CN114590886B - Self-degrading biological film filler and preparation method and application thereof - Google Patents
Self-degrading biological film filler and preparation method and application thereof Download PDFInfo
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- CN114590886B CN114590886B CN202210155025.3A CN202210155025A CN114590886B CN 114590886 B CN114590886 B CN 114590886B CN 202210155025 A CN202210155025 A CN 202210155025A CN 114590886 B CN114590886 B CN 114590886B
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
- C02F3/10—Packings; Fillings; Grids
- C02F3/105—Characterized by the chemical composition
- C02F3/108—Immobilising gels, polymers or the like
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/06—Nutrients for stimulating the growth of microorganisms
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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- General Chemical & Material Sciences (AREA)
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- Biological Treatment Of Waste Water (AREA)
Abstract
The invention belongs to the technical field of wastewater treatment. The self-degrading biomembrane filler is prepared by blending polylactic acid, a copolymerization modifier, a plasticizer, a heat stabilizer and a nucleating agent to obtain a polylactic acid substrate; washing the polylactic acid substrate with alkali to obtain a micro-nano material; impregnating the micro-nano material into a polymer solution to obtain a composite material; and (3) performing plasma grafting on the composite material to obtain the self-degradable biomembrane filler. The invention realizes the controllable release rate of polylactic acid as a carbon source by adjusting the proportion of polylactic acid and the copolymerization modifier. The alkaline washing polylactic acid substrate has the defects of forming a plurality of micro-nano grades on the surface, the specific surface area of the material is increased, hydrophilic groups are grafted through plasma bombardment, and the hydrophilicity of the biological film filler is improved. The biomembrane filler provided by the invention slowly releases the falling-off outer layer film in water, the inner active region forms a high-activity biomembrane, and the surface of the filler is continuously updated, so that the microbial activity is kept to be high-speed increased.
Description
Technical Field
The invention belongs to a preparation technology of a biological film filler in the field of wastewater treatment. In particular to a self-degrading biomembrane filler and a preparation method and application thereof.
Background
The biomembrane method has the advantages of small occupied area, good pollutant removal effect, high denitrification efficiency and the like, and is widely applied to the fields of industrial wastewater and domestic sewage. The filler is used as the most main component of the biological film technology and plays a decisive role in the growth environment of microorganisms. At present, the researches of scholars at home and abroad on biomembrane fillers are mainly carried out on the modification of the fillers, such as the introduction of hydrophilic groups on the surfaces, the increase of the surface roughness of the fillers, the internal doping of nutrient elements and the magnetic modification of the interiors of the fillers to influence the microbial activity. According to the method for enhancing the film forming performance of the graphene oxide modified biological film filler, disclosed in the invention patent with publication number of CN111647189A, the surface energy is increased by introducing polar groups, the surface roughness of the filler is improved, and the film forming efficiency is improved. The invention patent with publication number CN108751391A has increased hydrophilicity and biology through modifying inert filler base material with biological glue. The invention patent application with publication number of CN201810677116.7 describes a preparation method of a composite slow-release carbon source, wherein the carbon source is corncob particles or peanut shell particles, the artificially synthesized high molecular organic carbon source is polycaprolactone solid particles or polybutylene succinate solid particles, and the carbon source is microbial growth and propagation. At present, the problems that the surface of the microbial filler needs to be cleaned regularly, the carbon source cannot be decomposed sufficiently, the carbon source is easy to decay and lose efficacy and the like still exist in the application aspect of the microbial filler.
Disclosure of Invention
In order to solve the problems in the prior art, one of the purposes of the invention is to provide a preparation method of a self-degrading biomembrane filler, the prepared biomembrane filler does not need to be cleaned regularly, is used as a carrier and a carbon source and is fully utilized by microorganisms, the carbon source is prevented from being spoiled and invalid, and meanwhile, the film hanging can be accelerated, and the nutrition and mass transfer efficiency can be improved.
In order to achieve the above purpose, the present invention adopts the following technical scheme: a method for preparing self-degrading biological film filler, comprising the following steps:
s1, mixing polylactic acid, a copolymerization modifier, a plasticizer, a heat stabilizer and a nucleating agent, heating the mixture, and extruding and cooling the mixture through an extrusion device to prepare a polylactic acid substrate;
s2, soaking the polylactic acid substrate in the step S1 in a polymer solution, taking out and drying to obtain a composite material, and performing plasma grafting on the composite material to obtain the self-degrading biomembrane filler.
Further improvement of the preparation method as the self-degradable biological film filler:
preferably, the mixing mass ratio of the polylactic acid, the copolymerization modifier, the plasticizer, the heat stabilizer and the nucleating agent in the step S1 is (50-70)/(10-20)/(5-10)/(1-5).
Preferably, the copolymerization modifier in the step S1 is polyethylene glycol or caprolactone; or the plasticizer is dimethyl phthalate, diethyl phthalate or dioctyl phthalate; or the heat stabilizer is one or more than two of calcium ricinoleate, epoxidized soybean oil and maleic anhydride; or the nucleating agent is sodium dicarboxylic acid, sodium benzoate or nano silicon dioxide, and the particle size is 5-20nm.
Preferably, the heating mode of the mixture in the step S1 is gradient heating, the temperature range is 110-170 ℃, the difference between adjacent gradient temperatures is 10 ℃, and the heat preservation time at each gradient temperature is 5-10min.
Preferably, the polylactic acid substrate of step S1 is alkali washed before step S2, and a plurality of micro-nano defective regions are formed on the surface of the polylactic acid substrate.
Preferably, the solution for alkaline washing the polylactic acid substrate in the step S1 is sodium hydroxide or potassium hydroxide solution, the concentration is 10-30wt%, the alkaline washing mode is soaking, and the soaking time is 3-5h.
Preferably, the polymer solution in the step S2 comprises acrylic acid, chitosan and absolute ethyl alcohol, wherein the absolute ethyl alcohol is used as a solvent, the concentration of the acrylic acid in the polymer solution is 2-10wt% and the concentration of the chitosan is 1-5wt%; the mass ratio of the acrylic acid to the polylactic acid in the step S1 is (5-10) (50-70); the soaking time is 5-10min.
Preferably, in the step S2, the plasma is normal pressure plasma or vacuum plasma, the cavity pressure of the vacuum plasma is-5 to-3 pa, the grafting discharge power is 50-500W, and the grafting time is 1-10min.
It is a further object of the present invention to provide a self-degrading biofilm carrier prepared by any of the above methods.
The invention also aims to provide an application of the self-degradable biological film filler in sewage treatment.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention discloses a preparation method of a novel self-degradation biomembrane filler, which comprises the steps of mixing raw materials including polylactic acid, a copolymerization modifier and the like, and then performing hot melt co-extrusion to prepare a polylactic acid substrate, namely a plastic skeleton structure; the polylactic acid substrate mainly comprises polylactic acid, lactic acid is formed after hydrolysis, nutrition is provided for microorganisms in filler and water, the polylactic acid is controlled in release rate as a carbon source by adjusting the proportion of the polylactic acid to the copolymerization modifier, meanwhile, the surface impact resistance of the polylactic acid is improved, and the nucleating agent can promote the crystallization rate and efficiency of hot melting.
The heating mode of the hot melt is preferably gradient heating so as to control the crystallization hot melting rate, ensure the rigidity of the filler and ensure better hydrolyzability of the material.
Preferably, the polylactic acid base material is subjected to alkali washing treatment, so that a plurality of micro-nano defects are formed on the surface of the filler, and the specific surface area of the polylactic acid base material is enhanced.
However, polylactic acid has poor hydrophilicity and is easy to be biodegraded and utilized. According to the invention, the polylactic acid substrate is immersed in the polymer solution, a compact biological film layer can be formed on the surface of the polylactic acid substrate, so that the composite material is prepared, and the hydrophilicity and biocompatibility of the filler are improved.
After the composite material is subjected to plasma bombardment grafting, hydrophilic groups are loaded, and microorganisms can utilize nutrients in water and nutrients released by the filler, so that the adhesion and growth of the microorganisms are facilitated. The inner area of the biofilm packing is an active area for microorganism growth, and the polymer slowly releases and falls off after being decomposed by attached microorganisms in water, so that the active area is decomposed and utilized to form a biological cycle of growth-falling-growth so as to achieve the optimal growth state of the microorganisms.
2) The invention provides a self-degradable polylactic acid biomembrane filler which can be used as a carbon source, wherein polylactic acid is a natural degradable material, has better crystallinity, can be thoroughly degraded in a microbial environment to generate carbon dioxide and water, is nontoxic and harmless to organisms, and overcomes the defect of regular cleaning. The biomembrane filler provided by the invention is used as a carrier and a carbon source to be fully utilized by microorganisms, so that the carbon source is prevented from being spoiled and invalid, and meanwhile, the film formation can be accelerated, and the nutrition mass transfer efficiency can be improved. The self-degradable polylactic acid biomembrane filler slowly releases the outer polymer in water, and the inner active region forms a high-activity biological layer, so that the surface of the filler is continuously updated and grown, and the microbial activity is kept to be high-speed increased. Meanwhile, the microbial coating can provide nutrition for attached microorganisms and microorganisms in a water body, has the advantage of high strength, has natural hydrophilicity and biocompatibility, can promote the activity of the microorganisms, and has a better film forming effect.
Detailed Description
The present invention is described in detail by the following preferred embodiments, which are intended to illustrate the present invention in detail, but should not be construed as limiting the invention, and various changes and modifications can be made without departing from the spirit and the essential scope thereof, which are intended to be included within the scope of the present invention.
Example 1
The embodiment provides a preparation method of a self-degradable biological film filler, which comprises the following steps:
s1, uniformly mixing 65g of polylactic acid, 10g of caprolactone, 10g of dioctyl phthalate, 5g of epoxidized soybean oil and 5g of silicon dioxide nano particles for 3 hours by a high-speed mixer, adding the uniformly mixed materials into a double-screw extruder, blending for 5min at 120 ℃, 5min at 130 ℃, 5min at 140 ℃, 5min at 150 ℃, 5min at 160 ℃ and 5min at 170 ℃, and extruding and cooling to form after the blending is finished to obtain a polylactic acid substrate;
and (3) soaking the substrate in 10% sodium hydroxide solution for 4 hours, taking out, cleaning with pure water, and drying to form a plurality of micro-nano defects on the surface of the substrate.
S2, taking 5g of chitosan and 10g of acrylic acid to be dissolved in 1L of absolute ethyl alcohol, and uniformly stirring to form a polymer solution L1.
S3, soaking the dried base material in an L1 solution for 5min, taking out, drying, and then irradiating for grafting treatment under a plasma, wherein the pressure of a vacuum cavity is-3 pa, the discharge power is 100W, and the bombardment time is 10min. Taking out, cleaning with pure water, and drying for standby, thus obtaining the self-degrading biomembrane filler.
The prepared self-degradable biological film filler is tested, and the specific surface area of the material is 610m 2 /m 3 Contact angle 46.3 DEG, packing density 0.98g/cm 3 The water holding rate is 3.2%. Inoculating municipal sewage to the SBR reactor, taking the filler as a test group A (1), and simultaneously setting a traditional elastic filler as a control group A (2), wherein the COD removal rate is 79% and the nitrate nitrogen removal rate is 96%; the latter has a COD removal rate of 65% and a nitrate nitrogen removal rate of 76%. (1) The mass loss efficiency of the filler is 2% -3% per week, and the release of the carbon source can shorten the film forming timeThe film forming time is 14d, and the total nitrogen removal efficiency is improved.
Example 2
The embodiment provides a preparation method of a self-degradable biological film filler, which comprises the following steps:
s1, uniformly mixing 60g of polylactic acid, 20g of polyethylene glycol, 10g of dioctyl phthalate, 5g of epoxidized soybean oil and 5g of sodium benzoate for 3 hours by a high-speed mixer, adding the uniformly mixed materials into a double-screw extruder, blending for 10min at 120 ℃, 10min at 130 ℃, 10min at 140 ℃, 10min at 150 ℃, 10min at 160 ℃ and 10min at 170 ℃, and extruding, cooling and forming after the blending is finished to obtain a polylactic acid substrate;
and (3) putting the polylactic acid substrate into a 20% sodium hydroxide solution for soaking for 4 hours, taking out, cleaning with pure water, and drying to form a plurality of micro-nano level defects on the surface of the substrate.
S2, dissolving 5g of acrylic acid and 5g of chitosan in 1L of absolute ethyl alcohol, and uniformly stirring to form a polymer solution L2.
S3, soaking the dried substrate in an L2 solution for 5min, taking out, drying, and then irradiating for grafting treatment under a plasma, wherein the vacuum cavity pressure is-5 pa, the discharge power is 500W, and the bombardment time is 5min. Taking out, cleaning with pure water, and drying for standby, thus obtaining the self-degrading biomembrane filler.
The prepared self-degradable biological film filler is tested, and the specific surface area of the material is 550m 2 /m 3 Contact angle 48.5 deg. and packing density 1.15g/cm 3 The water holding rate is 3.8%, and the anaerobic CSTR complete mixed flow reactor is inoculated with municipal sewage, which indicates that the reactor is smoothly started. Taking the filler as a test group B (1), and simultaneously setting a traditional elastic filler as a control group B (2), wherein the COD (chemical oxygen demand) removal rate is 75%, and the nitrate nitrogen removal rate is 95%; the latter had a COD removal of 67% and a nitrate removal of 73%. (1) The efficiency of the mass loss of the filling material is 2-3% per week, the film forming time can be shortened by releasing the carbon source, the film forming time is 12d, and the biological film is thinner.
Example 3
The embodiment provides a preparation method of a self-degradable biological film filler, which comprises the following steps:
s1, uniformly mixing 70g of polylactic acid, 10g of polyethylene glycol, 10g of dioctyl phthalate, 5g of maleic anhydride and 5g of sodium benzoate for 3.5 hours by a high-speed mixer, adding the uniformly mixed materials into a double-screw extruder, blending for 5 minutes at 115 ℃, 8 minutes at 126 ℃, 10 minutes at 142 ℃, 5 minutes at 148 ℃, 8 minutes at 163 ℃ and 10 minutes at 175 ℃, and extruding, cooling and forming after the blending is finished to obtain a polylactic acid substrate;
and (3) putting the polylactic acid plastic substrate into 30% sodium hydroxide solution for soaking for 4 hours, taking out, cleaning with pure water, and drying to form a plurality of micro-nano level defects on the surface of the substrate.
S2, 8g of acrylic acid and 3g of chitosan are dissolved in 1 liter of absolute ethanol to form a polymer solution L3.
S3, soaking the prepared and dried base material in an L3 solution for 5min, taking out, drying, and then irradiating and grafting under a plasma, wherein the vacuum cavity pressure is-5 pa, the discharge power is 50W, and the bombardment time is 2min. Taking out, cleaning with pure water, and drying for standby, thus obtaining the self-degrading biomembrane filler.
The prepared self-degradable biological film filler is tested, and the specific surface area of the material is 480m 2 /m 3 Contact angle 50.8 DEG, packing density 1.05g/cm 3 Inoculating municipal sewage to an SBR reactor, taking the filler as a test group C (1), and simultaneously setting a traditional elastic filler as a control group C (2), wherein the COD removal rate is 88% and the nitrate nitrogen removal rate is 98%; the latter has a COD removal rate of 77% and a nitrate nitrogen removal rate of 76%. (1) The efficiency of the mass loss of the filling material is 2% -3% per week, the film forming time can be shortened by releasing the carbon source, the film forming time is 15d, and the total nitrogen removal efficiency is improved.
In conclusion, the biological film filler provided by the invention has the COD removal rate of 88%, the nitrate nitrogen removal rate of 98%, and excellent performance.
The present invention is not limited to the above-described specific embodiments. It will be understood that various changes and modifications may be made without departing from the spirit and scope of the invention, which is intended to be included within the scope of the invention.
Claims (9)
1. The preparation method of the self-degrading biological film filler is characterized by comprising the following steps:
s1, mixing polylactic acid, a copolymerization modifier, a plasticizer, a heat stabilizer and a nucleating agent, heating the mixture, and extruding and cooling the mixture through an extrusion device to prepare a polylactic acid substrate;
s2, soaking the polylactic acid substrate in the step S1 in a polymer solution, taking out and drying to obtain a composite material, and performing plasma grafting on the composite material to obtain the self-degrading biomembrane filler;
the polymer solution in the step S2 comprises acrylic acid, chitosan and absolute ethyl alcohol, wherein the absolute ethyl alcohol is used as a solvent, the concentration of the acrylic acid in the polymer solution is 2-10wt% and the concentration of the chitosan is 1-5wt%; the mass ratio of the acrylic acid to the polylactic acid in the step S1 is (5-10) (50-70); the soaking time is 5-10min.
2. The method for preparing the self-degrading biofilm carrier according to claim 1, wherein the mixing mass ratio of the polylactic acid to the copolymerization modifier to the plasticizer to the heat stabilizer to the nucleating agent in the step S1 is (50-70): 10-20): 5-10): 1-5.
3. The method for preparing the self-degrading biofilm pack according to claim 1, wherein the copolymerization modifier in the step S1 is polyethylene glycol or caprolactone; or the plasticizer is dimethyl phthalate, diethyl phthalate or dioctyl phthalate; or the heat stabilizer is one or more than two of calcium ricinoleate, epoxidized soybean oil and maleic anhydride; or the nucleating agent is sodium dicarboxylic acid, sodium benzoate or nano silicon dioxide, and the particle size is 5-20nm.
4. The method for preparing the self-degrading biofilm carrier according to claim 1, wherein the heating mode of the mixture in the step S1 is gradient heating, the temperature range is 110-170 ℃, the difference between adjacent gradient temperatures is 10 ℃, and the heat preservation time at each gradient temperature is 5-10min.
5. The method for producing a self-degrading biofilm carrier according to claim 1, wherein the polylactic acid substrate of step S1 is alkali washed before step S2, and a plurality of micro-nano defective areas are formed on the surface of the polylactic acid substrate.
6. The method for preparing the self-degrading biofilm carrier according to claim 1 or 5, wherein the solution for alkaline washing the polylactic acid substrate in the step S1 is sodium hydroxide or potassium hydroxide solution, the concentration is 10-30wt%, the alkaline washing mode is soaking, and the soaking time is 3-5h.
7. The method for preparing a self-degrading biofilm carrier according to claim 1, wherein in the step S2, the plasma is normal pressure plasma or vacuum plasma, the cavity pressure of the vacuum plasma is-5 to-3 pa, the grafted discharge power is 50-500W, and the grafting time is 1-10min.
8. A self-degrading biofilm carrier as obtained by the method of any of claims 1 to 7.
9. Use of the self-degrading biofilm pack of claim 8 in sewage treatment.
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