CN112093871B - Water treatment agent for advanced treatment of petrochemical wastewater and preparation method thereof - Google Patents

Water treatment agent for advanced treatment of petrochemical wastewater and preparation method thereof Download PDF

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CN112093871B
CN112093871B CN202010948929.2A CN202010948929A CN112093871B CN 112093871 B CN112093871 B CN 112093871B CN 202010948929 A CN202010948929 A CN 202010948929A CN 112093871 B CN112093871 B CN 112093871B
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water
treatment agent
water treatment
graphene oxide
treatment
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CN112093871A (en
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沈发治
左艳梅
李佳慧
谢伟
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Yangzhou Polytechnic Institute
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • 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
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56—Macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • 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
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C02F2103/365—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)

Abstract

The scheme relates to a water treatment agent for advanced treatment of petrochemical wastewater and a preparation method thereof. The water treatment agent prepared by the invention is a composite material with a porous structure, and can quickly adsorb and settle organic pollutants; calcium ion, aluminum ion and chloride ion form insoluble Freund's salt Ca4Al2Cl2(OH)12Precipitating to effectively remove the content of chloride ions in the water body; the composite material prepared by the invention is not limited in use environment, and the water quality after treatment can reach the standard of reuse water.

Description

Water treatment agent for advanced treatment of petrochemical wastewater and preparation method thereof
Technical Field
The invention relates to the field of wastewater treatment, in particular to a water treatment agent for advanced treatment of petrochemical wastewater and a preparation method thereof.
Background
The direct discharge of various municipal sewage, domestic sewage, agricultural wastewater, building wastewater, industrial wastewater and the like without treatment causes serious environmental pollution, wherein the petrochemical industrial wastewater is the main reason for water resource waste. At present, the development trend of wastewater treatment is to reduce the source of wastewater and increase recycled water, the industrial wastewater after treatment accounts for one fifth of the make-up water of the recycled water, however, the industrial wastewater contains a large amount of refractory organic matters, such as cyanides, sulfides, volatile phenols, polycyclic aromatic compounds, heterocyclic compounds and the like, the components are complex, even after pretreatment and biochemical treatment, the COD value and the content of various ions are still high, wherein chloride ions are typical corrosive ions, and if high-concentration chlorine-containing wastewater is directly discharged into a water body without treatment, the growth of animals and plants is hindered, aquaculture is influenced, the natural ecological balance of the water body is destroyed, and groundwater is polluted in serious cases.
The existing methods for removing chloride ions can be classified into a precipitated salt method, a separation method, an ion exchange method, and a redox method. The precipitation method can be used for removing chloride ions in water, but the method has higher requirements on the temperature, the treatment time and the addition amount of calcium and aluminum during water purification, can achieve better effect of removing the chloride ions under certain conditions, and cannot be used for reducing other indexes such as COD value of water.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to obtain a novel composite material by using modified graphene oxide loaded with calcium ions and aluminum ions, and the novel composite material is applied to further advanced treatment of chemical secondary sedimentation tank water so as to reach the standard of reuse water.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a water treatment agent for advanced treatment of petrochemical wastewater comprises the following steps:
s1: carrying out acidification and acyl chlorination treatment on Graphene Oxide (GO), drying, grinding, adding 60ml of DMF into the treated GO, carrying out ultrasonic dispersion for 1h, then adding octadecylamine, stirring and refluxing at 60 ℃ for 24h, washing the precipitate with absolute ethyl alcohol, and drying to obtain amide functionalized GO;
s2: adding amide functionalized GO, Azobisisobutyronitrile (AIBN) and dimethyl sulfoxide (DMSO) into a reaction bottle, performing ultrasonic treatment to uniformly disperse the mixture, and heating to 80 ℃; dropwise adding a polymerization monomer solution into the reaction bottle, reacting for 4 hours after dropwise adding, carrying out ultrasonic treatment for 0.5 hour after the reaction is finished under the protection of nitrogen in the whole reaction system, washing precipitates with anhydrous ether, carrying out suction filtration and drying to obtain polymer modified GO;
s3: and adding the polymer modified GO into pure water, adding water-soluble cellulose with equal mass, stirring for 2 hours to uniformly disperse the polymer modified GO, dropwise adding 20ml of calcium oxide/sodium aluminum metaaluminate mixed solution, keeping magnetic stirring for 12 hours, and filtering and freeze-drying the product to obtain the target water treatment agent.
Further, the acidification treatment conditions are preferably: GO is placed in a mixed solution of sulfuric acid and nitric acid with a volume ratio of 3:1 for ultrasonic dispersion for 1h, and then is refluxed in a water bath at 80 ℃ for 4 h.
Further, the acid chlorination treatment conditions are preferably: and putting the acidified GO into a solution of thionyl chloride and DMF, carrying out ultrasonic treatment for 0.5h, and stirring and refluxing for 2h at 80 ℃.
Further, the mass ratio of the amide functionalized GO, AIBN and the polymerized monomer is preferably 1:0.2: 15.
Further, the amount ratio of the calcium oxide/sodium aluminum metaaluminate mixed solution is preferably n (Ca)2+):n(Cl-)＝4:1。
Further, the polymerization monomer is polymerized by acrylamide or copolymerized with a propylene derivative; wherein the propylene derivative is selected from one or more of acrylic acid, acrylonitrile, methyl acrylate and 2-acrylamido-2-methylpropanesulfonic acid.
A water treatment agent for advanced treatment of petrochemical wastewater, which is prepared by the preparation method.
GO has a porous nano structure, can effectively adsorb pollutants in a water body, but cannot be well dispersed in a matrix due to the huge specific surface area, and the dispersity of GO in the water body can be effectively improved through acidification and amidation treatment. And then, through in-situ polymerization, a uniformly dispersed composite material taking a polymer as a continuous phase and graphene as a dispersed phase can be formed, and the flocculation adsorption capacity of the composite material in a water treatment system is further increased.
The Freund's salt precipitation method can be used for removing chloride ions in water, but the method has higher requirements on the temperature, the treatment time and the addition amount of calcium and aluminum during water purification, and can achieve better effect of removing the chloride ions under certain conditions. The water-soluble cellulose is dispersed in organic matter modified GO, which is beneficial to stripping and uniform dispersion of a GO laminated structure, so that calcium oxide/sodium aluminum metaphosphate can be well adsorbed, and calcium ions, aluminum ions and chloride ions form insoluble Freund's salt Ca4Al2Cl2(OH)12And (4) precipitating. The modified graphene oxide forms firm covalent bond, electrostatic attraction or hydrogen bond combination with layered structure Freund's salt and water-soluble cellulose active group, so that the combination of inorganic material and organic material is realized, and the mechanical property of the porous composite material is ensured.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the water treatment agent prepared by modifying graphene oxide and compounding calcium ions and aluminum ions is a composite material with a porous structure, so that organic pollutants can be rapidly adsorbed and settled; calcium ion, aluminum ion and chloride ion form insoluble Freund's salt Ca4Al2Cl2(OH)12Precipitating to effectively remove the content of chloride ions in the water body; the composite material prepared by the invention is not limited in use environment, and the water quality after treatment can reach the standard of reuse water.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
The invention provides a water treatment agent for advanced treatment of petrochemical wastewater, which can be prepared by the following steps:
s1: putting 10g of GO into 20ml of a mixed solution of sulfuric acid and nitric acid with the volume ratio of 3:1, performing ultrasonic dispersion for 1h, then refluxing in a water bath at 80 ℃ for 4h, and drying and grinding after the reaction is finished to obtain acidified GO powder; adding 5g of acidified GO into 60ml of DMF, performing ultrasonic dispersion for 1h, adding 50ml of thionyl chloride, stirring and refluxing for 2h at 80 ℃, then adding 10g of octadecylamine, stirring and refluxing for 24h at 60 ℃, washing the precipitate with absolute ethanol, and drying to obtain amide functionalized GO, wherein the formula is shown in the specification;
Figure BDA0002676265310000041
s2: adding 2g of amide functionalized GO, 0.4g of AIBN and 20ml of DMSO into a reaction bottle, performing ultrasonic treatment to uniformly disperse the mixture, and heating to 80 ℃; preparing 30g of polymerized monomer solution, dropwise adding the monomer solution into the reaction bottle, reacting for 4 hours after dropwise adding, carrying out the whole reaction system under the protection of nitrogen, carrying out ultrasonic treatment for 0.5 hour after the reaction is finished, washing the precipitate with anhydrous ether, carrying out suction filtration, and drying to obtain polymer modified GO;
s3: and adding the polymer modified GO into pure water, adding water-soluble cellulose with equal mass, stirring for 2 hours to uniformly disperse the polymer modified GO, dropwise adding 20ml of calcium oxide/sodium aluminum metaaluminate mixed solution, keeping magnetic stirring for 12 hours, and filtering and freeze-drying the product to obtain the target water treatment agent.
The amount ratio of the calcium oxide/sodium aluminum metaaluminate mixed solution is preferably n (Ca)2+):n(Cl-)＝4：1。
Wherein the polymerization monomer is prepared by self polymerization of acrylamide or copolymerization with propylene derivatives; wherein the propylene derivative is selected from one or more of acrylic acid, acrylonitrile, methyl acrylate and 2-acrylamido-2-methylpropanesulfonic acid.
The method comprises the steps of taking secondary sedimentation tank water after pretreatment and biochemical treatment in a petrochemical plant as test raw water, placing 300ml of raw water in a beaker, and measuring the chloride ion concentration of the raw water by using a chloride ion content measuring instrument, wherein the chloride ion content in the raw water is as high as 802.3mg/L and exceeds the standard that the recycled water requires that the chloride ion content is less than 250 mg/L. During the test, the wastewater treatment agent is uniformly scattered in 300ml of raw water, stirred for 1 minute at a speed of 80-140r/min and then kept stand, and various performance parameters before and after the treatment are tested.
Example 1
The objective water treatment agent was prepared according to the procedure described above, wherein the polymerized monomer was 30g of acrylamide.
Example 1-1: the water treatment agent of the embodiment 1 of the invention is uniformly scattered in 300ml of raw water according to 50mg/L, stirred for 1 minute at 80-140r/min and then kept stand, and various performance parameters before and after treatment are tested.
Examples 1 to 2: the water treatment agent in the embodiment 1 of the invention is uniformly scattered in 300ml of raw water according to 150mg/L, stirred for 1 minute at 80-140r/min and then kept stand, and various performance parameters before and after treatment are tested.
Examples 1 to 3: the water treatment agent in the embodiment 1 of the invention is uniformly scattered in 300ml of raw water according to 300mg/L, stirred for 1 minute at 80-140r/min and then kept stand, and various performance parameters before and after treatment are tested.
Example 2
The objective water treatment agent was prepared according to the procedure described above, wherein the polymerized monomers were 15g of acrylamide and 10g of acrylic acid and 5g of methyl acrylate.
The prepared water treatment agent is uniformly scattered in 300ml of raw water according to 300mg/L, stirred for 1 minute at 80-140r/min and then kept stand, and various performance parameters before and after treatment are tested.
Example 3
The objective water treatment agent was prepared according to the above procedure, wherein the polymerized monomers were 15g of acrylamide and 5g of acrylic acid and 10g of 2-acrylamido-2-methylpropanesulfonic acid.
The prepared water treatment agent is uniformly scattered in 300ml of raw water according to 300mg/L, stirred for 1 minute at 80-140r/min and then kept stand, and various performance parameters before and after treatment are tested.
Comparative example
Comparative example 1: taking calcium oxide/sodium aluminum metaaluminate (n (Ca)2+):n(Cl-) 4: 1 is uniformly scattered in 300ml raw water according to 300mg/L, stirred for 1 minute at 80-140r/min and then kept stand, and various performance parameters before and after treatment are tested.
Comparative example 2: mixing graphene oxide and water-soluble cellulose with equal mass, uniformly dispersing by ultrasonic, uniformly scattering the mixture in 300ml of raw water according to 300mg/L, stirring for 1 minute at 80-140r/min, standing, and testing various performance parameters before and after treatment.
Comparative example 3: mixing equal mass of graphene oxide, water-soluble cellulose, and calcium oxide/sodium aluminum metaaluminate (n (Ca)2+):n(Cl-) 4: 1) mixing and dispersing uniformly by ultrasonic.
Comparative example 3-1: uniformly scattering the mixture into 300ml of raw water according to 300mg/L, stirring for 1 minute at 80-140r/min, standing, and testing various performance parameters before and after treatment.
Comparative example 3-2: uniformly scattering the mixture into 300ml of raw water according to the concentration of 600mg/L, stirring for 1 minute at the speed of 80-140r/min, standing, and testing various performance parameters before and after treatment.
When 300mg/L of the water treatment agent of the invention is added into the water body, the water quality after treatment can reach the reuse water standard. In examples 2 and 3, when a functional propylene derivative was added to the monomer polymer, the performance of the water treatment agent was further improved.
Comparative examples 1 and 2 are the single use of graphene oxide or calcium oxide/sodium aluminum metaaluminate, and the performance of water treatment is too single, and the same amount of the treatment effect is not as good as that of example 3. When the graphene oxide, the cellulose and the calcium oxide/sodium aluminum metaaluminate mixture are directly used as the water treatment agent (the comparative example 3-1 and the comparative example 3-2), the effects of removing chloride ions and reducing COD value can be achieved to a certain extent, but the addition amount is large, and the standard of reuse water can not be achieved (GB/T19923-.
Figure BDA0002676265310000061
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the embodiments disclosed herein may be used in any combination, provided that there is no structural conflict, and the combinations are not exhaustively described in this specification merely for the sake of brevity and conservation of resources. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (7)

1. A preparation method of a water treatment agent for advanced treatment of petrochemical wastewater is characterized by comprising the following steps:
s1: sequentially carrying out acidification and acyl chlorination on graphene oxide, drying and grinding, adding 60ml of DMF (dimethyl formamide) into the treated graphene oxide, carrying out ultrasonic dispersion for 1h, then adding octadecylamine, stirring and refluxing at 60 ℃ for 24h, washing the precipitate with absolute ethyl alcohol, and drying to obtain amide functionalized graphene oxide;
s2: adding amide functionalized graphene oxide, azodiisobutyronitrile and dimethyl sulfoxide into a reaction bottle, performing ultrasonic treatment to uniformly disperse the materials, and heating to 80 ℃; dropwise adding a polymerization monomer solution into the reaction bottle, reacting for 4 hours after dropwise adding, carrying out ultrasonic treatment for 0.5 hour after the reaction is finished, washing the precipitate with anhydrous ether, carrying out suction filtration, and drying to obtain polymer modified graphene oxide;
s3: and adding the polymer modified graphene oxide into pure water, adding water-soluble cellulose, stirring for 2 hours to uniformly disperse the water-soluble cellulose, dropwise adding 20ml of calcium oxide/sodium aluminum metaaluminate mixed solution, keeping magnetic stirring for 12 hours, and filtering and freeze-drying the product to obtain the target water treatment agent.
2. The method for preparing a water treatment agent according to claim 1, wherein the acidifying treatment conditions are: the graphene oxide is placed in a mixed solution of sulfuric acid and nitric acid with a volume ratio of 3:1 for ultrasonic dispersion for 1h, and then is refluxed in a water bath at 80 ℃ for 4 h.
3. The method for producing a water treatment agent according to claim 1, wherein the treatment conditions of the acid chlorination are: and putting the acidified graphene oxide into a solution of thionyl chloride and DMF, carrying out ultrasonic treatment for 0.5h, and stirring and refluxing for 2h at 80 ℃.
4. The method for preparing a water treatment agent according to claim 1, wherein the mass ratio of the amide-functionalized graphene oxide to the azobisisobutyronitrile to the polymerized monomer is 1:0.2: 15.
5. The method for producing a water treatment agent according to claim 1, wherein the polymerizable monomer is polymerized by self-polymerization of acrylamide or copolymerization with a propylene derivative; wherein the propylene derivative is selected from one or more of acrylic acid, acrylonitrile, methyl acrylate and 2-acrylamido-2-methylpropanesulfonic acid.
6. The method for producing a water treatment agent according to claim 1, wherein the amount ratio of the mixed solution of calcium oxide/sodium aluminum metaaluminate is n (Ca)2+):n(Cl-)＝4:1。
7. A water treatment agent for advanced treatment of petrochemical wastewater, which is prepared by the method for preparing a water treatment agent according to any one of claims 1 to 6.
CN202010948929.2A 2020-09-10 2020-09-10 Water treatment agent for advanced treatment of petrochemical wastewater and preparation method thereof Active CN112093871B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105289523A (en) * 2015-11-05 2016-02-03 江苏大学 Preparation method and application of beta-cyclodextrin, graphene oxide and kieselguhr composite
CN107141680A (en) * 2017-06-12 2017-09-08 常州大学 A kind of preparation method of modified graphene oxide/PMMA composites
CN107899551A (en) * 2017-10-11 2018-04-13 福建鸿燕化工有限公司 Amino group graphene/cellulose acetate composite material and its application containing polypyrrole
CN111410460A (en) * 2019-12-17 2020-07-14 李韦皞 Method for immobilizing heavy metals and chloride in incineration fly ash of hazardous waste

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105289523A (en) * 2015-11-05 2016-02-03 江苏大学 Preparation method and application of beta-cyclodextrin, graphene oxide and kieselguhr composite
CN107141680A (en) * 2017-06-12 2017-09-08 常州大学 A kind of preparation method of modified graphene oxide/PMMA composites
CN107899551A (en) * 2017-10-11 2018-04-13 福建鸿燕化工有限公司 Amino group graphene/cellulose acetate composite material and its application containing polypyrrole
CN111410460A (en) * 2019-12-17 2020-07-14 李韦皞 Method for immobilizing heavy metals and chloride in incineration fly ash of hazardous waste

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