with a carbon source, namely the ion-responsive biofilm formation material for sewage treatment.
The photoinitiator in the step (2) is any one or a mixture of more of benzoin dimethyl ether, α, α -diethoxyacetophenone, 2' -azobisisobutyramidine hydrochloride, benzophenone, methyl o-benzoylbenzoate and 1-chloro-4-propoxythioanthracene-9-one.
The cross-linking agent in the step (2) is any one or a mixture of more of diethylene glycol dimethacrylate, vinyl tributyrinoxime silane, divinylbenzene, triallylamine and allyl glycidyl ether.
In the step (5), the carbon source is any one or a mixture of glucose, sucrose and fructose.
An ion response biofilm formation material for sewage treatment prepared according to the preparation method.
The ion-responsive interpenetrating network hydrogel loaded with the carbon source is an ion-responsive biofilm formation material for sewage treatment, and has good mechanical properties. Has ion strength responsiveness and can be based on NO generated in the nitrification process in sewage treatment3 -Or NO2 -To control the release rate of the carbon source required for the denitrification process.
Compared with the prior art, the invention has the beneficial effects that:
1. the ion response film forming material for sewage treatment prepared by the invention has high mechanical strength and good tensile property, and different shapes of film forming materials can be prepared by changing the mould, thereby meeting the requirements of sewage treatment on the film forming materials.
2. The carbon source is loaded on the biofilm formation material prepared by the invention, and the carbon source can be supplemented for rural domestic sewage with low C/N, so that the requirement of a denitrification process on the carbon source is met, and the sewage denitrification efficiency is improved.
3. The biofilm formation material prepared by the invention has ionic strength responsiveness and can be used for treating NO generated in the nitrification process in sewage treatment3 -Or NO2 -To control the release rate of the carbon source required for the denitrification process. The stronger the ionic strength, the higher the carbon source release rate of the film-forming material. When the C/N of the sewage is low, the carbon source in the water is not enough to support the denitrification process to be carried out, and the accumulated NO3 -Or NO2 -The concentration is high, and the release rate of the carbon source in the film forming material is accelerated due to the ionic strength response. The carbon source release with the response of the ionic strength avoids the condition that the denitrification efficiency is reduced due to insufficient carbon source release amount or the secondary pollution is caused by excessive carbon source release amount.
Drawings
FIG. 1 shows the relationship between the carbon source release rate and time of the film forming material prepared in example 1 of the present invention.
FIG. 2 shows the carbon source cumulative release rate of the biofilm formation material prepared in example 2 of the present invention within 5 days and the NO in the experimental simulation wastewater3 -The concentration relationship.
Detailed Description
The present invention is described in detail below with reference to examples, which are provided for further illustration of the present invention and are not to be construed as limiting the scope of the present invention. It should be understood that various changes and modifications can be made by those skilled in the art after reading the disclosure of the present invention, and equivalents fall within the scope of the appended claims.
Example 1
(1) Adding carboxyl nano-cellulose into water, and carrying out ultrasonic treatment for 5 minutes to prepare 1 wt% carboxyl nano-cellulose suspension.
(2) Mixing the raw materials in a mass ratio of 80g to 100: 0.5: 0.15: 7, adding the mixture of N-vinyl pyrrolidone, benzoin dimethyl ether, divinyl benzene and amino-terminated polyethylene glycol into 500ml of water, and stirring for 10min to form a uniform mixed solution 1. And the mixed solution 1 was bubbled with nitrogen for 10 min.
(3) 80ml of a 1 wt% carboxyl nanocellulose suspension was added to the mixture 1 to form a mixture 2, and the pH was adjusted to 8. The mixture 2 was stirred for 15min to disperse uniformly. The resulting mixture 2 was added to a mold and heated to 35 ℃ for 40 min. Then, the mixture 2 was gradually cooled to room temperature and left to stand for 30min to obtain an intermediate 1.
(4) And (3) irradiating the intermediate product 1 for 3 hours under 254nm ultraviolet rays, and taking out the intermediate product from the mold after the irradiation is finished. The reaction mixture was soaked in deionized water for 2 days, and the water was changed every 10 hours to remove unreacted monomers. And washing after soaking to obtain the interpenetrating network hydrogel with ion responsiveness.
(5) Preparing glucose into an aqueous solution, soaking the interpenetrating network hydrogel with the ion responsiveness in the aqueous glucose solution for 45 days, and changing the aqueous glucose solution every 5 days. And washing the soaked product with deionized water to obtain the ion-responsive interpenetrating network hydrogel loaded with a carbon source, namely the ion-responsive biofilm formation material for sewage treatment.
The tensile strength of the film forming material prepared by the embodiment reaches 1.3 MPa. After the biofilm formation material prepared in the embodiment is placed in simulated sewage for 30 days, the cumulative release rate of the carbon source is 41%.
In order to verify the carbon source slow release performance of the biofilm culturing material, six equal parts of the biofilm culturing material prepared in the embodiment are respectively put into the same amount of simulated wastewater with the same proportion. The carbon source release rate was measured in one portion on day 5, day 10, day 15, day 20, day 25 and day 30, and the results are shown in FIG. 1.
Example 2
(1) Adding carboxyl nano-cellulose into water, and carrying out ultrasonic treatment for 10 minutes to prepare 2 wt% carboxyl nano-cellulose suspension.
(2) The total weight is 85g, the mass ratio is 100: 0.6: 0.2: 7 of N-vinyl pyrrolidone, benzoin dimethyl ether, divinyl benzene and amino terminated polyethylene glycol are added into 550ml of water and stirred for 15min to form a uniform mixed solution 1. And the mixed solution 1 was bubbled with nitrogen for 15 min.
(3) 85ml of a 2 wt% carboxyl nanocellulose suspension was added to the mixture 1 to form a mixture 2, and the pH was adjusted to 8. The mixture 2 was stirred for 20min to disperse the mixture uniformly. The resulting mixture 2 was added to a mold and heated to 45 ℃ for 40 min. Then, the mixture 2 was gradually cooled to room temperature and left to stand for 30min to obtain an intermediate 1.
(4) And (3) placing the intermediate product 1 under 254nm ultraviolet rays for irradiating for 2 hours, and taking out from the mold after the irradiation is finished. The reaction mixture was immersed in deionized water for 3 days, and the water was changed every 12 hours to remove unreacted monomers. And washing after soaking to obtain the interpenetrating network hydrogel with ion responsiveness.
(5) Preparing glucose into an aqueous solution, soaking the interpenetrating network hydrogel with the ion responsiveness in the aqueous solution of the glucose for 50 days, and replacing a carbon source aqueous solution every 5 days. And washing the soaked product with deionized water to obtain the ion-responsive interpenetrating network hydrogel loaded with a carbon source, namely the ion-responsive biofilm formation material for sewage treatment.
The tensile strength of the film forming material prepared by the embodiment reaches 1.1 MPa. After the biofilm formation material prepared in the embodiment is placed in simulated sewage for 30 days, the cumulative release rate of the carbon source is 44%.
To verify the ion responsiveness of the biofilm formation material, 5 parts of the biofilm formation material prepared in this example were placed in experimental simulated wastewater with NO 3-concentrations of 0.2 wt%, 0.4 wt%, 0.6 wt%, 0.8 wt%, and 1.0 wt% for 5 days, and the carbon source release rate was measured, and the results are shown in FIG. 2.
Example 3
(1) Adding carboxyl nano-cellulose into water, and carrying out ultrasonic treatment for 10 minutes to prepare 1 wt% carboxyl nano-cellulose suspension.
(2) The total weight is 100g, the mass ratio is 100: 0.5: 0.15: 6, adding the mixture of N-vinyl pyrrolidone, benzophenone, triallylamine and terminal amino polyethylene glycol into 600ml of water, and stirring for 20min to form a uniform mixed solution 1. And the mixed solution 1 was bubbled with nitrogen for 15 min.
(3) 100ml of a 1 wt% carboxyl nanocellulose suspension was added to the mixture 1 to form a mixture 2, and the pH was adjusted to 8.5. The mixture 2 was stirred for 20min to disperse the mixture uniformly. The resulting mixture 2 was added to a mold and heated to 30 ℃ for 50 min. Then, the mixture 2 was gradually cooled to room temperature and left to stand for 30min to obtain an intermediate 1.
(4) And (3) placing the intermediate product 1 under 254nm ultraviolet rays for irradiating for 2 hours, and taking out from the mold after the irradiation is finished. The reaction mixture was immersed in deionized water for 3 days, and the water was changed every 12 hours to remove unreacted monomers. And washing after soaking to obtain the interpenetrating network hydrogel with ion responsiveness.
(5) Preparing sucrose into an aqueous solution, soaking the interpenetrating network hydrogel with the ion responsiveness in the sucrose aqueous solution for 40 days, and replacing a carbon source aqueous solution every 5 days. And washing the soaked product with deionized water to obtain the ion-responsive interpenetrating network hydrogel loaded with a carbon source, namely the ion-responsive biofilm formation material for sewage treatment.
The tensile strength of the film forming material prepared by the embodiment reaches 0.9 MPa. After the biofilm culturing material prepared in the embodiment is placed in simulated sewage for 30 days, the cumulative release rate of the carbon source is 63%.
Example 4
(1) Adding carboxyl nano-cellulose into water, and carrying out ultrasonic treatment for 20 minutes to prepare a 3 wt% carboxyl nano-cellulose suspension.
(2) Mixing the raw materials in a mass ratio of 100: 0.7: 0.2: 8, adding the mixture of N-vinyl pyrrolidone, benzophenone, triallylamine and terminal amino polyethylene glycol into 550ml of water, and stirring for 35min to form a uniform mixed solution 1. And the mixed solution 1 was bubbled with nitrogen for 20 min.
(3) 85ml of a 3 wt% carboxyl nanocellulose suspension was added to the mixture 1 to form a mixture 2, and the pH was adjusted to 8.5. The mixture 2 was stirred for 20min to disperse the mixture uniformly. The resulting mixture 2 was added to a mold and heated to 55 ℃ and maintained for 10 min. Then, the mixture 2 was gradually cooled to room temperature and left to stand for 40min to obtain an intermediate 1.
(4) And (3) placing the intermediate product 1 under 254nm ultraviolet rays for irradiating for 2 hours, and taking out from the mold after the irradiation is finished. The reaction mixture was soaked in deionized water for 2 days, and the water was changed every 10 hours to remove unreacted monomers. And washing after soaking to obtain the interpenetrating network hydrogel with ion responsiveness.
(5) Preparing sucrose into aqueous solution, soaking the interpenetrating network hydrogel with the ion responsiveness in the sucrose aqueous solution for 60 days, and replacing the carbon source aqueous solution every 10 days. And washing the soaked product with deionized water to obtain the ion-responsive interpenetrating network hydrogel loaded with a carbon source, namely the ion-responsive biofilm formation material for sewage treatment.
The tensile strength of the film forming material prepared by the embodiment reaches 0.8 MPa. After the biofilm formation material prepared in the embodiment is placed in simulated sewage for 30 days, the carbon source accumulative release rate is 48%.
Example 5
(1) Adding carboxyl nano-cellulose into water, and carrying out ultrasonic treatment for 20 minutes to prepare a 3 wt% carboxyl nano-cellulose suspension.
(2) Adding a mixture of N-vinyl pyrrolidone, α -diethoxyacetophenone, vinyl tributyrinoxime silane and amino-terminated polyethylene glycol with the total weight of 100g and the mass ratio of 100: 0.7: 0.2: 9 into 600ml of water, stirring for 35min to form a uniform mixed solution 1, and introducing nitrogen into the mixed solution 1 to bubble for 20 min.
(3) 85ml of a 3 wt% carboxyl nanocellulose suspension was added to the mixture 1 to form a mixture 2, and the pH was adjusted to 7.5. The mixture 2 was stirred for 25min to disperse the mixture uniformly. The resulting mixture 2 was added to a mold and heated to 45 ℃ for 60 min. Then, the mixture 2 was gradually cooled to room temperature and left to stand for 30min to obtain an intermediate 1.
(4) And (3) placing the intermediate product 1 under 365nm ultraviolet rays for irradiating for 4 hours, and taking out from the mold after the irradiation is finished. The reaction mixture was immersed in deionized water for 3 days, and the water was changed every 12 hours to remove unreacted monomers. And washing after soaking to obtain the interpenetrating network hydrogel with ion responsiveness.
(5) Preparing fructose into an aqueous solution, soaking the interpenetrating network hydrogel with the ion responsiveness in the aqueous solution of the fructose for 55 days, and replacing the aqueous solution of the carbon source every 5 days. And washing the soaked product with deionized water to obtain the ion-responsive interpenetrating network hydrogel loaded with a carbon source, namely the ion-responsive biofilm formation material for sewage treatment.
The tensile strength of the film forming material prepared by the embodiment reaches 1.0 MPa. After the biofilm formation material prepared in the embodiment is placed in simulated sewage for 30 days, the cumulative release rate of the carbon source is 57%.
Example 6
(1) Adding carboxyl nano-cellulose into water, and carrying out ultrasonic treatment for 30 minutes to prepare 2.5 wt% carboxyl nano-cellulose suspension.
(2) Adding a mixture of N-vinyl pyrrolidone, α -diethoxyacetophenone, vinyl tributyrinoxime silane and amino-terminated polyethylene glycol with the total weight of 110g and the mass ratio of 100: 0.6: 0.23: 8 into 700ml of water, stirring for 50min to form a uniform mixed solution 1, and introducing nitrogen into the mixed solution 1 to bubble for 30 min.
(3) 90ml of a 2.5 wt% carboxyl nanocellulose suspension was added to the mixture 1 to form a mixture 2, and the pH was adjusted to 7.5. The mixture 2 was stirred for 30min to disperse the mixture uniformly. The resulting mixture 2 was added to a mold and heated to 50 ℃ for 30 min. Then, the mixture 2 was gradually cooled to room temperature and left to stand for 45min to obtain an intermediate 1.
(4) And (3) placing the intermediate product 1 under 365nm ultraviolet rays for irradiating for 4 hours, and taking out from the mold after the irradiation is finished. The reaction mixture was soaked in deionized water for 2 days, and the water was changed every 12 hours to remove unreacted monomers. And washing after soaking to obtain the interpenetrating network hydrogel with ion responsiveness.
(5) Preparing fructose into an aqueous solution, soaking the interpenetrating network hydrogel with the ion responsiveness in the aqueous solution of the fructose for 60 days, and replacing the aqueous solution of the carbon source every 5 days. And washing the soaked product with deionized water to obtain the ion-responsive interpenetrating network hydrogel loaded with a carbon source, namely the ion-responsive biofilm formation material for sewage treatment.
The tensile strength of the film forming material prepared by the embodiment reaches 1.2 MPa. After the biofilm formation material prepared in the embodiment is placed in simulated sewage for 30 days, the cumulative release rate of the carbon source is 42%.
The above is only a specific embodiment of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions or modifications made on the basis of the present invention to solve the same technical problems and achieve the same technical effects are all covered in the protection scope of the present invention.
Claims (5)
1. A preparation method of an ion response biofilm formation material for sewage treatment is characterized by comprising the following steps:
(1) adding carboxyl nano-cellulose into water, and carrying out ultrasonic treatment for 2-30 minutes to prepare 1-3.5 wt% carboxyl nano-cellulose suspension;
(2) mixing the raw materials in a mass ratio of 80-120 g: 0.5-0.7: 0.15-0.25: 6-9 of N-vinyl pyrrolidone, a photoinitiator, a cross-linking agent and a terminal amino polyethylene glycol mixture are added into 700ml of water with 500-; introducing nitrogen into the mixed solution 1 for bubbling for 5-30 min;
(3) adding 80-100ml of 1-3.5 wt% carboxyl nano cellulose suspension into the mixed solution 1 to form a mixed solution 2, adjusting the pH to 7.5-9, and stirring the mixed solution 2 for 5-30min to uniformly disperse the mixed solution; adding the obtained mixed solution 2 into a mold, heating to 30-50 ℃ and maintaining for 5-60 min; then gradually cooling the mixed solution 2 to room temperature, and standing for 15-50min to obtain an intermediate product 1;
(4) placing the intermediate product 1 under 254nm or 365nm ultraviolet rays for irradiating for 1-5h, taking out the intermediate product from a mold after the irradiation is finished, soaking the intermediate product in deionized water for 2-5 days, and changing water every 8-24 hours to remove unreacted monomers; after soaking, washing with deionized water to obtain interpenetrating network hydrogel with ion responsiveness;
(5) preparing a carbon source into a saturated carbon source aqueous solution, soaking the interpenetrating network hydrogel with the ion responsiveness in the carbon source aqueous solution for 1-60 days, and changing the carbon source aqueous solution every 1-10 days; and washing the soaked product with deionized water to obtain the ion-responsive interpenetrating network hydrogel loaded with a carbon source, namely the ion-responsive biofilm formation material for sewage treatment.
2. The preparation method according to claim 1, wherein the photoinitiator in the step (2) is any one or more selected from benzoin dimethyl ether, α, α -diethoxyacetophenone, 2' -azobisisobutyramidine hydrochloride, benzophenone, methyl o-benzoylbenzoate and 1-chloro-4-propoxythioxan-9-one.
3. The method of claim 1, wherein: the cross-linking agent in the step (2) is any one or a mixture of more of diethylene glycol dimethacrylate, vinyl tributyrinoxime silane, divinylbenzene, triallylamine and allyl glycidyl ether.
4. The method of claim 1, wherein: in the step (5), the carbon source is any one or a mixture of glucose, sucrose and fructose.
5. An ion-responsive biofilm formation material for sewage treatment prepared by the preparation method according to any one of claims 1 to 4.
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| CN116395841A (en) * | 2023-06-09 | 2023-07-07 | 天津壹帆水务有限公司 | Double-response slow-release carbon source preparation method for low-C/N wastewater denitrification process |
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