CN112209567B - Adsorption purification method of livestock and poultry wastewater - Google Patents

Adsorption purification method of livestock and poultry wastewater Download PDF

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CN112209567B
CN112209567B CN202011048224.1A CN202011048224A CN112209567B CN 112209567 B CN112209567 B CN 112209567B CN 202011048224 A CN202011048224 A CN 202011048224A CN 112209567 B CN112209567 B CN 112209567B
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wastewater
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poultry wastewater
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CN112209567A (en
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高航
胡竞
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Jiangsu Yancheng Environmental Protection Science And Technology City Soil Pollution Remediation Research And Development Center
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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
    • C02F3/28—Anaerobic digestion processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B01J20/28019—Spherical, ellipsoidal or cylindrical
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
    • C02F2101/30—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
    • 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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  • Life Sciences & Earth Sciences (AREA)
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  • Environmental & Geological Engineering (AREA)
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  • Hydrology & Water Resources (AREA)
  • Microbiology (AREA)
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  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention provides an adsorption purification method of livestock and poultry wastewater, which comprises the steps of pretreating the livestock and poultry wastewater, adding mullite powder, mixing uniformly, performing anaerobic fermentation to generate biogas and a treatment solution, wherein the biogas is used for the subsequent use, adding an adsorbent into the treatment solution, standing, performing solid-liquid separation to obtain effluent and sludge, directly discharging the effluent and the sludge, adding a medicine into the treatment solution, mixing, drying and transporting the mixture outside, and effectively reducing the Chemical Oxygen Demand (COD) concentration and ammonia Nitrogen (NH) in the livestock and poultry wastewater 3 -N) concentration and Total Phosphorus (TP) concentration, and has wide application prospect.

Description

Adsorption purification method of livestock and poultry wastewater
Technical Field
The invention relates to the technical field of adsorption and purification, in particular to an adsorption and purification method of livestock and poultry wastewater.
Background
Along with the development of the breeding industry, the discharge amount of livestock and poultry waste water in China is continuously increasing. The livestock wastewater is usually organic wastewater which contains high nitrogen and phosphorus and is difficult to biodegrade, and direct discharge can cause eutrophication of water bodies, consume a large amount of dissolved oxygen in the water and cause black and odorous water bodies. Meanwhile, the phenomenon of seedling burning due to overhigh nitrogen and phosphorus in soil is easily caused by directly returning the livestock and poultry wastewater to the field.
The traditional method for treating the wastewater is to introduce the wastewater into a wastewater treatment plant to treat the wastewater in an intensive mode, but the problems of large culture area, low density and overhigh pipeline laying cost for constructing the wastewater treatment plant in rural livestock and poultry culture are solved. Therefore, the in-situ livestock and poultry wastewater treatment technology, namely the technology for directly treating wastewater by adding materials at a pollution source, is an economical and efficient wastewater treatment technology.
The adsorption technology is to put the adsorbent into polluted media (such as wastewater, soil, flue gas and the like) and enrich pollutants on the surface of the adsorbent by using the physical and chemical properties of the adsorbent, so as to achieve the purpose of purifying water bodies or other media. Common adsorbents in the market are processed to a certain extent, and have the characteristics of relatively high cost and possibility of causing secondary pollution. Therefore, the development of natural low cost sorbent materials has been reluctant.
The Chemical Oxygen Demand (COD) concentration of the livestock and poultry wastewater is up to 10000mg/L, and the ammonia Nitrogen (NH) 3 N) at a concentration of 500 to 1300mg/L and Total Phosphorus (TP) at a concentration of 50 to 100mg/L, is rich in N,The P organic wastewater is a serious pollution source in cities and countryside, and has high treatment difficulty and high cost. The livestock and poultry breeding wastewater has the characteristics that: the discharge amount is large, and the impact load is large; solid and liquid are mixed, the concentration of organic matters is high, and the treatment difficulty is high; n, P has particularly high nutrient content and low carbon-nitrogen ratio.
Lignite is a natural coal with low metamorphic grade and is produced in many places in China. Because the lignite has high specific surface area and large porosity, the lignite also has a certain attention in the adsorption field. Patent CN109012588A discloses a method for preparing a sewage treatment agent by using lignite as a raw material, which is obtained by compounding lignite treated by acid and alkali with ferric chloride, has adsorption and photocatalysis effects, is mainly suitable for removing dyes such as methyl orange, has a removal rate of only 92%, and has a poor treatment effect on livestock and poultry wastewater. In addition, a large amount of hydrochloric acid and sodium hydroxide are used in the preparation process, so that the pollution of acid and alkali is large, and the preparation method is not environment-friendly.
Disclosure of Invention
The invention aims to provide an adsorption purification method of livestock and poultry wastewater, which can effectively reduce the Chemical Oxygen Demand (COD) concentration and ammonia Nitrogen (NH) in the livestock and poultry wastewater 3 -N) concentration and Total Phosphorus (TP) concentration.
In order to achieve the purpose, the invention is realized by the following scheme:
an adsorption purification method of livestock and poultry wastewater comprises the steps of pretreating 100 parts of livestock and poultry wastewater by weight, adding 0.8-1 part of mullite powder, uniformly mixing, carrying out anaerobic fermentation to generate methane and a treatment solution, allowing the methane to be used subsequently, adding 1.2-1.8 parts of an adsorbent into the treatment solution, standing for 8-10 hours, carrying out solid-liquid separation to obtain effluent and sludge, directly discharging the effluent and the sludge, adding a chemical, mixing and drying the chemical, and transporting the dried sludge for external use; the preparation method of the adsorbent comprises the following steps:
(1) firstly, carrying out surface modification on lignite powder by utilizing methacryloxypropyl trimethoxy silane to obtain modified lignite powder;
(2) then, taking acrylamide and N- (4-aminophenyl) acrylamide as raw materials to carry out polymerization reaction, and adding modified lignite powder in the polymerization process to prepare gel particles;
(3) and finally, adding the gel particles into a polyvinyl alcohol aqueous solution, adding polysilicate aluminum sulfate, stirring for reaction, and performing post-treatment to obtain the adsorbent.
Preferably, the concrete method for pretreating the livestock and poultry wastewater comprises the following steps: firstly, adjusting the pH value of the livestock and poultry wastewater to 6.5-7.5, and then carrying out electrolytic treatment for 10-15 minutes under the condition of 1-2 mA. The pretreatment is helpful for degrading organic matters in the livestock wastewater.
Preferably, the process conditions of anaerobic fermentation are as follows: the dissolved oxygen is controlled at 0.3-0.5 mg/L, the temperature is 32-40 ℃, and the time is 5-8 days.
Preferably, the biogas generated by anaerobic fermentation enters a water seal device for storage for subsequent use.
Preferably, the agent used for adding the sludge is prepared by the following method: adding N- (4-aminophenyl) acrylamide, an aniline monomer, a diacrylate polyethylene glycol ester and a chain transfer agent into N-vinyl pyrrolidone, carrying out ultrasonic oscillation for 30-40 minutes, adding an initiator, carrying out stirring reaction for 8-10 hours at 0-5 ℃, heating in a water bath to 40-50 ℃, and continuously carrying out stirring reaction for 3-5 hours to obtain the N- (4-aminophenyl) acrylamide modified polyacrylamide; wherein the mass ratio of the N- (4-aminophenyl) acrylamide, the aniline monomer, the diacrylate polyethylene glycol ester, the chain transfer agent, the N-vinyl pyrrolidone and the initiator is 1: 0.7-0.9: 0.3-0.4: 0.05-0.08: 2.8-3.5: 0.03-0.04 percent, the dosage of the medicament is 1.8-2.2 percent of the weight of the sludge, and the treatment time is 5-7 hours.
Further preferably, the chain transfer agent is a mixture of 2-methoxyethyl 2-phenyl-2- (pentylthiocarbonylthio) acetate and ethyl xanthogen acetate in a molar ratio of 1: 2-3; the initiator is azodiisopropyl imidazoline.
Preferably, the drying time is 13-15 hours.
Preferably, the specific method of step (1) is as follows: adding lignite powder into methacryloxypropyl trimethoxy silane in an amount which is 3-5 times the weight of the lignite powder, stirring and reacting for 4-6 hours at 120-130 ℃, and centrifuging to obtain the modified lignite powder.
Preferably, the specific method of step (2) is as follows, in parts by weight: adding 1 part of acrylamide and 0.08-0.1 part of N- (4-aminophenyl) acrylamide into 3-5 parts of water, stirring until the acrylamide and the N- (4-aminophenyl) acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 2-3 hours at 68.34Gy/min, adding 0.7-0.9 part of modified lignite powder, stirring and uniformly mixing, continuously irradiating the mixture for 8-10 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to prepare gel particles.
Further preferably, the post-treatment method comprises the following steps: the water in the hydrogel is fully replaced by normal hexane, and then dried by carbon dioxide supercritical fluid to obtain dry gel, and the dry gel is crushed to obtain gel particles.
More preferably, the process conditions of the supercritical fluid drying by carbon dioxide are as follows: the pressure is 6-8 MPa, the temperature is 45-50 ℃, and the time is 8-10 hours.
More preferably, the particle size of the gel particles is 1 to 2 mm.
Preferably, in the step (3), the mass ratio of the gel particles, the polyvinyl alcohol aqueous solution and the polyaluminum silicate sulfate is 1: 3.5-4.5: 5.5-7.5, wherein the mass concentration of the polyvinyl alcohol aqueous solution is 8-10%.
Preferably, in the step (3), the stirring reaction time is 30-40 minutes.
Preferably, in the step (3), the post-treatment method comprises the following specific steps: and (3) preparing raw material balls by using a ball forming mill, roasting for 2-3 hours at the temperature of 100-107 ℃, and naturally cooling to room temperature (25 ℃) to obtain the adsorbent.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method comprises the steps of pretreating the livestock wastewater, adding mullite powder, uniformly mixing, performing anaerobic fermentation to generate biogas and treatment liquid, using the biogas for subsequent use, adding an adsorbent into the treatment liquid, standing, performing solid-liquid separation to obtain effluent and sludge, directly discharging the effluent and the sludge, adding a Chemical Oxygen Demand (COD) concentration and ammonia Nitrogen (NH) in the livestock wastewater, mixing, drying and transporting the mixture outside for use, and effectively reducing the Chemical Oxygen Demand (COD) concentration and the ammonia Nitrogen (NH) in the livestock wastewater 3 -N) concentration and Total Phosphorus (TP) concentration.
(2) The mullite powder is rich in metal elements such as magnesium, aluminum and the like, plays a role in catalyzing, promotes the anaerobic fermentation to be fully carried out, and degrades organic matters in the livestock wastewater. The biogas generated by anaerobic fermentation can be reused, and the method is green and environment-friendly.
(3) The key technical point of the invention is that the preparation of the adsorbent is that firstly, the surface of the lignite powder is modified by utilizing methacryloxypropyltrimethoxysilane to obtain modified lignite powder; then, taking acrylamide and N- (4-aminophenyl) acrylamide as raw materials to carry out polymerization reaction, and adding modified lignite powder in the polymerization process to prepare gel particles; and finally, adding the gel particles into a polyvinyl alcohol aqueous solution, adding polysilicate aluminum sulfate, stirring for reaction, and performing post-treatment to obtain the adsorbent. The main raw material lignite powder is low in cost and porous, has a certain adsorption effect, but is poor in hydrophilicity, and the adsorption effect is influenced.
(4) According to the invention, the lignite powder is subjected to surface modification by utilizing methacryloxypropyltrimethoxysilane, double bonds are introduced, the lignite powder also participates in the reaction in the polymerization process of acrylamide and N- (4-aminophenyl) acrylamide, the lignite powder exists in a system in the form of chemical bonds, the structure is stable, the formed gel particles contain hydrophilic amino groups, the hydrophilicity is improved, and the gelation enables the product pores to be richer, so that the improvement of the adsorption effect is facilitated. Finally, the gel particles are added into the polyvinyl alcohol aqueous solution, and then the poly-silicon aluminum sulfate is added for stirring reaction to form a net structure, so that the product has more abundant pores, and the adsorption and purification effects are further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be 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
An adsorption purification method of livestock and poultry wastewater, firstly pretreating 100kg of livestock and poultry wastewater, then adding 0.8kg of mullite powder, uniformly mixing, carrying out anaerobic fermentation to generate biogas and treatment liquid, wherein the biogas is used for subsequent use, 1.8kg of adsorbent is added into the treatment liquid, standing for 8 hours, carrying out solid-liquid separation to obtain effluent and sludge, the former is directly discharged, and the latter is used by external transportation after adding, mixing and drying; the preparation method of the adsorbent comprises the following steps:
(1) firstly, carrying out surface modification on lignite powder by utilizing methacryloxypropyl trimethoxysilane to obtain modified lignite powder;
(2) then, taking acrylamide and N- (4-aminophenyl) acrylamide as raw materials to carry out polymerization reaction, and adding modified lignite powder in the polymerization process to prepare gel particles;
(3) and finally, adding the gel particles into a polyvinyl alcohol aqueous solution, adding polysilicate aluminum sulfate, stirring for reaction, and performing post-treatment to obtain the adsorbent.
The concrete method for pretreating the livestock and poultry wastewater comprises the following steps: firstly, the pH value of the livestock and poultry wastewater is adjusted to 7.5, and then the livestock and poultry wastewater is electrolyzed for 15 minutes under the condition of 1 mA.
The process conditions of anaerobic fermentation are as follows: the dissolved oxygen is controlled at 0.3mg/L, the temperature is 40 ℃, and the time is 5 days.
The marsh gas generated by anaerobic fermentation enters a water seal device for storage for subsequent use.
The medicament used for adding the medicine into the sludge is prepared by the following method: adding N- (4-aminophenyl) acrylamide, an aniline monomer, diacrylate polyethylene glycol ester and a chain transfer agent into N-vinyl pyrrolidone, carrying out ultrasonic oscillation for 40 minutes, adding an initiator, carrying out stirring reaction for 10 hours at 0 ℃, heating in a water bath to 40 ℃, and continuously carrying out stirring reaction for 5 hours to obtain the compound N-vinyl pyrrolidone; wherein the mass ratio of N- (4-aminophenyl) acrylamide, aniline monomer, diacrylate polyethylene glycol ester, chain transfer agent, N-vinyl pyrrolidone and initiator is 1: 0.7: 0.4: 0.05: 3.5: 0.03, the dosage of the medicament is 2.2 percent of the weight of the sludge, and the treatment time is 5 hours.
The chain transfer agent is a mixture of 2-methoxyethyl 2-phenyl-2- (pentylthiocarbonylthio) acetate and ethyl xanthogen acetate, and the molar ratio of the two is 1: 3; the initiator is azodiisopropyl imidazoline.
The drying time was 13 hours.
The specific method of the step (1) is as follows: adding lignite powder into methacryloxypropyltrimethoxysilane of which the weight is 5 times that of the lignite powder, stirring and reacting for 6 hours at 120 ℃, and centrifuging to obtain the modified lignite powder.
The specific method of the step (2) is as follows: firstly, 1kg of acrylamide and 0.08kg of N- (4-aminophenyl) acrylamide are added into 5kg of water, stirred until the acrylamide and the acrylamide are completely dissolved, transferred into a cobalt source chamber, irradiated for 2 hours at 68.34Gy/min, added with 0.9kg of modified lignite powder, stirred and mixed evenly, and continuously irradiated for 8 hours at 108.93Gy/min to obtain hydrogel, and the hydrogel is subjected to post-treatment to prepare gel particles.
The specific method of post-treatment is as follows: the water in the hydrogel is fully replaced by normal hexane, and then dried by carbon dioxide supercritical fluid to obtain dry gel, and the dry gel is crushed to obtain gel particles.
The process conditions of the supercritical fluid drying of the carbon dioxide are as follows: the pressure is 8MPa, the temperature is 45 ℃, and the time is 10 hours.
The particle size of the gel particles was 1 mm.
In the step (3), the mass ratio of the gel particles, the polyvinyl alcohol aqueous solution and the poly-aluminum silicate sulfate is 1: 4.5: 5.5, wherein the mass concentration of the polyvinyl alcohol aqueous solution is 10%.
In the step (3), the reaction time was stirred for 30 minutes.
In the step (3), the post-treatment method comprises the following specific steps: preparing raw material balls by using a ball forming mill, roasting for 2 hours at 107 ℃, and naturally cooling to room temperature to obtain the adsorbent.
Example 2
An adsorption purification method of livestock and poultry wastewater comprises the steps of pretreating 100kg of livestock and poultry wastewater, adding 1kg of mullite powder, uniformly mixing, carrying out anaerobic fermentation to generate biogas and treatment liquid, allowing the biogas to be used subsequently, adding 1.2kg of adsorbent into the treatment liquid, standing for 10 hours, carrying out solid-liquid separation to obtain effluent and sludge, directly discharging the effluent and the sludge, adding chemicals into the treatment liquid, mixing, drying and carrying out outward for use; the preparation method of the adsorbent comprises the following steps:
(1) firstly, carrying out surface modification on lignite powder by utilizing methacryloxypropyl trimethoxysilane to obtain modified lignite powder;
(2) then, taking acrylamide and N- (4-aminophenyl) acrylamide as raw materials to carry out polymerization reaction, and adding modified lignite powder in the polymerization process to prepare gel particles;
(3) and finally, adding the gel particles into a polyvinyl alcohol aqueous solution, adding polysilicate aluminum sulfate, stirring for reaction, and performing post-treatment to obtain the adsorbent.
The concrete method for pretreating the livestock and poultry wastewater comprises the following steps: firstly, the pH value of the livestock and poultry wastewater is adjusted to 6.5, and then the livestock and poultry wastewater is electrolyzed for 10 minutes under the condition of 2 mA.
The process conditions of anaerobic fermentation are as follows: the dissolved oxygen is controlled at 0.5mg/L, the temperature is 32 ℃, and the time is 8 days.
The marsh gas generated by anaerobic fermentation enters a water seal device for storage for subsequent use.
The medicament used for adding the chemicals into the sludge is prepared by the following method: adding N- (4-aminophenyl) acrylamide, an aniline monomer, diacrylate polyethylene glycol ester and a chain transfer agent into N-vinyl pyrrolidone, carrying out ultrasonic oscillation for 30 minutes, adding an initiator, carrying out stirring reaction for 8 hours at the temperature of 5 ℃, heating in a water bath to 50 ℃, and continuously carrying out stirring reaction for 3 hours to obtain the compound N-vinyl pyrrolidone; wherein the mass ratio of N- (4-aminophenyl) acrylamide, aniline monomer, diacrylate polyethylene glycol ester, chain transfer agent, N-vinyl pyrrolidone and initiator is 1: 0.9: 0.3: 0.08: 2.8: 0.04, the dosage of the medicament is 1.8 percent of the weight of the sludge, and the treatment time is 7 hours.
The chain transfer agent is a mixture of 2-methoxyethyl 2-phenyl-2- (pentylthiocarbonylthio) acetate and ethylxanthic acid, and the molar ratio of the two is 1: 2; the initiator is azodiisopropyl imidazoline.
The drying time was 15 hours.
The specific method of the step (1) is as follows: adding lignite powder into methacryloxypropyltrimethoxysilane of which the weight is 3 times that of the lignite powder, stirring and reacting for 4 hours at 130 ℃, and centrifuging to obtain the modified lignite powder.
The specific method of the step (2) is as follows: firstly adding 1kg of acrylamide and 0.1kg of N- (4-aminophenyl) acrylamide into 3kg of water, stirring until the acrylamide and the acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 3 hours at 68.34Gy/min, adding 0.7kg of modified lignite powder, stirring and uniformly mixing the mixture, continuously irradiating the mixture for 10 hours at 108.93Gy/min to obtain hydrogel, and performing post-treatment to prepare gel particles.
The specific method of post-treatment is as follows: the water in the hydrogel is fully replaced by normal hexane, and then dried by carbon dioxide supercritical fluid to obtain dry gel, and the dry gel is crushed to obtain gel particles.
The process conditions of the supercritical fluid drying of the carbon dioxide are as follows: the pressure is 6MPa, the temperature is 50 ℃, and the time is 8 hours.
The particle size of the gel particles was 2 mm.
In the step (3), the mass ratio of the gel particles, the polyvinyl alcohol aqueous solution and the poly-aluminum silicate sulfate is 1: 3.5: 7.5, wherein the mass concentration of the polyvinyl alcohol aqueous solution is 8%.
In the step (3), the reaction time was 40 minutes with stirring.
In the step (3), the post-treatment method comprises the following specific steps: and preparing raw material balls by using a ball forming mill, roasting for 3 hours at 100 ℃, and naturally cooling to room temperature to obtain the adsorbent.
Example 3
An adsorption purification method of livestock and poultry wastewater, firstly pretreating 100kg of livestock and poultry wastewater, then adding 0.9kg of mullite powder, uniformly mixing, carrying out anaerobic fermentation to generate biogas and treatment liquid, wherein the biogas is used for subsequent use, 1.5kg of adsorbent is added into the treatment liquid, standing for 9 hours, carrying out solid-liquid separation to obtain effluent and sludge, the former is directly discharged, and the latter is used by external transportation after adding, mixing and drying; the preparation method of the adsorbent comprises the following steps:
(1) firstly, carrying out surface modification on lignite powder by utilizing methacryloxypropyl trimethoxy silane to obtain modified lignite powder;
(2) then, taking acrylamide and N- (4-aminophenyl) acrylamide as raw materials to carry out polymerization reaction, and adding modified lignite powder in the polymerization process to prepare gel particles;
(3) and finally, adding the gel particles into a polyvinyl alcohol aqueous solution, adding polysilicate aluminum sulfate, stirring for reaction, and performing post-treatment to obtain the adsorbent.
The concrete method for pretreating the livestock and poultry wastewater comprises the following steps: firstly, the pH value of the livestock and poultry wastewater is adjusted to 7, and then the livestock and poultry wastewater is electrolyzed for 12 minutes under the condition of 2 mA.
The process conditions of the anaerobic fermentation are as follows: the dissolved oxygen was controlled at 0.4mg/L at 38 ℃ for 6 days.
The marsh gas generated by anaerobic fermentation enters a water seal device for storage for subsequent use.
The medicament used for adding the medicine into the sludge is prepared by the following method: adding N- (4-aminophenyl) acrylamide, an aniline monomer, a diacrylate polyethylene glycol ester and a chain transfer agent into N-vinyl pyrrolidone, carrying out ultrasonic oscillation for 35 minutes, adding an initiator, carrying out stirring reaction for 9 hours at the temperature of 3 ℃, heating in a water bath to 45 ℃, and continuously carrying out stirring reaction for 4 hours to obtain the acrylic acid/acrylic acid copolymer resin; wherein the mass ratio of the N- (4-aminophenyl) acrylamide, the aniline monomer, the diacrylate polyethylene glycol ester, the chain transfer agent, the N-vinyl pyrrolidone and the initiator is 1: 0.8: 0.35: 0.07: 3: 0.035, the dosage of the medicament is 2 percent of the weight of the sludge, and the treatment time is 6 hours.
The chain transfer agent is a mixture of 2-methoxyethyl 2-phenyl-2- (pentylthiocarbonylthio) acetate and ethyl xanthogen acetate, and the molar ratio of the two is 1: 2.5; the initiator is azodiisopropyl imidazoline.
The drying time was 14 hours.
The specific method of the step (1) is as follows: adding lignite powder into 4 times of methacryloxypropyltrimethoxysilane by weight, stirring at 125 ℃ for reaction for 5 hours, and centrifuging to obtain the modified lignite powder.
The specific method of the step (2) is as follows: firstly, 1kg of acrylamide and 0.09kg of N- (4-aminophenyl) acrylamide are added into 4kg of water, stirred until the acrylamide and the N- (4-aminophenyl) acrylamide are completely dissolved, transferred into a cobalt source chamber, irradiated for 2.5 hours at 68.34Gy/min, added with 0.8kg of modified lignite powder, stirred and mixed evenly, and continuously irradiated for 9 hours at 108.93Gy/min to obtain hydrogel, and the hydrogel is subjected to post-treatment to prepare gel particles.
The specific method of post-treatment is as follows: the water in the hydrogel is fully replaced by normal hexane, and then dried by carbon dioxide supercritical fluid to obtain dry gel, and the dry gel is crushed to obtain gel particles.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 7MPa, the temperature is 48 ℃, and the time is 9 hours.
The particle size of the gel particles was 1.5 mm.
In the step (3), the mass ratio of the gel particles, the polyvinyl alcohol aqueous solution and the poly-aluminum silicate sulfate is 1: 4: and 6, wherein the mass concentration of the polyvinyl alcohol aqueous solution is 9%.
In the step (3), the reaction time was stirred for 35 minutes.
In the step (3), the post-treatment method comprises the following specific steps: and preparing raw material balls by using a ball forming mill, roasting for 2.5 hours at 105 ℃, and naturally cooling to room temperature to obtain the adsorbent.
Comparative example 1
An adsorption purification method of livestock and poultry wastewater, firstly pretreating 100kg of livestock and poultry wastewater, then adding 0.8kg of mullite powder, uniformly mixing, carrying out anaerobic fermentation to generate biogas and treatment liquid, wherein the biogas is used for subsequent use, 1.8kg of adsorbent is added into the treatment liquid, standing for 8 hours, carrying out solid-liquid separation to obtain effluent and sludge, the former is directly discharged, and the latter is used by external transportation after adding, mixing and drying; the preparation method of the adsorbent comprises the following steps:
(1) then, taking acrylamide and N- (4-aminophenyl) acrylamide as raw materials to carry out polymerization reaction, and adding lignite powder in the polymerization process to prepare gel particles;
(2) and finally, adding the gel particles into a polyvinyl alcohol aqueous solution, adding polysilicate aluminum sulfate, stirring for reaction, and performing post-treatment to obtain the adsorbent.
The concrete method for pretreating the livestock and poultry wastewater comprises the following steps: firstly, the pH value of the livestock and poultry wastewater is adjusted to 7.5, and then the livestock and poultry wastewater is electrolyzed for 15 minutes under the condition of 1 mA.
The process conditions of anaerobic fermentation are as follows: the dissolved oxygen is controlled at 0.3mg/L, the temperature is 40 ℃, and the time is 5 days.
The marsh gas generated by anaerobic fermentation enters a water seal device for storage for subsequent use.
The medicament used for adding the medicine into the sludge is prepared by the following method: adding N- (4-aminophenyl) acrylamide, an aniline monomer, diacrylate polyethylene glycol ester and a chain transfer agent into N-vinyl pyrrolidone, carrying out ultrasonic oscillation for 40 minutes, adding an initiator, carrying out stirring reaction for 10 hours at 0 ℃, heating in a water bath to 40 ℃, and continuously carrying out stirring reaction for 5 hours to obtain the compound N-vinyl pyrrolidone; wherein the mass ratio of N- (4-aminophenyl) acrylamide, aniline monomer, diacrylate polyethylene glycol ester, chain transfer agent, N-vinyl pyrrolidone and initiator is 1: 0.7: 0.4: 0.05: 3.5: 0.03, the dosage of the medicament is 2.2 percent of the weight of the sludge, and the treatment time is 5 hours.
The chain transfer agent is a mixture of 2-methoxyethyl 2-phenyl-2- (pentylthiocarbonylthio) acetate and ethyl xanthogen acetate, and the molar ratio of the two is 1: 3; the initiator is azodiisopropyl imidazoline.
The drying time was 13 hours.
The specific method of the step (1) is as follows: firstly, 1kg of acrylamide and 0.08kg of N- (4-aminophenyl) acrylamide are added into 5kg of water, stirred until the acrylamide and the acrylamide are completely dissolved, transferred into a cobalt source chamber, irradiated for 2 hours at 68.34Gy/min, added with 0.9kg of lignite powder, stirred and mixed evenly, and continuously irradiated for 8 hours at 108.93Gy/min to obtain hydrogel, and the hydrogel particles are prepared after post-treatment.
The specific method of post-treatment is as follows: the water in the hydrogel is fully replaced by normal hexane, and then dried by carbon dioxide supercritical fluid to obtain dry gel, and the dry gel is crushed to obtain gel particles.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 8MPa, the temperature is 45 ℃, and the time is 10 hours.
The particle size of the gel particles was 1 mm.
In the step (2), the mass ratio of the gel particles, the polyvinyl alcohol aqueous solution and the poly-aluminum silicate sulfate is 1: 4.5: 5.5, wherein the mass concentration of the polyvinyl alcohol aqueous solution is 10%.
In the step (2), the reaction time was stirred for 30 minutes.
In the step (2), the post-treatment method comprises the following specific steps: and preparing raw material balls by using a ball forming mill, roasting for 2 hours at 107 ℃, and naturally cooling to room temperature to obtain the adsorbent.
Comparative example 2
An adsorption purification method of livestock and poultry wastewater, firstly pretreating 100kg of livestock and poultry wastewater, then adding 0.8kg of mullite powder, uniformly mixing, carrying out anaerobic fermentation to generate biogas and treatment liquid, wherein the biogas is used for subsequent use, 1.8kg of adsorbent is added into the treatment liquid, standing for 8 hours, carrying out solid-liquid separation to obtain effluent and sludge, the former is directly discharged, and the latter is used by external transportation after adding, mixing and drying; the preparation method of the adsorbent comprises the following steps:
(1) firstly, carrying out surface modification on lignite powder by utilizing methacryloxypropyl trimethoxysilane to obtain modified lignite powder;
(2) and then adding the modified lignite powder into a polyvinyl alcohol aqueous solution, adding polysilicate aluminum sulfate, stirring for reaction, and performing post-treatment to obtain the adsorbent.
The concrete method for pretreating the livestock and poultry wastewater comprises the following steps: firstly, the pH value of the livestock and poultry wastewater is adjusted to 7.5, and then the livestock and poultry wastewater is electrolyzed for 15 minutes under the condition of 1 mA.
The process conditions of anaerobic fermentation are as follows: the dissolved oxygen is controlled at 0.3mg/L, the temperature is 40 ℃, and the time is 5 days.
The marsh gas generated by anaerobic fermentation enters a water seal device for storage for subsequent use.
The medicament used for adding the medicine into the sludge is prepared by the following method: adding N- (4-aminophenyl) acrylamide, an aniline monomer, diacrylate polyethylene glycol ester and a chain transfer agent into N-vinyl pyrrolidone, carrying out ultrasonic oscillation for 40 minutes, adding an initiator, carrying out stirring reaction for 10 hours at 0 ℃, heating in a water bath to 40 ℃, and continuously carrying out stirring reaction for 5 hours to obtain the compound N-vinyl pyrrolidone; wherein the mass ratio of N- (4-aminophenyl) acrylamide, aniline monomer, diacrylate polyethylene glycol ester, chain transfer agent, N-vinyl pyrrolidone and initiator is 1: 0.7: 0.4: 0.05: 3.5: 0.03, the dosage of the medicament is 2.2 percent of the weight of the sludge, and the treatment time is 5 hours.
The chain transfer agent is a mixture of 2-methoxyethyl 2-phenyl-2- (pentylthiocarbonylthio) acetate and ethyl xanthogen acetate, and the molar ratio of the two is 1: 3; the initiator is azodiisopropyl imidazoline.
The drying time was 13 hours.
The specific method of the step (1) is as follows: adding lignite powder into methacryloxypropyltrimethoxysilane of which the weight is 5 times that of the lignite powder, stirring and reacting for 6 hours at 120 ℃, and centrifuging to obtain the modified lignite powder.
In the step (2), the mass ratio of the modified lignite powder, the polyvinyl alcohol aqueous solution and the polyaluminum silicate sulfate is 1: 4.5: 5.5, wherein the mass concentration of the polyvinyl alcohol aqueous solution is 10%.
In the step (2), the reaction time was stirred for 30 minutes.
In the step (2), the post-treatment method comprises the following specific steps: and preparing raw material balls by using a ball forming mill, roasting for 2 hours at 107 ℃, and naturally cooling to room temperature to obtain the adsorbent.
Comparative example 3
An adsorption purification method of livestock and poultry wastewater, firstly pretreating 100kg of livestock and poultry wastewater, then adding 0.8kg of mullite powder, uniformly mixing, carrying out anaerobic fermentation to generate biogas and treatment liquid, wherein the biogas is used for subsequent use, 1.8kg of adsorbent is added into the treatment liquid, standing for 8 hours, carrying out solid-liquid separation to obtain effluent and sludge, the former is directly discharged, and the latter is used by external transportation after adding, mixing and drying; the preparation method of the adsorbent comprises the following steps:
(1) firstly, carrying out surface modification on lignite powder by utilizing methacryloxypropyl trimethoxy silane to obtain modified lignite powder;
(2) then, acrylamide and N- (4-aminophenyl) acrylamide are used as raw materials to carry out polymerization reaction, and modified lignite powder is added in the polymerization process to prepare gel particles, namely the adsorbent.
The concrete method for pretreating the livestock and poultry wastewater comprises the following steps: firstly, the pH value of the livestock and poultry wastewater is adjusted to 7.5, and then the livestock and poultry wastewater is electrolyzed for 15 minutes under the condition of 1 mA.
The process conditions of anaerobic fermentation are as follows: the dissolved oxygen is controlled at 0.3mg/L, the temperature is 40 ℃, and the time is 5 days.
The marsh gas generated by anaerobic fermentation enters a water seal device for storage for subsequent use.
The medicament used for adding the medicine into the sludge is prepared by the following method: adding N- (4-aminophenyl) acrylamide, an aniline monomer, diacrylate polyethylene glycol ester and a chain transfer agent into N-vinyl pyrrolidone, carrying out ultrasonic oscillation for 40 minutes, adding an initiator, carrying out stirring reaction for 10 hours at 0 ℃, heating in a water bath to 40 ℃, and continuously carrying out stirring reaction for 5 hours to obtain the compound N-vinyl pyrrolidone; wherein the mass ratio of N- (4-aminophenyl) acrylamide, aniline monomer, diacrylate polyethylene glycol ester, chain transfer agent, N-vinyl pyrrolidone and initiator is 1: 0.7: 0.4: 0.05: 3.5: 0.03, the using amount of the medicament is 2.2 percent of the weight of the sludge, and the treatment time is 5 hours.
The chain transfer agent is a mixture of 2-methoxyethyl 2-phenyl-2- (pentylthiocarbonylthio) acetate and ethyl xanthogen acetate, and the molar ratio of the two is 1: 3; the initiator is azodiisopropyl imidazoline.
The drying time was 13 hours.
The specific method of the step (1) is as follows: adding lignite powder into methacryloxypropyltrimethoxysilane of which the weight is 5 times that of the lignite powder, stirring and reacting for 6 hours at 120 ℃, and centrifuging to obtain the modified lignite powder.
The specific method of the step (2) is as follows: firstly, 1kg of acrylamide and 0.08kg of N- (4-aminophenyl) acrylamide are added into 5kg of water, stirred until the acrylamide and the acrylamide are completely dissolved, transferred into a cobalt source chamber, irradiated for 2 hours at 68.34Gy/min, added with 0.9kg of modified lignite powder, stirred and mixed evenly, and continuously irradiated for 8 hours at 108.93Gy/min to obtain hydrogel, and the hydrogel is subjected to post-treatment to prepare gel particles.
The specific method of post-treatment is as follows: the water in the hydrogel is fully replaced by normal hexane, and then dried by carbon dioxide supercritical fluid to obtain dry gel, and the dry gel is crushed to obtain gel particles.
The process conditions of the supercritical carbon dioxide fluid drying are as follows: the pressure is 8MPa, the temperature is 45 ℃, and the time is 10 hours.
The particle size of the gel particles was 1 mm.
Test examples
Wastewater in a certain cattle farm, and the water quality of inlet water: chemical Oxygen Demand (COD) concentration of 12000mg/L, ammonia Nitrogen (NH) 3 -N) concentration of 1200mg/L and Total Phosphorus (TP) concentration of 100mg/L, and the treatment is performed according to the methods of examples 1-3 or comparative examples 1-3, respectively, and the water quality conditions of the effluent are shown in Table 1.
TABLE 1. quality inspection of effluent
Figure BDA0002708696990000171
As can be seen from Table 1, examples 1 to 3 showed good effects of adsorbing and purifying wastewater in cattle farms, COD and NH 3 The concentration of-N and TP reach the national emission standard.
In the comparative example 1, the lignite powder is not modified, so that the dispersibility and the hydrophilicity in a system are poor, and the adsorption and purification effects on the wastewater are influenced; step (2) is omitted in comparative example 2, step (3) is omitted in comparative example 3, and porosity is not abundant enough, so that the adsorption and purification effects on the wastewater are influenced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (7)

1. An adsorption purification method of livestock and poultry wastewater is characterized in that 100 parts of livestock and poultry wastewater is pretreated firstly, then 0.8-1 part of mullite powder is added, after uniform mixing, anaerobic fermentation is carried out to generate methane and treatment liquid, the methane is used for subsequent use, 1.2-1.8 parts of adsorbent is added into the treatment liquid, standing is carried out for 8-10 hours, solid-liquid separation is carried out to obtain effluent and sludge, the former is directly discharged, and the latter is used for external transportation after adding and mixing and drying; the preparation method of the adsorbent comprises the following steps:
(1) firstly, carrying out surface modification on lignite powder by utilizing methacryloxypropyl trimethoxysilane to obtain modified lignite powder;
(2) then, taking acrylamide and N- (4-aminophenyl) acrylamide as raw materials to carry out polymerization reaction, and adding modified lignite powder in the polymerization process to prepare gel particles;
(3) finally, adding the gel particles into a polyvinyl alcohol aqueous solution, then adding polysilicate aluminum sulfate, stirring for reaction, and carrying out post-treatment to obtain the adsorbent;
the specific method of the step (1) is as follows: adding lignite powder into methacryloxypropyltrimethoxysilane of which the weight is 3-5 times that of the lignite powder, stirring and reacting for 4-6 hours at the temperature of 120-130 ℃, and centrifuging to obtain the modified lignite powder;
wherein the specific method of the step (2) comprises the following steps in parts by weight: adding 1 part of acrylamide and 0.08-0.1 part of N- (4-aminophenyl) acrylamide into 3-5 parts of water, stirring until the acrylamide and the N- (4-aminophenyl) acrylamide are completely dissolved, transferring the mixture into a cobalt source chamber, irradiating the mixture for 2-3 hours at 68.34Gy/min, adding 0.7-0.9 part of modified lignite powder, stirring and uniformly mixing, continuously irradiating the mixture for 8-10 hours at 108.93Gy/min to obtain hydrogel, then fully replacing the water in the hydrogel with N-hexane, drying the hydrogel with carbon dioxide supercritical fluid to obtain dried gel, and crushing the dried gel to prepare gel particles;
wherein the Chemical Oxygen Demand (COD) concentration of the livestock and poultry wastewater is 12000mg/L, and ammonia Nitrogen (NH) 3 -N) concentration of 1200mg/L and Total Phosphorus (TP) concentration of 100 mg/L.
2. The method for adsorbing and purifying livestock and poultry wastewater as claimed in claim 1, wherein the concrete method for pretreating livestock and poultry wastewater comprises the following steps: firstly, adjusting the pH value of the livestock and poultry wastewater to 6.5-7.5, and then carrying out electrolytic treatment for 10-15 minutes under the condition of 1-2 mA.
3. The method for adsorbing and purifying livestock wastewater as claimed in claim 1, characterized in that the anaerobic fermentation process conditions are as follows: the dissolved oxygen is controlled at 0.3-0.5 mg/L, the temperature is 32-40 ℃, and the time is 5-8 days.
4. The method for adsorbing and purifying livestock and poultry wastewater as claimed in claim 1, wherein the process conditions of the supercritical fluid drying by carbon dioxide are as follows: the pressure is 6-8 MPa, the temperature is 45-50 ℃, and the time is 8-10 hours.
5. The method for adsorbing and purifying livestock and poultry wastewater as claimed in claim 1, wherein in the step (3), the mass ratio of the gel particles, the polyvinyl alcohol aqueous solution and the polyaluminum silicate sulfate is 1: 3.5-4.5: 5.5-7.5, wherein the mass concentration of the polyvinyl alcohol aqueous solution is 8-10%.
6. The method for adsorbing and purifying livestock and poultry wastewater as claimed in claim 1, wherein in the step (3), the stirring reaction time is 30-40 minutes.
7. The method for adsorbing and purifying livestock wastewater as claimed in claim 1, wherein in the step (3), the post-treatment comprises the following specific steps: and (3) preparing raw material balls by using a ball forming mill, roasting for 2-3 hours at 100-107 ℃, and naturally cooling to room temperature to obtain the adsorbent.
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